Chemical Engineering April 2017

April
2017
www.chemengonline.com
Filtration
Facts at Your Fingertips:
Gas Detection
Focus on Pipes, Tubes
and Fittings
Fertilizers
Safety Sensors
Cooling Towers
Perspectives
on Drying
page 36
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April 2017 Volume 124 | no. 4
Cover Story
36 Part 1 Batch Drying with Vacuum Contact Dryers
Drying is a demanding unit operation where solvents need to be removed
without altering product chemistry. Vacuum contact dryers are essential
pieces of equipment for accomplishing this task
43 Part 2 Optimizing Analysis for Spray Drying
Precise control over spray-drying processes can be enabled
by modern measurement approaches that provide realtime
information on particle size and shape
In the News
9 Chementator
Algae printing ink has safety and sustainability benefits; Pilot project
captures rainwater for wine production; Award to lower costs
for flow-battery reactants and membranes; A quest for making
ammonia at moderate conditions; and more
16 Business News
Messer opens its largest CO2-recovery plant; Wacker expands
silicon-metal capacity at Norwegian production site; KBR awarded revamp
contract for LG Chem ethylene plant expansion; Worlds largest MTO plant 36
starts up in China; and more
18 Newsfront The Spread of Nitrogen Fertilizers
As price margins tighten, ammonia and urea producers are diversifying their
products, while new catalysts and process improvements boost capacities and
lower energy consumption
22 Newsfront The Future of Safety Sensors is Here Now
Wearable sensors enhance chemical plant worker safety and help close the
approaching skills gap 49
Technical and Practical

33 Facts at your Fingertips Gas Detection
This one-page reference provides information on major classes of gas detection
technologies and on the characteristics of several gases that may be targets of 18
detection in CPI facilities
34 Technology Profile Bio-based Adipic Acid Production
from Glucose This process description outlines a catalytic approach
for making adipic acid from glucose
49 Feature Report Part 1 Crossflow Membrane Filtration 22
Essentials Several aspects of crossflow membrane filtration, including
process design, equipment selection and control, are detailed here
60 Feature Report Part 2 Gas-Phase Filtration Media

Properties: What to Know There are many physical properties that
can impact the ultimate performance of adsorbent media in gas-phase filtration
applications
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM APRIL 2017 1

64 Engineering Practice Cooling Towers: Estimate
Evaporation Loss and Makeup Water Requirements
Applying mass and energy balance calculations yields critical operating insight
Equipment and Services

28 Focus on Pipes, Tubes and Fittings
This pipe-milling end-prep tool is for beveling boiler tubes; Flat-faced seal
replaces elastomeric O-rings; Drum pumps now offer a broader choice of
tubes; Silicone hose is compatible with many clean applications; Isolation joint
improves safety of flanged pipe connections; and more
31 New Products
28 A compact compressor for H2-refueling stations; Save time and water with
this tank-cleaning machine; This range of diaphragm pumps is extended;
Predict product performance with a digital twin; Flow measurement at low
temperatures; This closed-system mixer requires no transfer steps; and more
Departments
5 Editors Page Designating a day for water
31
March 22 has been designated as World Water Day. Its observance brings
attention to global water resources and, this year, particularly to the need to
focus on wastewater
6 Letters
80 Economic Indicators
Advertisers
35 Hot Products
69 Solids Processing Special Advertising Section
76 Product Showcase
77 Classified
78 Reader Service
79 Ad Index
Chemical Connections
Follow @ChemEngMag on Twitter
Join the Chemical Engineering Magazine
LinkedIn Group
Visit us on www.chemengonline.com for Latest News,
Webinars, Test your Knowledge Quizzes, Bookshelf
and more
Coming in May
Look for: Feature Reports on Maintenance & Reliability; and Storage
Tanks; A Focus on Solids Handling Equipment; A Facts at your
Fingertips on Level Measurement and Control; News Articles
on Petroleum Refining; and Water & Wastewater Treatment; a Solids
Processing article on Powder Testing Techniques; New Products;
and much more
Cover photo: Photo courtesy of Ekato Systems

Cover design: Rob Hudgins
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Editor s Page
EDITORS ART & DESIGN
Designating a day for water
DOROTHY LOZOWSKI ROB HUDGINS
L
Editorial Director Graphic Designer ast month, special recognition to water-related issues was
rhudgins@accessintel.com
dlozowski@chemengonline.com given on March 22, the date designated by the United Nations
GERALD ONDREY (FRANKFURT) PRODUCTION as World Water Day. The first World Water Day was observed
Senior Editor
gondrey@chemengonline.com SOPHIE CHAN-WOOD in 1993, and has been celebrated every year since. The pur-
Production Manager
schan-wood@accessintel.com pose of the observance is to bring attention to our water resources
SCOTT JENKINS
Senior Editor INFORMATION and offer learning opportunities, as well as to inspire others to sustain-
sjenkins@chemengonline.com SERVICES ably manage those resources. This year, the theme of World Water
MARY PAGE BAILEY CHARLES SANDS Day was wastewater, to focus on the need to improve water reuse.
Associate Editor Director of Digital Development
mbailey@chemengonline.com csands@accessintel.com We cover water treatment regularly in our magazine, and I have
PUBLISHER, SALES & CONTRIBUTING EDITORS
written about its importance a number of times, yet each time I learn
MARKETING
SUZANNE A. SHELLEY
more, it impresses upon me how far-reaching the impact of water-
MATTHEW GRANT sshelley@chemengonline.com related issues is. The World Water Day website (www.worldwaterday.
mattg@powermag.com
CHARLES BUTCHER (U.K.) org) offers the following information in its Fact Sheet.
cbutcher@chemengonline.com
AUDIENCE
DEVELOPMENT
Over 80% of wastewater generated by society goes back into the
PAUL S. GRAD (AUSTRALIA) ecosystem without being used or recycled. High-income countries
SARAH GARWOOD pgrad@chemengonline.com
Audience Marketing Director treat around 70% of wastewater, and the percentage drops dra-
sgarwood@accessintel.com
TETSUO SATOH (JAPAN)
tsatoh@chemengonline.com
matically in lower-income countries
JESSICA GRIER
Marketing Manager
1.8 billion people are at risk for life-threatening diseases because of
jgrier@accessintel.com JOY LEPREE (NEW JERSEY) contaminated sources of drinking water
jlepree@chemengonline.com
GEORGE SEVERINE The portion of the worlds population living in cities is expected to
Fulfillment Manager
gseverine@accessintel.com
grow from 50% to 70% by 2050, while many cities are not equipped
to address growing wastewater management needs
JEN FELLING
List Sales, Statlistics (203) 778-8700
j.felling@statlistics.com The CPI contributes
EDITORIAL ADVISORY BOARD Industrial production accounts for nearly 25% of global water con-
sumption, according to a statement released in conjunction with
JOHN CARSON JOHN HOLLMANN
Jenike & Johanson, Inc. Validation Estimating LLC World Water Day by Lanxess (www.lanxess.com). The chemical
DAVID DICKEY HENRY KISTER process industries (CPI) are well equipped to provide solutions to in-
MixTech, Inc. Fluor Corp. dustrial, as well as municipal water- and wastewater-treatment chal-
HEADQUARTERS
lenges. Our engineers and scientists are very familiar with pertinent
40 Wall Street, 50th floor, New York, NY 10005, U.S. technologies, such as advanced filtration techniques (see the Feature
Tel: 212-621-4900
Fax: 212-621-4694 Report in this issue on Crossflow Membrane Filtration, pp. 4959).
EUROPEAN EDITORIAL OFFICES
And new technologies are being developed around the world. See
Zeilweg 44, D-60439 Frankfurt am Main, Germany for example, the Chementator article in this issue about a group in
Tel: 49-69-9573-8296
Fax: 49-69-5700-2484 Singapore who are working on removing pollutants from water with
CIRCULATION REQUESTS: iron hydroxides (p. 12), and the work in Korea on developing a new
Tel: 847-564-9290 water-treatment adsorbent reported last month (A New Adsorbent for
Fax: 847-564-9453
Fullfillment Manager; P.O. Box 3588, Wastewater Treatment, Chem. Eng. March 2017, p. 11).
Northbrook, IL 60065-3588
email: chemeng@omeda.com
ADVERTISING REQUESTS: SEE P. 62 Spotlighting World Water Day

For reprints, licensing and permissions: Wright's Media, 1-877-652-5295,
sales@wrightsmedia.com
CPI companies have joined in the observance of World Water Day to
help spread the news about water scarcity issues and how to address
ACCESS INTELLIGENCE, LLC
them. The Dow Chemical Company (www.dow.com) for example,
DON PAZOUR
Chief Executive Officer
JONATHAN RAY
Vice President, Digital
participated in an event in Tucson, Ariz. where representatives from
industry, business, academia and government interacted on water-
HEATHER FARLEY MICHAEL KRAUS
Chief Operating Officer Vice President, related topics. The event included a tour of the University of Arizonas
Production, Digital Media & Design
Water and Energy Sustainable Technology Center, as well as the un-
ED PINEDO
Executive Vice President STEVE BARBER veiling of the World Water Day paint scheme for the
& Chief Financial Officer Vice President,
Financial Planning and Internal Audit No. 3 Dow Chevrolet car, which competed in the
MACY L. FECTO
Exec. Vice President, GERALD STASKO
Camping World 500 at the Phoenix International
Human Resources & Administration Vice President/Corporate Controller Raceway on March 19.
JENNIFER SCHWARTZ Current world news has many concerned about the
Senior Vice President & Group Publisher
Aerospace, Energy, Healthcare future of environmental endeavors. The need to share
information about the importance of better wastewa-
ROB PACIOREK
Senior Vice President,
9211 Corporate Blvd., 4th Floor
Rockville, MD 20850-3240
ter treatment is perhaps greater that it has been, mak-
Chief Information Officer www.accessintel.com
ing a designated day all the more important.
Dorothy Lozowski, Editorial Director

Letters
Steam Concepts
I enjoy reading your magazine and find many of its ar-
ticles informative and helpful. I noticed several errors in
the [Facts at Your Fingertips] article, Steam Concepts,
[February 2017, p. 32] and wanted to bring them to your
Where can you find all your attention:
1. In the section Pressure-temperature relation the
CPI solutions in one spot? author states: enthalpy, a thermodynamic property
of a fluid that is defined as the internal energy of
the fluid added to the product of its pressure and
temperature. This is incorrect. Enthalpy is the inter-
The Chemical Processing Industry covers a nal energy added to the product of its pressure and
broad range of products such as petrochemical specific volume.
2. In the second paragraph under Industrial practice
and inorganic chemicals, plastics, detergents,
the author states: Lower heat transfer rates occur
paints, pulp & paper, food & beverage, rubber because condensed water can form a film on heat-
and many more. Chemical Engineering transfer surfaces, which reduces heat transfer be-
cause thermal conductivity of water is much lower
magazine is uniquely suited to cover this
than that of steam. The observation is correct but
worldwide market. the reasoning is incorrect. The thermal conductiv-
ity of liquid water is in fact significantly higher than
steam. This is true for most liquids when compared
to gases. The reason for the lower heat transfer
rates when a film of liquid water forms on the heat
transfer surfaces is as the author stated earlier in
the article: the heat transfer coefficient (capacity) for
condensing steam is significantly higher than for liq-
uid water (at the same temperature and pressure).
And this higher heat-transfer capacity is mainly due
to it changing phase from a gas to a liquid where
large amounts of energy are released. So in fact
liquid water must form when steam is condens-
ing on heat transfer surfaces. The trick is to design
the surfaces so that this condensate drains away
quickly and that steam traps are suitably sized so
that condensate doesnt backup onto the heat
transfer surfaces.
Mike Protheroe
Auckland University of Technology
Written for engineers by engineers, Chemical Editors note: Thank you for pointing out the errors in
the column. Regarding the definition of enthalpy, you are
Engineering delivers solid engineering essentials correct the inclusion of temperature for volume was
and developing industry trends to keep its readers a typographical error. Regarding the discussion of water
films on heat-transfer surfaces, the author was trying to
abreast of everything they need to keep their condense a longer explanation, and it was indeed flawed.
facilities running smoothly. Thank for you clarifying this. The online version has been
updated to reflect these corrections, and can be found
at www.chemengonline.com/steam-concepts/.
Missing archived issues or what Making ammonia at milder conditions

There were errors in two chemical formulas in the
to share Chemical Engineering Chementator article, Making ammonia at milder con-
with your colleagues? ditions, (Chem. Eng., November 2016, p. 11). The for-
mulas shown as Ru/CO2 and Ry/MgO should be Ru/
Visit www.chemengonline.com/ CeO2 and Ru/MgO. The corrected version of the story
can be found online at www.chemengonline.com/
chemical-engineering-magazine making-ammonia-milder-conditions.
for more information. Thank you to our long-time reader, Sorab R. Vatcha,
consultant from Mountain View, California, for finding
the error and bringing it to our attention.
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Chementator
Algae printing ink has safety and
sustainability benefits Edited by:
Gerald Ondrey
S
cientists at Liv- Algae-to-ink process
ing Ink Technol- EFFICIENT DISTILLATION
ogies (Denver,
Toyo Engineering Corp.
Colo.; www. (Toyo; Chiba, www.toyo-eng.
livinginktechnologies. co.jp) has completed con-
com) have developed struction for an energy-sav-
biodegradeable printing distillation system used in
ing ink made from natu- a project for Maruzen Petro-
ral cyanobacteria and 1. Species 2. Cultivation 3. Harvest 4. Ink 5. Print
chemical Co. (Tokyo, Japan;
algae as a sustainable www.chemiway.co.jp). This
and non-toxic alterna- system, tradenamed Su-
tive to conventional petroleum-derived and simple, because Living Ink uses the perHIDiC, has achieved an
energy saving of over 50%
printing inks. whole cell for the ink, rather than extracting
compared with conventional
Living Inks method involves using sun- pigments from the cells with downstream distillation, says Toyo.
light and carbon dioxide to grow a variety processing steps, explains Scott Fulbright, The newly installed sys-
of algae and cyanobacteria species that are the companys co-founder and CEO. For tem was designed with the
colored by pigmented molecules they pro- the ink strains, We needed to find the aim of providing large en-
duce. For example, green ink comes from right combination of pigment color, ability ergy savings for the methyl
chlorophyll produced by the cells, while to grow effectively in industrial settings and ethyl ketone (MEK) pro-
other strains result in red, yellow and or- cell size, which is on the order of 15 mi- duction plant at Maruzen
ange inks. Living Ink is also working on a crons, Fulbright adds. Petrochemical site in Chiba
genetically engineered algae strain that can Living Ink is targeting the packaging ink Prefecture, and is the first
commercial application of a
be used for black-colored ink. and stationery markets initially. The com-
SuperHIDiC system.
To make the inks, algae is grown in con- pany has partnered with algae produc- SuperHIDiC is based on
trolled containers, then concentrated in a tion company Cellana Inc. (Kailua, Ha- the heat-integrated distilla-
harvesting step (photos). Other plant-based waii; www.cellana.com) for high-volume tion column (HIDiC) tech-
materials are added to the cells to complete production of algae, and was recently nology, which has been
the ink formulations, which can then be awarded a Small Business Innovation researched for many years
printed onto paper, cardboard and cotton Research (SBIR) grant from the U.S. Na- by companies, universities
textiles using conventional printers. tional Science Foundation to further de- and research institutions
The ink production process is low-cost velop the algae-based inks. around the world. Toyo has
further refined this technol-
ogy (Chem. Eng., Janu-
A pilot project to capture rainwater for ary, p. 10), in collaboration
with the National Institute
wine production of Advanced Industrial Sci-
ence and Technology (AIST;
A
pilot project set up by the Univer- pilot system, which captures and trans- Tokyo, www.aist.go.jp), and
sity of California Davis (UC Davis; ports rainwater from the roofs of several plants to expand commer-
Davis, Calif.; www.ucdavis.edu), UC Davis campus buildings to a hold- cial applications.
GE Water & Process Technolo- ing tank. After subsequent filtration, the
gies (Trevose, Pa.; www.gewater.com) and water is pumped into 45,000-gal feed SOLAR STEAM
wine-industry service provider Winesecrets tanks for the water-treatment process. Queen Mary University of
LLC (www.winesecrets.com) seeks to cap- Most of what the membrane technology London (QMUL; www.qmul.
ture rainwater for use in wine production, separates from the rainwater are the dust ac.uk) and industry partner
specifically for cleaning the winemaking and particulate matter that settles on the Larkfleet Ltd. (Bourne, U.K.;
equipment. Collected rainwater represents roofs and in the gutters between rainfalls, www.larkenergy.co.uk) have
received 800,000 (about
an attractive source for water, especially says Hertel.
$98,000) in funding to further
in areas that swing from extreme rainfall UC Davis has been operating the pilot develop a concentrated-
to drought, explains GEs sales manager system at its discretion since commission- solar-thermal technology for
Ryan Hertel. Since rainwater naturally has ing was completed in December 2016, producing industrial steam.
little alkalinity or mineral content, the water- reportedly treating about 7,000 gal/d of The funding for the two-year
treatment requirements to achieve com- water. With the extremely wet and rainy project, provided by Innovate
parable purity are much less complex and season California has recently experi- UK, the Newton Fund and the
costly than drawing water from traditional enced, the system has been running a National Science and Tech-
sources, such as wells, aquifers or rivers. lot, comments Hertel. For the projects nology Council in Mexico, will
GE provided a reverse-osmosis mem- next phase, UC Davis plans to livestream allow an already developed
prototype of the solar collec-
brane system and equipment for total- the analytics from the treatment system di-
oxygen-content (TOC) analysis to the rectly over the Internet. (Continues on p. 10)

tor to be improved, to the point Award to lower costs for flow-battery
of commercialization, at a site
in Mexicos Morelos state.
membranes and reactants
U
Developed and patented by nited Technologies Research Cen- that was originally used in phosphoric-acid
Larkfleet, the solar collectors ter (UTRC; East Hartford, Conn.; fuel cells. The simple, porous ionic separator
use plastic Fresnel lenses in- www.utrc.utc.com) has been is doped with sulfuric acid and may obviate
stead of conventional glass awarded a $2.7-million cooperative the need for more expensive ion-exchange
reflectors. The Fresnel lenses research agreement to further develop two membranes in stationary flow batteries.
frame rotates to track the technologies aimed at lowering the capital Such a membrane could lower the cost of
movement of the sun using a cost of flow batteries for electrical grid-en- that component by a factor of five, says
fully automatic system, which
ergy storage. UTRC researcher Michael Perry.
allows for the concentration
of maximum levels of solar ra-
UTRC will lead the U.S. Department of In addition, the award will support devel-
diation on the collector tubes, Energys ARPA-E (Advanced Research opment work on lower-cost flow-battery
says the company. The new Projects Agency Energy) Integration and reactants. Currently, most flow-battery reac-
design is lighter than glass Optimization of Novel Ion-Conducting Sol- tants are based on vanadium or other tran-
systems, which makes it ids (Ionics) program. Other participants in sition metals, but the research team will be
transportable and potentially the Ionics program include Harvard Univer- screening engineered organic molecules for
easier to manufacture. sity, Lawrence Berkeley National Labora- new reactant possibilities. These organic-
The technology is said to tory, the University of South Carolina and based reactants, or iron-ligand complexes,
be ideal for medium-temper- Advent Technologies. could lower flow-battery reactant costs while
ature applications, such as
The research team will seek to build upon maintaining electrochemical performance,
the manufacturing of textiles,
chemicals and medicines,
UTRCs work on a polar polymer membrane Perry suggests.
for cooking, or any other
processes requiring temper-
atures up to 250C. A quest for making ammonia
at moderate conditions
OXIDATION CATALYST
T
Last month, BASF SE (Lud- oday, am- NH3 High prerssure, P < 10 bars N2
wigshafen, Germany; www. monia con-
basf.com) launched Camet tinues to Porous Ru
catalyst layer
ST, a new sulfur-tolerant oxi- be manu- 3H2 + N2 2NH3
dation catalyst for controlling factured by the
CO emissions from natural- Haber-Bosch pro-
gas-fired power plants. Camet cess an energy- H2 dissociation BCC metal (Nb, V & alloys)
ST builds on the companys H diffusion
intensive process Catalyst (5100 nm)
standard Camet oxidation
catalyst technology, while
that operates at
also improving the ability of high temperatures H H H H H H
Dissociative H2 H-H
the catalyst to perform in and pressures adsorption H-H
the presence of most forms (above 400C and H-H H-H
of sulfur contamination with 100 bars). For de-
minimal deactivation. In ex- cades, researchers around the world have conventional Haber-Bosch synthesis, says
tended full-scale trials, BASF been looking for alternative routes to making Way. We use a niobium or vanadium foil
Camet ST catalyst maintains NH3, such as those based on electrochem- membrane which is several orders of
performance while the com- istry, but for now, industrial efforts are pre- magnitude less expensive than palladium
petitive catalyst rapidly deac-
dominantly focused on process and catalyst coated with an H2-dissociation catalyst on
tivated, says BASF. Camet ST
is currently deployed in several
refinements for Haber-Bosch synthesis (see one side, and a nanostructured N2-dissocia-
commercial units where sulfur the Newsfront article on pp. 1821). tion catalyst on the other side.
contamination previously re- A new approach is being investigated by In proof-of-concept experiments, a ruthe-
sulted in excessive downtime researchers at the Colorado School of Mines nium catalyst was used for N2 dissociation,
and frequent cleaning. (Golden, Co.; www.mines.edu), as part of an but other materials are being examined as
Ideas project funded by the U.S. Dept. of part of the project, says Way. With ruthenium,
3-D PRINTING BNNT Energys ARPA-E program. The 11.5-year the researchers have demonstrated NH3
Researchers at the Institute project aims to demonstrate the feasibility synthesis at 0.8 bar and 500C, achieving
for Frontier Materials, Dea- of a low-cost membrane reactor for synthe- a higher rate (6 105 mol/m2.s) than that
kin University (Waum Ponds, sizing NH3. The concept uses a hydrogen- achieved by solid-state electrochemical pro-
Australia; www.deakin.edu. permeable metallic membrane to transport cesses, and without the need for supplying
au/ifm) have achieved a atomic hydrogen to the other side of the an external voltage. Ultimately, the membrane
world-first in successfully membrane where the NH3 synthesis reac- reactor has the potential to increase the NH3
3-D printing a boron nitride
tion occurs (diagram), explains professor J. flux to more than 0.1 mol/m2.s by optimizing
nanotube/titanium (BNNT)
composite. BNNTs are an
Douglas Way, the project coordinator. This the N2-dissociation catalyst, says Way. A pat-
advanced new nanomaterial makes it possible to decouple the two dis- ent has been filed on the membrane reactor
sociation reactions of H2 and N2, which concept, and Way would welcome hearing
(Continues on p. 12) compete for active sites on the catalyst of from potential industrial partners.
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with many unique properties, Hydronium ions as charge carriers
explains professor Ying (Ian)
Chen, chair in Nanotechnol-
S
cientists at Oregon State University (rather than single protons) were incorporated
ogy. They are ultralight, super (Corvallis; www.oregonstate.edu) into the PTCDA crystal lattice, indicating a
strong and incredibly resistant
have for the first time demonstrated new chemistry for charge storage, Ji explains.
to heat, he says.
However, in the 20 years
the use of hydronium ions (H3O+) as The researchers also found that H3O+ ions
since the materials discovery, charge carriers. The research opens another diffuse at higher rates than K+ or Na+ ions
it has only been possible to avenue of exploration for high-power, sus- through the electrode structure, suggesting
produce it in small amounts, tainable batteries for stationary power-stor- that H3O+ has lower migration-activation
which has seriously limited its age applications. energy, Ji says. Although the reason for this
practical use in product devel- The research team, led by professor Xiulei low-friction property is not yet clear, it could
opment. Our novel and scal- Ji, demonstrated that hydronium ions can eventually give rise to higher-power batteries.
able manufacturing process be reversibly stored in an organic crystal- The next stage of research in this area may
can effectively eliminate this line material, perylenetetracarboxylic dianhy- be to focus on identifying cathode, anode
production bottleneck and un-
dride (PTCDA), which has been used as an and electrolyte materials for a battery system
leash the real power of BNNTs
into the marketplace.
electrode in lithium-ion and other batteries. using H3O+ as a charge carrier.
Using dilute sulfuric acid as the electrolyte, The research was published in a recent
(Continues on p. 13) the researchers confirmed that the H3O+ ions issue of Angewandte Chemie, Intl. ed.
A less expensive alternative to platinum for water electrolysis
A
suitable catalyst for splitting also less stable in an alkaline envi- Ru and C2N, a two-dimensional gra-
water to make hydrogen ronment. Catalysts made of inex- phene-like structure, to verify its per-
must exhibit high H2-con- pensive, non-noble metals corrode formance as a water-splitting catalyst.
version efficiency, excellent rapidly under acidic conditions and To synthesize the Ru@C2N catalyst,
durability, and must operate well operate at very high voltages, which the team mixed the ruthenium salt
under low voltage. For an efficient limits productivity. (RuCl3) with the monomers that form
H2-evolution reaction, the catalyst Now, researchers from Ulsan the C2N. The catalyst was then pro-
must be able to trigger proton re- National Institute of Science and duced through reduction and heat-
duction with minimal overpotential Technology (UNIST; Ulsan, South treatment processes.
and must have fast kinetics. Cur- Korea; www.unist.ac.kr), led by The researchers used the same pro-
rently, the most efficient catalysts professor Jong-Beom Baek, have cesses to produce M@C2N (M = Co,
in acidic media are platinum-based, developed a ruthenium-based Ni, Pb, Pt) catalysts. The Ru@C2N
because the strength of the PtH water splitting catalyst that acts catalyst exhibited the highest perfor-
bond is associated with the fastest almost as effectively as platinum, mance at the lowest overvoltage. It
reaction rate for the H 2-evolution but is less expensive and is not af- exhibits high turnover frequencies at
reaction. However, the Pt-based fected by the water pH. 25 mV, as high as Pt, and can be used
catalysts are expensive, and are The UNIST team has synthesized in any environment.
Remove pollutants from wastewater with this

nano-tailored coating
R
esearchers from the Agency lutants. If iron particles are turned nanoparticles to maintain a high
for Science, Technology into nanomaterials their, active sur- active surface area for effective
and Research (A*STAR, face areas are increased, which pollutant removal.
Singapore; www.a-star. enhances their chemical adsorp- The researchers observed that this
edu.sg) have developed low-cost, tion capability. However, it remains material safely traps and removes
environmentally friendly iron-hy- difficult to separate iron hydroxide contaminants by immersion in dirty
droxide coatings with unique fin-like particles from water, which is nec- water, and can then be regener-
shapes that absorb large amounts essary due to their toxicity. ated by means of a simple chemical
of pollutants, such as dyes, from To overcome this drawback, the treatment. For example, they tested
drinking water, by means of a sim- researchers synthesizing iron-hy- the material in water contaminated
ple dipping procedure. droxide coatings with a hierarchy by a Congo red dye. Within 30 min.,
Iron hydroxides are being in- of structural features, from nano- the water turned almost colorless,
creasingly used instead of con- to micrometer scales, by electro- with more than 90% of the dye at-
ventional activated charcoal (AC), deposition of aqueous metal ions tached to the special coating. Even
because AC does not easily re- onto nickel foam at mild voltages. though these coatings have some
move heavy metals and bulky or- Electron microscopy shows that of the highest capacities ever re-
ganic compounds from water. Ion the coatings nanostructure has ported, they are only operating at a
hydroxides, on the other hand, can elongated, fin-like protrusions, fraction of their theoretical capacity,
form stable bonds to those pol- which enable the immobilized the researchers say.
Peltier refrigeration expands While BNNTs have a structure
into untapped applications similar to carbon nanotubes
and share the same extraordi-
nary mechanical properties and
W
hen compared to traditional re- for scalability in terms of the amount of heat
thermal conductivity, they are
frigeration cycles, Peltier (ther- removed. As you apply an electric current
able to withstand double the
moelectric) technology has across a semiconductor chip, one side gets temperatures (up to 800C).
many benefits, including no hot and one side gets cold. The application This superior heat tolerance is
moving parts and no hazardous refrigerant of that coldness determines the commercial critical for surviving the extreme
chemicals. However, it has not yet been efficacy, he explains. However, the key to a temperatures involved in melt-
widely adopted into large-scale industrial robust thermoelectric cooling system is not ing and liquefying powders dur-
processes (due to poor efficiency, inabil- the chip itself, but the incorporation of the chip ing the 3-D printing process for
ity to scale cooling and high costs) until into a thermal system that can handle high metal matrix composites.
now. Phononic Inc.s (Durham, N.C.; www. heat flux with low parasitic losses. The me- BNNTs also have greater
phononic.com) line of Peltier-cooled refrig- chanical system design is just as important as chemical stability and elec-
trical insulation properties,
erators known as Evolve have been the semiconductor chip itself, Atti comments.
the ability to shield against
deployed into the healthcare and life-sci- Phononics thermal design involves com- neutron and ultraviolet radia-
ences sectors. The company is also cur- bining active and passive heat-transport tion and to generate electrical
rently investigating the integration of Peltier systems, that when integrated with the ad- current when subjected to
systems into industrial chilled-water loops. vanced semiconductor chips, result in per- mechanical stress.
Phononic has built working prototype refrig- formance metrics that are competitive with Deakin has patented its
erators for augmenting chilled-water loops compressor-based refrigeration systems. BNNT production technol-
in data-center cooling, and has conducted Depending on the application, the Peltier ogy, which is ready to be
successful benchtop demonstrations. units may consume 1030% less energy scaled up to meet the increas-
Phononics patented semiconductor chips than compressor cycles, says Atti. Phonon- ing demand for BNNTs, and
plans to build a commercial
deliver a large temperature gradient between ics current product offerings include 1.8-
BNNT pilot plant at its Waurn
the hot and cold side while simultaneously and 5.5-ft3 pharmacy-grade refrigerators, Ponds campus to produce
pumping a tremendous amount of heat per as well as household wine coolers. Later BNNTs in kilogram quantities.
unit area, says Tony Atti, Phononic founder this year, the company plans to release the
and CEO. This combination of traits allows worlds first solid-state freezer. (Continues on p. 14)

HIGH-THROUGHPUT SCREENING New glass electrolytes yield safer,
The number of combinations of substances for more efficient batteries
coatings formulations is enormous: Even if only
A
glassy solid-state electro- glass-electrolyte battery systems.
ten hardeners, ten binding agents, ten pigments
and ten additives are to be taken into account in
lyte (SSE) developed by re- The new SSEs compatibility with
the development of a coating formulation, this searchers from the University lithium, sodium and potassium en-
results in 10,000 combinations. And this does of Texas at Austin (UT; www. ables the use of these alkali metals
not even include variations in proportions. With utexas.edu) will aid in the evolution on anodes, which isnt possible with
its new, fully automated plant for testing coating of safer, longer-lasting rechargeable traditional batteries. Furthermore, the
formulations, Evonik Resource Efficiency GmbH batteries. A major concern with the SSE is also universally compatible with
(Essen, Germany; www.evonik.com) can now use of lithium- and sodium-ion bat- off-the-shelf cathodes, enabling its
accelerate the search for optimal formulations. teries is the formation of dendrites, use as a drop-in replacement for liquid
In the first step, the plant dispenses raw ma- which can interfere with liquid and electrolytes, according to Murchison
terials automatically and formulates them into
crystalline electrolytes, causing bat- and Braga. The SSE is produced via
coatings. In the second step, the substrates are
coated with the formulations, dried, and then
tery short-circuits or worse, ex- wet chemistry, in a process the team
transported to the test stand. At the test stand, plosions and fires. UTs glassy elec- believes could be readily scaled up.
the properties of the formulations are character- trolytes are non-flammable and allow Another potential benefit of batter-
ized. All steps are carried out automatically ac- for homogenous plating on the cath- ies employing the new SSEs is the
cording to a precisely defined program that can ode and anode, which eliminates ability to operate at much lower tem-
be reproduced at any time. the formation of dendrites, say UT peratures. The glass electrolyte has
The plant consists of 52 elements that are com- researchers Andrew Murchison and low activation energy for the conduc-
bined in 30 functionalities; each functionality is de- Helena Braga. Furthermore, the elec- tion of the working ions. Therefore,
signed to handle a specific task (for example, to trolyte will not oxidize at the voltages we think it will be able to work at low
apply a coating formulation to a substrate). The 52
needed to charge and discharge the temperatures, says Murchison. The
elements are connected by a rail system that goes
through all parts of the plant; on the rail systems,
electrodes that are currently available team has tested cells at temperatures
containers and substrates are transported via on the market. Simplified battery-cell as low as 20C, and in experiments,
shuttle. In addition, there are 13 robots that carry fabrication, high volumetric energy the glass electrolyte has performed
out various activities, such as loading the shuttle density and faster rates of recharge considerably better than other SSEs
or placing coated substrates in the oven. are among the other benefits of the at temperatures below 60C. n
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Business News
LINEUP Plant Watch which has doubled the companys catalyst
SNC-Lavalin wins EPC contract for manufacturing capacity in India.
ABENGOA
ammonia plant in Oman
AMEC FOSTER March 9, 2017 SNC-Lavalin (Montreal, Ingleside Ethylene starts up
WHEELER Que., Canada; www.snclavalin.com) has been ethylene cracker in Texas
ARKEMA awarded a contract by Salalah Methanol Co. March 1, 2017 Ingleside Ethylene, LLC, the
LLC (SMC) for the engineering, procurement 50/50 joint venture (JV) between Mexichem
BASF and construction (EPC) of an anhydrous liquid S.A.B. de C.V. (Tlalnepantla, Mexico; www.
CEPSA ammonia plant, including its utilities and offsite mexichem.com) and OxyChem (Dallas, Tex.;
infrastructure, in the city of Salalah, located in www.oxychem.com), begun operation of its
ENI ethylene cracker at OxyChems Ingleside, Tex
the Sultanate of Oman. Closing of financing
EVONIK by SMC is expected to occur in June 2017. site. The cracker has the capacity to produce
550,000 m.t./yr of ethylene.
GE WATER
Messer opens its largest
GRUPO IDESA CO2-recovery plant Arkema to increase PEKK production
March 8, 2017 Messer Group (Bad Soden, in France and the U.S.
HENKEL
Germany; www.messergroup.com) recently February 24, 2017 Arkema (Colombes,
HONEYWELL UOP opened its largest CO2-recovery plant on the France; www.arkema.com) recently doubled
globe. Located in Nanjing, China, the plant the capacity of its poly-ether-ketone-ketone
KBR
has a capacity of 150,000 metric tons per (PEKK) product line in France, and confirms
LG CHEM year (m.t./yr). Messer is now recovering a its future investment at its Mobile, Ala. site in
MESSER total of 300,000 m.t. of CO2 from industrial a world-scale PEKK plant expected to come
processes per year in China. In addition to the onstream in the second half of 2018. These
MEXICHEM CO2 recovery plant, Messer is also building a investments will serve the growing needs of
OXYCHEM new technology center for gas applications the composites and 3-D printing markets.
in Nanjing.
PERSTORP KBR awarded revamp contract for
ROYAL DSM Wacker expands silicon-metal LG Chem ethylene plant expansion
capacity at Norwegian production site February 23, 2017 KBR, Inc. (Houston;
SNC-LAVALIN www.kbr.com) was awarded a technology
March 8, 2017 Wacker Chemie AG (Munich,
SUEZ Germany; www.wacker.com) is expanding licensing and basic engineering design
the capacity of its silicon-metal site in Holla, revamp contract by LG Chem (Seoul, South
SYNTHOMER Korea; www.lgchem.com) for its ethylene
Norway. The company is constructing an
WACKER additional world-scale plant in Holla, with plant in Daesan, South Korea. KBR will
capital expenditures of around 85 million provide services to expand ethylene capacity
budgeted for the capacity increase and for by 230,000 m.t./yr, resulting in a total capacity
expanding local infrastructure. Completion of 1,270,000 m.t./yr through the addition of two
of the plant is expected during the first half new furnaces and other system modifications.
of 2019.
CyPlus Idesa inaugurates
Amec Foster Wheeler wins EPC contract sodium cyanide plant in Mexico
from Eni for steam-reforming plant February 22, 2017 CyPlus Idesa, a JV
March 8, 2017 Amec Foster Wheeler between Evonik Industries AG (Essen,
(London, U.K.; www.amecfw.com) was Germany; www.evonik.com) and Grupo
awarded an EPC contract in excess of 50 Idesa S.A. De C.V. (Mexico City, Mexico;
million by Eni S.p.A. (Rome, Italy; www.eni.com) www.grupoidesa.com), officially opened its
for a new steam-reforming plant for hydrogen new production plant for sodium cyanide in
production to be built at Enis petroleum refinery Veracruz, Mexico. The new plant has capacity
in Gela, Italy. Amec Foster Wheeler will also to produce 40,000 m.t./yr of sodium cyanide.
support Eni during commissioning, startup
and testing. The companys role is expected Worlds largest MTO
to be completed in the fourth quarter of 2018. plant starts up in China
February 22, 2017 Honeywell UOP (Des
BASF inaugurates catalyst Plaines, Ill.; www.uop.com) announced that
manufacturing site in Chennai Jiangsu Sailboat Petrochemical Co. started
March 3, 2017 BASF SE (Ludwigshafen, up its methanol-to-olefins (MTO) unit during a
Germany; www.basf.com) inaugurated its new 10-day test to confirm successful operation.
mobile-emissions-catalysts manufacturing site When the full unit goes online, it will have
in Chennai, India. The site includes a new a production capacity of 833,000 m.t./yr,
Look for more 47,000-m2 production plant, which replaces reportedly making it the largest single-train
latest news on an existing BASF plant in Chennai, and is the MTO unit in the world. The facility utilizes UOPs
chemengonline.com culmination of a three-year expansion project, process technology and catalysts.
Mergers & Acquisitions Packaging Technologies (Cambridge, Germany; www.covestro.com) has
Evonik and Royal DSM form JV Mass.) business for $1.05 billion. Darex agreed to sell its North American
for algae-based omega-3 fatty is a supplier of high-performance spray polyurethane foam business to
acids sealants and coatings that generated Accella Polyurethane Systems LLC
March 8, 2017 Royal DSM (Heerlen, sales of around $300 million in 2016. (www.accellacorp.com). The sale is
the Netherlands; www.dsm.com) Darex operates 20 production sites scheduled to be completed in the second
and Evonik plan to establish a JV for in 19 countries. quarter of 2017. Financial terms have
omega-3 fatty acid produced from natural not been disclosed. Covestros spray
marine algae. The companies will build Covestro agrees to sell spray polyurethane-foam business is located
a commercial-scale production facility polyurethane-foam business in Spring, Tex.
in the U.S. at an existing Evonik site, February 22, 2017 Covestro (Leverkusen, Mary Page Bailey
which is expected to come onstream
in 2019. The JV plans to invest around
$200 million in the facility.
GE Water & Process Technologies

acquired by Suez and CDPQ for
$3.4 billion
March 8, 2017 Suez Environnement
S.A. (Paris, France; www.suez-
environnement.fr) and Canadian fund
manager Caisse de dpt et placement
du Qubec (CDPQ) entered into an
agreement to acquire GE Water &
Process Technologies (Trevose, Pa.;
www.gewater.com) from General Electric
Co. (GE). The transaction values GE
Water at approximately $3.4 billion.
CDPQ will hold a 30% stake and Suez
will have the remaining 70%.
Cepsa finalizes acquisition of

Abengoa biofuels plant
March 6, 2017 Compaa Espaola
de Petrleos S.A.U. (Cepsa; Madrid,
Spain; www.cepsa.com) formalized the
8-million purchase offer for Abengoas
biofuels plant in San Roque, Spain.
Abengoa started operations at the plant
in 2009, but stopped production in 2015.
According to Cepsa, the production
unit is due to be fully operative again
during 2017.
Synthomer acquires Industrial Solutions for the fertilizer industry

Perstorp Oxo Belgium AB
March 6, 2017 Perstorp Holding
AB (Malm, Sweden; www.perstorp.
Leading-edge
com) announced the sale of Perstorp
Oxo Belgium AB, Perstorps additives
fertilizer technologies.
operations located at its facility at Gent, To secure global food supplies, our engineers
Belgium, to Synthomer plc (Essex, at thyssenkrupp Industrial Solutions have been
U.K.; www.synthomer.com). The total developing leading-edge fertilizer technologies
and large-scale plants for over 90 years.
consideration for the sale of Perstorp www.thyssenkrupp-industrial-solutions.com
Oxo Belgium is 78 million.
Henkel submits offer to acquire

U.S.-based sealant company
March 2, 2017 Henkel AG & Co.
KGaA (Dsseldorf, Germany; www.
henkel.com) has entered into exclusive
negotiations with GCP Applied
Technologies to acquire GCPs Darex
Newsfront
The Spread of Nitrogen Fertilizers

As price margins tighten, ammonia and urea producers are diversifying their products, while
new catalysts and process improvements boost capacities and lower energy consumption
Haldor Topsoe
IN BRIEF
DIVERSIFICATION
SAVING ENERGY
NEW CATALYSTS
S
ince the start of shale-gas boom FIGURE 1. This facility in Tatarstan, Russia has a nameplate
capacity of 2,050 m.t./d of ammonia in a single train, and can
in 2012, the U.S. has been moving be operated to co-produce up to 668 m.t./d of methanol and
toward becoming an exporter of 1,382 m.t./d of ammonia using Haldor Topsoes IMAP Am-
fertilizer after decades of importing monia process
most of its fertilizers. New production plants
are beginning to come onstream some- in sustainable and energy-efficient production,
thing the country has not seen for 35 years. in part driven by stricter environmental regu-
The startup of new large facilities in major lations. Currently, three new ammonia plants
importing nations, like the U.S., Indonesia and are under construction that will use Topsoes
a few in Africa has created tremendous price SCR [selective catalytic reduction] technology
pressure in the ammonia market in the west, that limits the NOx emissions to ultra-low lev-
says Viswadeb Ganguly, director of Technol- els below 20 parts per million by volume.
ogy, Ammonia & Syngas, KBR, Inc. (Houston;
www.kbr.com). Meanwhile, the Chinese ex- Diversification
port at a very low price has created the same New requirements for diversification have
impact in urea processes in Asia, he says. increased the interest in Topsoes IMAP (In-
With quite a few new plants expected to tegrated Methanol & Ammonia Process) so-
come onstream in 2017 and 2018, it will take lution for co-producing ammonia and meth-
some time for prices to improve significantly. anol, says Kjul Hoffmann. The IMAP portfolio
In the last 23 years, the market has been of processes provide varying ranges of flex-
characterized by oversupply of urea and de- ibility between ammonia and methanol pro-
clining nitrogen prices, says Merethe Kjul duction tailored to the market needs. The
Hoffmann, technology marketing manager, IMAP process combines state-of-the-art
Haldor Topsoe A/S (Lyngby, Denmark; www. NH3 and methanol technologies in a way
topsoe.com). Producers have reacted by di- that minimize the emissions from the plant,
versifying their production, making specialty because all CO2 generated from the process
fertilizer, and revamping plants to improve ef- feed is converted to either urea or methanol,
ficiency and capacity, she says. Across the and all the process condensate is recycled
board, producers are increasingly interested back to process. Over 24 years, eight IMAP
thyssenkrupp Industrial Solutions
Exhaust
Plant air
Dedusting filter
Storage Scrubber
Ammonium tank Droplet separator
sulfate
solution
Granulation
Water
Scrubbing
PROCESS
additive
Fluidized-bed
granulator
Recycle
conveyor
Screen-
solution tank
PLANTS FOR
ing
Crusher
Steam
Coating
agent Ammonium
Air Coating sulfate
drum granules
Condensate
FIGURE 2. Launched last month, this patented process produces ammonium sulfate granulate using a
fluidized-bed process
plants (both revamps and grassroots for additives to make urea granulate
plants) have been taken into indus- containing sulfur either as elemen-
trial operation. The worlds largest tal S or as sulfate and will commis-
IMAP plant (Figure 1) was commission its first urea-ammonium-sulfate
sioned in 2015 in Tatarstan and was (UAS) plant in Russia this year. As an
the first grassroots fertilizer in the for- alternative to its FB granulation, the
mer Soviet Union in decades. company is also working with pastil-
Margins have become thin for lation technology in collaboration with
many producers, many of which are Sandvik Process Systems (Fellbach,
looking to sell a product with an edge, Germany; www.sandvik.com).
says Stephen Zwart, vice president Meanwhile, Shell Thiogro (www.
licensing, sales and services, Stami- shell.com/sulphur/thiogro) and Uhde
carbon B.V. (Sittard, the Netherlands; Fertilizer Technologies (UFT; www.
www.stamicarbon.com). That means uhde-fertilizer-technology.com), part
not just urea, but urea with other addi-
tives, such as sulfur or sulfate, micro-
of thyssenkrupp Industrial Solutions
AG (tkIS; Essen, Germany; www.
Hydrogenation
nutrients and others, he says. Also, thyssenkrupp-industrial-solutions. Solids blending / drying
applications for urea other than fertil- com), established a partnership to in-
izer are emerging, he says. tegrate UFTs FB granulation technol- Pharma, food, cosmetics
Ten years ago, 90% of the urea ogy with Shells Urea-ES (enhanced
manufactured was used for fertilizer; sulfur) technology, which was intro- Finechemicals
now its dropping to 80%, says Zwart. duced in May 2015. The two com-
This shows the growth of non-fertilizer panies successfully granulated Shell-
applications, he says. For example, developed Urea-ES emulsion in UFTs
the use of urea solutions, known as FB granulation pilot plant in Leuna,
DEF (diesel exhaust fluids), as deNOx Germany. Combining the two tech-
agents for SCR of the exhaust from nologies will enable the largest urea Your fast lane to
diesel-engines is now widespread in plants in the world to produce granu- advanced mixing technology:
the U.S., Europe and Brazil, taking off lated sulfur-containing urea (Chem.
in China, and is expected to grow in Eng., May 2016, p. 8). Phone: +1 201 825 4684
other regions as well, such as South- The advantages of Shells technol- Ext.: 205
east Asia and Russia, says Zwart, ogy have been combined with the fea-
usa@ekato.com
adding that Stamicarbon has applied tures of UFTs FB granulation process,
technologies in urea plants to produce where the granulation mode is accre-
DEF and improve operating margins. tion instead of layering. The elemental
Stamicarbons widely used urea sulfur liquor is finely dispersed in the www.ekato.com
fluidized-bed (FB) granulation tech- urea melt before the solution is fed to
nology appears to be very suitable the granulator. Just as in the normal

Stamicarbon team. We want to give already proven in installed plants, ac-
fertilizer manufacturers cording to tkIS, and the company says
NH3/H2O the opportunity to con- it is continuing to develop its technolo-
vert byproducts into high- gies further to make continuous prog-
NH3/H2O
quality nitrogen fertilizers, ress on minimizing energy consump-
Pre-evaporator / Medium-pressure
(MP) carbamate condenser which command pre- tion for ammonia production.
mium prices compared Similar efforts are underway for urea
with standard products in production as well, such as Stamicar-
Reactor crystalline form. bons newly developed Launch Melt
Urea The new patented Flash Design with improved energy
solution
Pool
condenser process (Figure 2) starts efficiency (Figure 3). With this de-
Flash with ammonium sulfate sign, the steam consumption in the
vessel
solution, an industrial by- urea plant is reduced by about 100
NH3
product occurring mainly kg/ton of final product by installing a
in the production of cap- small in-line flashing step between the
CO2 from compressor rolactam and in coal-fired synthesis loop and the traditional low-
Stripper
Low-pressure recirculation section
furnaces. (NH4)2SO4 is pressure stage, explains Zwart. This
mixed with an additive, concept has a better heat integration
FIGURE 3. This urea process is said to have reduced energy
consumption, and also lower investment costs due to a reduction in which results in greatly and reduces the investment cost of
high-pressure equipment reduced dust forma- the high-pressure (HP) equipment,
tion during granulation becoming smaler in size, and some of
urea granulation, the Urea-ES particles and high crushing strength in the end them dispensed with entirely, he says.
grow collectively through the solidifica- product. In a second step, the liquid Stamicarbons latest process scheme
tion of tiny droplets on the seed mate- mixture is sprayed into a FB granulator for the Launch Melt Low Opex de-
rial. The result is a very hard granule. and processed into solid granules. The sign (Figure 4; online version at www.
Last September, OCP (www. product from the granulator is taken to chemengonline.com) allows for steam
ocpgroup.ma) and Shell signed a a screen. Oversize pieces are crushed consumption to be reduced down to
strategic agreement regarding the and returned to the granulator together around 550 kg/ton of final product.
license of Shell Thiogro technology. with undersized particles. Then the
The Shell Thiogro technology will be product is conveyed to a storage fa- New catalysts
installed at OCPs Jorf Lasfar site in cility. The granules are round and very Catalysts have always played a
Morocco, enabling the company to hard and therefore very resistant to im- major role in the production of syn-
expand its portfolio by incorporating pacts and abrasion. thesis gas (syngas; H2 + CO), the
elemental sulfur into its existing am- Following successful laboratory water-shift reaction to make H2,
monium phosphate, NPKs (nitrogen, and bench-scale tests, tkIS built a and the ammonia synthesis itself.
phosphorus, potassium) and current pilot plant in 2016 with an initial pro- Because all of these reactions are
sulfur-enhanced products. The tech- duction capacity of 500 kg/h. Here energy intensive, it is not surprising
nology is expected to be installed too all the tests have been success- that catalyst suppliers continue to
and commissioned in 2017. ful so we can now scale up the pro- improve catalysts to have higher effi-
In a related development, tkIS intro- cess to industrial scale with capaci- ciencies, longer lifetimes, lower pres-
duced at the recent Nitrogen + Syn- ties between 5 and 20 metric tons sure drops and so on.
gas conference (February 27 March per hour (m.t./h), says Mathiak. Steam-reforming catalysts. Last
2; London, U.K.) a new granula- month, for example, Clariant (Mut-
tion process to produce ammonium Saving energy tenz, Switzerland; www.clariant.com)
sulfate granulate. The new plant type Technology providers for ammonia introduced a new generation of high-
produces a sulfur-containing nitrogen and urea production are continu- performance catalysts for the steam-
fertilizer in granular form from byprod- ally working to improve capacities reforming process in the production of
uct ammonium sulfate solution. The through process refinements. The H2, NH3 and methanol. The new Re-
process offers fertilizer manufacturers ammonia technology has continued forMax 330 LDP Plus and ReforMax
major advantages: firstly, much greater to improve in energy consumption, 210 LDP Plus catalysts are designed
cost efficiency compared with con- unit reliability and ease of operability, with a unique and innovative eight-
ventional processes producing granu- says KBR s Ganguly. KBRs propri- hole flower-like configuration that en-
lar (NH4)2SO4 from NH3 and H2SO4, etary cryogenic Purifier process can sures an extremely low pressure drop
and secondly improved spreading and increase plant capacities by up to in the tubular reforming reactor while
mixing properties compared with crys- 50% and, combined with other im- offering outstanding catalyst activity
talline products, says the company. provements, can reduce plant energy and selectivity, says the company.
Demand for granular ammonium consumption, says the company. The shape of the catalyst, used for
sulfate exists all over the world, ex- Extensive concepts have been de- primary reforming, plays a key role in
plains tkISs Jens Mathiak, who devel- veloped to minimize energy consump- the catalysts activity, heat transfer,
oped the new process together with his tion, which are readily available and pressure drop and physical strength.
The new ReforMax LDP Plus catalysts offer optimized
shape parameters. Compared to its ten-hole predeces-
sor, the new eight-hole floral design of ReforMax LDP
Plus allows a pressure-drop decrease of up to 20%,
says the company. This allows plant operators to signifi-
cantly reduce energy costs or increase the reformer gas
throughput (or both) in existing plants.
Moreover, the new catalysts retain the very high geo- Visit us!
metric surface area of Clariant's well-known ReforMax interpack, Dsseldorf, Germany
LDP ten-hole catalyst series, thus maintaining high ac- May 4 10, 2017
tivity for the steam reforming reaction. Heat transfer is Hall 12, Stand E37
improved thanks to increased hole diameters. Particu-
larly when used together, ReforMax 330 LDP Plus and
ReforMax 210 LDP Plus effectively suppress carbon
formation in the process, adds Clariant.
Another way to reduce pressure drop in steam reform-
ers is the Catacel SSR catalyst from Johnson Matthey
plc (JM; London, U.K.; www.matthey.com). In the Cata-
cel SSR system (Chem. Eng., March 2010. p. 11), which
JM acquired in 2014, alloy strip is formed into engineered
supports called fans, which are coated with a nickel-
based steam-reforming catalyst. The fans are stacked
inside of the reformer tubes. This design offers many ad-
vantages over traditional ceramic pellets, and provides
lower pressure drop, high heat transfer and high activity, SOME THINK
says the company. Introduced several years ago, Catacel
SSR is said to represent the single biggest step forward
when it comes to the development of catalyst shape.
A 90%
Compared to standard pellets, Catacel SSR leads to a
20% decrease in pressure drop. The value of increased DECREASE
efficiency when exchanging an old catalyst with a new
optimized one can normally pay for the optimized catalyst
charge within 12 yr of operation, says the company.
IN ENERGY
Shift catalysts. In February 2016, Clariant introduced the
Low Temperature Shift (LTS) chloride guard ShiftGuard USE WILL
200 into the market. ShiftGuard 200 effectively adsorbs
and retains chlorides a typical catalyst poison in an
NH3 or H2 plant so that the downstream main LTS cat-
COMPROMISE
alyst, such as Clariants ShiftMax 217, is fully protected.
In September 2014, Clariant also launched ShiftMax THROUGHPUT.
120 HCF, an enhanced high-temperature shift (HTS)
catalyst that avoids health and safety risks in NH3 or H2
production because it contains essentially no hexava-
WE THINK
lent chromium (Cr6+), says the company (for more de-
tails, see Chem. Eng., October 2014, p. 14)
Last year, Topsoe launched a new high temperature
DIFFERENT.
shift catalyst SK-501 Flex, which uses a promoted mag-
nesium/aluminum spinel structure instead of the tradi- At BEUMER we have a reputation for making things
tional iron/chromium structure. It removes the steam-to- a little different. Take the stretch-lm pallet packaging
carbon ratio bottleneck and lets NH3 producers save on system, BEUMER stretch hood. In a sector where
feedstock and energy or boost production by up to 5% energy-intensive shrink hooding is still common, BEUMER
in their existing set-up. The new catalyst also eliminates stretch hood uses a non-thermal stretch-lm system.
the risks related to Cr6+, both to the environment and The result: better load stability, higher throughput, up to
plant personnel, says Topsoes Kjul Hoffmann. 10 times less lm consumption and 90% energy savings.
NH3 synthesis. In 2014, Topsoe introduced the KM 111, All this makes a big difference to productivity and to the
an NH3 synthesis catalyst optimized for the lower beds of environment.
the converter with a high concentration of NH3. KM 111 For more information, visit www.beumergroup.com
lifts the performance of the NH3-synthesis loop significantly
and improves energy efficiency, says the company. n
Gerald Ondrey
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM Circle 05 on p. 78 or go to adlinks.chemengonline.com/66427-05

Newsfront
The Future of Safety Sensors

is Here Now
Wearable sensors enhance CPI worker safety and help close
the approaching skills gap
American Industrial Hygiene Association
IN BRIEF or many years, sen- FIGURE 1. Smaller, wireless sensors have the po-
THE FUTURE OF SAFETY
IS HERE TODAY
THE SUM OF THE PARTS
COLLECTING DATA
F sors have been used tential
in the chemical pro-
cess industries (CPI)
for many activities, includ-
ing monitoring the health
to change the health and safety paradigm
regarding collection of employee exposure data
THE FUTURE OF and safety of employees.

WEARABLE SENSORS In these applications, sen-
sors were especially helpful
PROCESS SENSORS when used to accumulate
USED FOR SAFETY
data on workers, identify
APPLICATIONS
potential exposures to haz-
ardous chemicals and to
monitor confined space
entry and dangerous inspec-
tions. However, many of the
sensors that were used for
these applications were
large and had to be carried
by hand or placed at a specific point within proper procedures and processes in place,
the plant or process line. More recently, the wearable sensors can now be placed on
advent of smaller, advanced sensor tech- all operators in a particular chemical plant
nologies and the ability to locate them in unit and set to alert workers when they
wearable items, such as helmets, smart enter an area of excessive exposure to
watches and smart glasses, and connect a particular substance. When the alarm
them to todays powerful communications triggers, the exposure is investigated and
infrastructures, all contribute to enhance the data points are captured in a central
the safety of CPI employees. repository and analyzed. It can then be
With the advent of smaller sensors and determined when, where and why the
microprocessors, monitors are becoming alarm triggered and the situation can be
compact and wearable. They are wireless, corrected in a virtually realtime manner,
so it is no longer necessary to have wires he says. Prior to advanced sensor tech-
that interfere with an employees work, and nology, we didnt have the opportunity to
they can transmit the information to the In- monitor all operators and identify the areas
ternet of Things or the cloud so that data of risk that operators were encountering
can be downloaded into a computer and on a task-by-task basis.
analyzed in real time, explains Russell Hay- Another game changer is the ability to
ward, managing director of Strategic & Tech- place arrays of these advanced, miniaturized
nical Initiatives with the American Industrial sensors around operating units and along
Hygiene Association (AIHA; Falls Church, facility fence lines and, during emergency
Va.; www.aiha.org). Smaller, wireless sen- response situations, link them to a commu-
sors have the potential to change the health nications infrastructure and provide virtually
and safety paradigm regarding collection of realtime data analysis. In these situations,
employee exposure data (Figure 1). the data can be used to make emergency
For instance, Hayward says, with the response decisions.
Upskill
The future of safety is here today
If this safety-enhancing sensor
technology, coupled with wearable
devices such as helmets, smart
watches and smart glasses, seems
like something that might be seen
in the future, think again. Its here
now and is slowly beginning to
make its way into the world of in-
dustrial processes.
For instance, Honeywell (Morris
Plains, N.J.; www.honeywell.com)
offers its Connected Worker solu-
tion, which provides safety intelli-
gence to reduce worker injuries and
prevent loss of life from man-down
scenarios. The solution collects and
provides sensor fusion, which refers
to data collected from a variety of
sensors on a worker that are com- FIGURE 2. The benefit of wearable technology, such as smart glasses, is that their hands are now free
so workers can keep their hands and eyes on the tasks at hand. This provides increased productivity, im-
piled to provide an accurate picture proved safety and better efficiency in activities throughout the facility and in hazardous situations
of what that worker is experiencing.
The solution monitors workers for managers and incident commanders erate a safer environment, so we tried
toxic gas exposure, breathing, heart the information needed to better an- to create a solution that would help
rate, posture and motion. The result- ticipate unsafe conditions and pre- them with that. It can help protect the
ing data and actionable intelligence vent potential man-down scenarios lone worker those in hazardous
are displayed remotely on a visual, that could threaten worker safety. areas or remote locations because
cloud-based dashboard, giving plant Employers are always trying to op- it uses the sensors and the connectiv-
DOWNTIME IS COSTLY
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exchanger tube repair requirements For more information visit cw-estgroup.com/ce04 EST Group

PROCESS SENSORS USED FOR SAFETY APPLICATIONS
I
f youre in the market to increase facility and employee safety but baths, pipe joints for chemical tanks or fluid levels, the safety applica-
arent ready to don wearable technologies just yet, experts sug- tion is in correcting the issue immediately and reducing the probability
gest looking outside the realm of safety sensors and into sensors of unnecessary future access into the hazard area.
that werent traditionally used for safety applications. Sensors such And, non-traditional sensors can be used in conjunction with safety
as those used for level and leak detection and tunable diode lasers sensors for further improvements. For example, when using machine
(TDLs) are currently being employed in chemical applications to avoid automation controllers, which integrate motion, robotics, safety vision
accidents and prevent processes from going out of control, keeping and sensing along with Omrons SQL database, a date and time stamp
plant and personnel safer than ever before. can be tracked. This information can be used to look for trends and
What were seeing is the application of sensors that were tradition- lead to design improvements, says Hull. For example, the liquid-leak
ally used for other applications being applied and related to the safety sensor may detect leakage on a cleaning device at a consistent time,
of not only the process, but the people around the process, as well, such as 4:00 PM, and the safety devices record that the interlocking
says Gene Cammack, director, System Product Marketing with Yok- safety switch is activated within 30 minutes of detection. Activating the
ogawa Corp. of America (Sugar Land, Texas; www.yokogawa.com). interlocking safety device puts the machine into a safe state. The data
For example, we are applying TDL analyzers into a lot of safety ap- could be a warning that a change elsewhere in the system might be
plications because it gives an open path that scans all the way across needed, she says. Perhaps there is a heating element too close to
the boiler to look for specific gases that may create problems with the cleaning station that either needs to be placed at another location
safety, he says. We hadnt really done that before, but its an excel- or it needs to be insulated. This type of change would then reduce the
lent application and now the TDL technology is having a moment as leakage pattern, and thus reduce the operators need to access the
a safety-related sensor, rather just in its traditional use for measuring hazardous area, and even increase production.
the content of the process. In addition, safety is further promoted because the devices are be-
Because the TDL technology shoots a beam across a space and coming more reliable thanks to self diagnostics, says William Sholette,
scans for specific gases, it is possible to set it to scan for gases such level product business manager for Endress+Hauser, Northeast,
as oxygen, carbon monoxide and hydrocarbons in a boiler. The sen- (Greenwood, Ind.; www.us.endress.com). There are more diagnos-
sor technology allows sight into different areas of a boiler that are tics inside the unit, such as watchdog circuits to make sure the micro-
more susceptible to buildups of gases, which can create fire or ex- processors are all working and communicating with each other, he
plosion hazards. Many of these areas couldnt be measured before, says. This is constantly done in the background and is monitored all
but because TDLs are a non-contact technology, the sensors dont the time so, if it fails or gets into a fault condition, a notification is sent
have to be embedded into the gas stream. So instead of using a point to alert users that something is wrong.
sensor, the TDL provides a broader look at whats happening inside, He adds that some companies, such as E+H, take self diagnostics
all the way across the boiler, making it much more advantageous to a step further in some sensors, such as the companys FTL 81-point
sensing the safety level in boiler, cracker or refinery application where level switch, and add a square wave signal onto the current so that it
explosions occur due to offgas in the electrostatic precipitators. is constantly modulating. The unit makes sure it can actually change
He adds that another bonus of the TDL technology is that the in- current by looking at the square signal. If it is modulating, the cur-
formation is provided in realtime, which traditional safety sensors for rent can obviously change, and therefore, it will change in a situation
these applications cant provide. This is why its a big deal in the where it needs to go into a fault condition, he explains. We are trying
safety world. to make these units, especially those used in personnel and process
Tina Hull, product engineering-safety, with Omron Corp. (Hoffman safety, more reliable and more responsible for themselves so they will
Estates, Ill.; www.omron.com) sees a similar trend. We are learning reliably signal if theres a problem that needs attention.
to apply a lot of non-safety sensors to detect activities or events that Its an interesting and evolving area as we try to figure out how
could potentially send a human into a hazardous area or situation, so to keep people and processes safe, especially as we scale back on
by applying more advanced sensors for things like leak detection and human resources and make things more automated, notes Cam-
motion, we are providing more benefits than safety sensors alone. mack. We have to ensure that safety is built into the systems and
For example, she says, detecting when a leak begins and correcting ensure that we maintain the sensors and other parts of the functioning
it quickly can reduce the probability of a slip or fall. While the sensors safety system. Everyone is trying to do more with less, but they dont
primary purpose is detecting leaks on applications such as measuring want to do it with less safety.
ity element to alert the worker that he that use sensor technology to con- provides critical sensor nodes within
or she may be in a dangerous situa- nect workers to realtime information the visual factory. Glasses and
tion and also gives an alert to some- and to each other (Figure 2). The wearables go everywhere hands-
one if the worker is in trouble. It also fundamental purpose is connecting, on employees go, so a tremendous
provides situational awareness in that keeping safe and providing informa- amount of data is generated by these
the sensors are consistently measur- tion to the hands-on workforce as operators, he says. Those data go
ing exposure limits and warning the they do their work, says Jay Kim, back into the system to make data
workers of danger. Theres a third chief strategy officer with Upskill. analysts and workers even smarter.
benefit around worker productivity, as The benefit of wearable technol- In addition, the wearables allow
the connectivity can be used to pro- ogy, such as smart glasses, is that information sharing. Shared informa-
vide information to the workers with their hands are now free so work- tion could include the actions and
instructions about work flow, says ers can keep their hands and eyes steps of safety procedures, such as
Prabhu Soundarrajan, Connected on the tasks at hand. This provides lock out/tag out. Another safety-en-
Worker leader, with Honeywell. increased productivity, improved hancing example might be the use of
Upskill, formerly known as APX safety and better efficiency in ac- what Kim refers to as a simple see-
Labs, (Herndon, Va.; www.upskill. tivities throughout the facility and in what-I-see scenario in which the
io) provides its Skyline platform, hazardous situations. number of people sent into a hazard-
which powers enterprise wearables Further, says Kim, the technology ous area can be reduced because
Vandrico Solutions
head-mounted displays, make sense
because it goes on the body, which
helps determine the realtime location
of the worker, if needed, and gets the
workers attention, says Gonzalo
Tuleda, CEO with Vandrico. With the
prolific use of smartphones, we all
have notification fatigue and tend to
ignore a lot of notifications. But a vi-
bration on the wrist or a flashing light
under a hard hat will get the workers
attention when needed. By combin-
ing the sensors that are in the mine
with a sensor on wearable technol-
FIGURE 3. Vandrico Solutions is exploring the use of networked sensors coupled with software solutions ogy, you can provide realtime safety
and electronic technologies to increase the safety of miners
alerts in an automated way.
remotely located experts could pro- increase the safety of miners (Figure
vide over-the-shoulder coaching to 3). One of the potential uses here The sum of the parts
an individual completing tasks in a would be to use sensors that are Advanced safety solutions such as
dangerous area using a front-facing able to determine shifts in rock and these are dependent upon several
camera on the smart glasses, rather seismic activity, which are linked to system components. According to
than sending the entire team in to software and wearable devices and Honeywells Soundarrajan, in most
complete the activity. used to send realtime alerts to work- solutions, advanced sensors are
And, Vandrico Solutions (Vancou- ers in an automated way. In min- used to measure the hazard, such as
ver, Canada; www.vandrico.com) ing, its often difficult to get signal a chemical parameter, gas or chemi-
is exploring the use of networked propagation, so one of the theories cal substance. That data gets com-
sensors coupled with software solu- we have is that wearable technology, municated from point A to point B
tions and electronic technologies to such as helmets, smart watches and via a communications infrastructure,

such as a bluetooth transmitter that it and then using that information Vandricos Tuleda agrees and says
takes the information to a cell phone to predict an incident before it hap- it is possible to take it a step further in
or wearable device or a WiFi network pens. The ability to alert users on the future: We have the opportunity
that takes it to a control room or the their mobile or wearable devices no- to capture the knowledge that the
cloud for storage. The communica- tifies them and allows them to react experienced workers have and the
tion infrastructure may also include to the situation quickly, which has the decisions they make given the data
location technology to track the lo- potential to save lives and millions of they are presented. We can capture
cation of the employee and sensor. dollars, says Soundarrajan. those data and use machine learn-
And the third component, accord- He adds that other software ad- ing algorithms to train artificial intel-
ing to Vandricos Tuleda, is software. vancements allow the software to do ligences, which allows us to make
Software is needed to help translate a good sum of the work traditionally a giant step toward the automated
information from the sensors and done by industrial hygienists. Today decision component of industrial and
the platform with which the sen- in industry, the data are often in silos, process operations, he says. The
sor is communicating. The software sitting in different systems, but using things smart sensors do reliably al-
should also have a logic component software that brings it all together lows us to tap into the knowledge
that is capable of analyzing the data from the data from the sensor level of trained, experienced people and
and making realtime decisions about that is associated with a worker all learn from their decisions what works
sending out alerts if set limits are the way to the enterprise systems. and what doesnt and then transmit
surpassed or an incident is about to This means the experts dont have that information in both directions
occur, says Tuleda. to do the crunching of data. Typi- into the system and into the hands of
In addition, software connects the cally, hygienists spend at least 8 to the worker in the field.
workers and the wearables to the 10 hours a week with Excel sheets,
IT infrastructure so they can access but todays technology can reduce The future of wearable sensors
the information they need, and also the burden of analysis. Regular re- Right now, such advanced technolo-
has the capability to connect work- ports are now available on demand. gies are in the early adoption stage
ers to the Internet of Things or WiFi In addition, those data are avail- with larger enterprises and, within
network to provide situational aware- able if an incident has occurred or those businesses, are mostly being
ness, says Kim. Software platforms if a regulatory agency requests a re- employed in critical applications.
connect the human interface to the port. Hygienists can pull that report However, early adopters are begin-
rest of the system, he says. in seconds, rather than crunching ning to see enough significant in-
numbers for 10 hours, he explains. creases in efficiency and safety that
Collecting the data In addition, software and stored many are moving the technology into
Prior to the use of advanced sen- data can be used to lessen the bur- full-scale operational settings. We
sors, sophisticated software might den of the ever-growing skills gap in are seeing not only early adopters
not have been as important because the process industry, says Upskills making excellent progress with suc-
there wasnt as much data. We were Kim. One of the biggest themes cessfully implementing this technol-
happy to have one or two data points we see in the industrial workforce ogy into real operational settings, but
per shift on an operator in a process is that there is a potential skills gap. we are also seeing them doing this
unit, says AIHAs Hayward. But with The baby boomers have become the faster than they have over the past
the advancement of todays direct- real domain experts, but as they are five or six years. The technology is
read instruments, it may be possible heading to retirement and millennials getting into the mainstream mindset
to capture one, two, six or more data are coming in to replace the work- of operational leaders in larger enter-
points per second. With that much force, the facilities are at risk of hav- prises, which means it will likely begin
data, it is becoming necessary to ing a tremendous loss of knowledge to accelerate with new customers at
identify or develop tools, techniques that wasnt captured in their digital a rate that is faster than it has been
and knowledge to analyze large data systems, explains Kim. Equipping in the past, says Kim.
sets in order to make good, useful, workers with wearable, connected Honeywells Soundarrajan adds
scientifically based decisions. devices enables easier capturing and that the chemical industry is show-
Honeywells Soundarrajan calls this sharing of that tribal knowledge and ing interest because they are con-
data with context. This is where the information. In some cases, it can be stantly pushing the envelope on
intelligence of connecting data col- as simple as recording a video of a safety. Sensing and connected sys-
lected by the sensors with software certain process and associating it tems are an excellent way to share
comes into play. We are develop- with a specific workflow. Once that knowledge and improve safety, he
ing software and successfully imple- is stored in the system, it can then says. And for the chemical indus-
menting software architectures that be made available to trainees and try, which is a risky environment, this
are capable of collecting data and employees who may not know how type of connected sensing technol-
reporting exceptions. to complete the task. This has the ogy helps make their world a much
Todays software is capable of col- potential to eliminate the expected safer place. n
lecting data, storing and analyzing knowledge and skills gap. Joy LePree
GO THINK
GREEN BLUE

Think Magnetrol .
To meet increasing regulatory,
environmental, social and bottom line
demands, rely on Thermatel TA2 for
your energy management solutions.
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magnetrol.com 1-800-624-8765 info@magnetrol.com 2017 Magnetrol International, Incorporated
Focus
Pipes, Tubes and Fittings

Esco Tool This pipe-milling end-prep tool Flat-faced seal replaces
is for beveling boiler tubes elastomeric O-rings
The Esco Wart Millhog (photo) is a The Parker Seal-Lok Xtreme line of
pipe-beveling machine that is de- flat-face seal fittings (photo) was re-
signed for making repairs to water- cently awarded a patent for its newest
wall boiler tubes. It features a rigid- addition a stainless-steel, flat-face
inner-dia. clamping system, and uses sealing ring that is designed for use
titanium-nitride-coated cutter blades with tube fittings in extreme- (high-
to machine carbon steel or highly and low-) temperature applications.
alloyed tubes without the need for The innovative metal seal features a
cutting fluids. The machine is able to unique trap-style seal with three re-
bevel, face and bore simultaneously, tainer clips that extend into the exist-
with relatively simple tooling changes, ing fittings O-ring groove and prevent
says the company, and it is designed the seal from falling out during assem-
to machine water-boiler tubes with bly or reassembly. It is said to provide
inner dia. from 2 to 3 in. The ma- an alternative to elastomeric O-rings
chine is sealed to prevent debris from in traditional O-ring face-seal fittings
entering the tool. It rigidly attaches that are not able to meet high- or low-
to the tube with clamps that fit the temperature or chemical compatibility
inner dia. and expand on the mandrel requirements of certain applications.
using a self-centering, draw-rod as- These metal seals can be used in ap-
sembly and attached wrenches. The plications from 328 to 1,200F (200
machine is available with both pneu- to 650C), while elastomeric O-rings
matic and electric motors. It is avail- seals are limited to a temperature
able for purchase or for rent. Esco range of 65F to 450F (54C to
Tool, Holliston, Mass. 232C). This seal is designed for liq-
www.escotool.com uefied natural gas (LNG) storage and
fueling systems, combustion turbines,
Drum pumps now offer a cryogenic applications, and other de-
broader choice of tubes manding CPI applications, according
These high-performance sealless to the manufacturer. Parker Hanni-
drum pumps (photo) are designed for fin Corp., Columbus, Ohio
transferring liquids from intermediate www.parker.com
bulk containers (IBCs). The pumps are
now offered with a choice of six tube Silicone hose is compatible
lengths. The newest tube length option with many clean applications
Michael Smith Engineers (137 cm; 54 in.) is available in several The APSW high-purity silicone suc-
materials (two polypropylene versions, tion hose (photo) now has a National
a polyvinylidene fluoride option, and a Sanitation Foundation listing (NSF-
stainless steel version). This variety of 51). The hose is designed for ultra-
wetted materials ensures resistance to pure water transfer, food processing,
the widest range of aggressive liquids beverage conveyance, washdown
and therefore maximum application stations, skid systems and other
flexibility, says the company. The other applications in the pharmaceutical,
key features of the PF Series drum biopharmaceutical, bioprocessing,
pumps include a sealless design that chemical and cosmetics industries.
is said to improve reliability, a double- The APSW hose begins with a liner
suction impeller that provides high-flow of low-volatile-grade, platinum-cured
and high-head capability (flows to 151 silicone. This liner is then slipped onto
L/min., and heads to 24 m), and easy a mandrel and wrapped with four
disassembly for cleaning. The tubes plies of polyester mesh fabric, 316
Parker Hannifin
are interchangeable with different stainless reinforcing wire and addi-
motor options. Michael Smith En- tional silicone. It is then cured into a
gineers Ltd., Sheerwater, U.K. smooth and uniform hose that can
www.michael-smith-engineers. handle both suction and discharge
co.uk applications. The hose is available in
Note: For more information, circle the 3-digit number on p. 78, or use the website designation.
New Age Industries
ity advantages for polyethylene
(PE) compounds that are highly
mineral-filled (to improve flame
retardancy) and used in wire and
cable insulation and jacketing ap-
plications, says the company. By
reducing screw torque, die buildup
and die pressure, the material can
improve extrusion throughput by
up to 110% compared to PE com-
pounds without a processing addi- PROVEN
smooth and convoluted-outer-diam- tive. The MB25-502 masterbatch
eter styles, can withstand tempera- enables wire and cable customers PERFORMANCE
tures from 100 to 350F, and may to maximize productivity without
be sterilized using several different paying a premium for unneeded
methods. New Age Industries, functionality, says the company. It
AdvantaPure Div., Southampton, Pa. raises the throughput of PE com-
www.newageindustries.com pounds with mineral loadings up to
70 wt.%, by reducing screw torque
Break-away coupling by as much as 30%. Lower torque, ROTOFORM
improves safety during tanker in turn, speeds production and cuts GRANULATION
loading energy costs. The silicone master-
Emco Wheaton
batch also avoids buildup on the FOR PETROCHEMICALS
die (and increased die pressure) AND OLEOCHEMICALS
that would require frequent inter-
ruptions for cleaning. The product
is compatible with low-density PE,
linear low-density PE, and cross-
linked PE, and it is supplied glob-
ally as free-flowing pellets. Dow
Corning, Midland, Mich.
www.dowcorning.com
The TODO TTMA 4-in. Aluminum Fittings now have Type 316
High productivity solidi cation of
Break-Away Coupling (photo) is de- stainless-steel options
products as di erent as resins, hot
signed to reduce the potential for The T&B Liquidtight Systems family
melts, waxes, fat chemicals and
damage and spillage and product of stainless-steel fittings (photo) for
caprolactam has made Rotoform the
loss during the loading and unloading stainless-steel flexible conduit has granulation system of choice for
of road tankers. The device has been added a new addition: SAE Type chemical processors the world over.
adapted for bottom-loading-arm ap- 316 stainless steel, a marine-grade Whatever your solidi cation
plications, and it can be used on new stainless steel with enhanced resis- requirements, choose Rotoform for
loading arms, or retrofitted into exist- tance to galvanic corrosion in food- reliable, proven performance and a
ing ones that currently use the same and-beverage applications and premium quality end product.
type of TTMA flange in their con- other particularly corrosive settings.
struction. It consists of two identical The design of these fittings has High productivity
halves joined together by a series of also been updated for improved on-stream factor of 96%
3-mm break pins allowing the device protection against liquid ingress. Proven Rotoform technology
to be configured to separate at a de- New features include the dome- nearly 2000 systems installed
fined load. Should an excessive load shaped gland nut that is unique in 30+ years
be placed on the loading arms, the to this family of products, says the Complete process lines or
pins automatically close the internal company, which prevents liquids retro t of existing equipment
valves, to protect the driver and the from pooling in the electric box. Global service / spare parts supply
environment. The device can then be And, the SafeEdge ground cone
reset onsite. Emco Wheaton USA, securely attaches to the conduit for
Houston improved pullout performance that
www.emcowheaton.com exceeds UL requirements, says
the company. Sizes range from
Silicone masterbatch 3/8 to 2 in., and they are available Sandvik Process Systems
Division of Sandvik Materials Technology Deutschland GmbH
improves polyethylene in 45-deg, 90-deg and straight Salierstr. 35, 70736 Fellbach, Germany
Tel: +49 711 5105-0 Fax: +49 711 5105-152
processability configurations. Thomas & Betts, info.spsde@sandvik.com
The MB25-502 silicone mas- Memphis, Tenn. www.processsystems.sandvik.com
terbatch provides processabil- www.tnb.com

Thomas & Betts Isolation joint improves safety tity. Full traceability of each compo-
of flanged pipe connections nent is maintained throughout the
The ElectroJoint monolithic isola- assembly process and is provided
tion joint replaces flanged-joint with detailed documentation. A
connections with a weld-in-place range of materials are available, as
connection, which is said to re- are numerous associated clamps,
duce human error, reduce corro- valves, adapters and connectors.
sion and increase safety. The iso- This ensures that these single-use
lation joint replaces bolts, sleeves tube assemblies are ready to use
and washers with a coated, sealed upon delivery, and meet the exact-
cathodic-protection system to ing requirements by cGMP manu-
eliminate corrosion, is secured facturing and validation standards,
with two butt welds, and is es- says the company. Watson-Mar-
pecially well-suited for smaller- low Tubing, BioPure Div., Wilming-
diameter pipes, including those ton, Mass.
used in gas-distribution lines, says www.wmftg.com
the company. Garlock Pipeline
Technologies, Houston These hoses are designed to
www.garlock.com deliver liquid cryogens
Viega This company offers a variety of
Cold-press connections for cryogenic transfer hoses, to en-
pipe installation are versatile sure the safe and efficient trans-
MegaPress and MegaPressG fit- fer of liquid crygogens, including
tings, such as reducers and unions liquid helium, liquid nitrogen, liq-
(photo), are easy to use, flameless uid argon and liquid oxygen. The
and provide secure, watertight hose options range from simple,
and airtight connections. These non-jacketed flex lines to vacuum-
fittings are FM-compliant for fire encased systems, for use in indus-
sprinkler applications and ASME trial settings, laboratory settings or
B31 compliant for pressure and as an instrumentation accessory.
boiler piping, and they are CSA Users can match the materials of
LC4 compliant for fuel -gas and oil construction to the cryogenic liq-
applications. The design reduces uid being transferred, and choose
buildup of joining materials, ex- from many options, including rigid
posed threads or tarnish, creating versus flexible hoses, and may
a clean, professional appearance, consider uninsulated, vacuum-in-
says the company. Since the sys- sulated or foam-insulated designs,
tem of fittings is flameless, it is to suit the needs of the application.
safer than traditional systems and The company also offers a range
eliminates the need for hot-work of components, such as, tanks,
permits. The system requires no valves, bayonets, and more, as well
welding rods or cutting oils. It can as custom system design. Cryo-
be installed under flow conditions, fab, Kenilworth, N.J.
making it ideal for maintenance www.cryofab.com
or emergency repair jobs and re-
ducing costly downtime, says the Handy tool lets users design
company. More than 200 Mega- pipe transits in the field
Press fittings, including elbows, Roxtec Transit Designer 4.0 lets
couplings, reducers, tees, reduc- designers and engineers envision
ing tees, threaded adapters, caps, and design pipe and cable rout-
flanges and unions, are available ing in the field, and it provides
in sizes from 0.5 to 2 in. Viega full documentation (ranging from
LLC, Wichita, Kan. certification to installation instruc-
www.viega.us tions). The latest improvements to
the tool include a product selector
Single-use tube assemblies are that helps users identify the right
designed for bioprocessing sealing solution for each applica-
The Puresu family of single-use tub- tions. Roxtec International AB,
ing assemblies provides a broad Karlskrona, Sweden
range of customizable configura- www.roxtec.com n
tions and components, which can Suzanne Shelley
be ordered with no minimum quan-
New Products
A compact compressor for Save time and water with this Kobe Steel
H2-refueling stations tank-cleaning machine

This company has started marketing The new TJ40G rotary tank-cleaning
the HyAC mini-A (photo), an all-in- machine (photo) uses a high-impact
one, compact compressor package jet stream to effectively clean tough
for stationary hydrogen refueling sta- tank residues and minimize the risk of
tions designed for use in the U.S. The product contamination. This four-noz-
HyAC mini-A consists of a high-pres- zle rotary jet head also cleans tanks
sure H2 compressor and a refrigera- 60% faster than static spray-ball tech-
tor sold together with a high-pressure nology, thereby increasing production
storage tank unit and a dispenser as a uptime. And because it cleans faster,
set. The HyAC mini-A has a footprint this new device uses less water and
10% smaller than the HyAC mini sold less cleaning agents which reduces
in Japan since 2014. The HyAC series operating costs by up to 70%, says
consists of two models: a single-unit, the company. The TJ40G is capable of
high-pressure H2 compressor, named handling tough tank residues, as well
HyAC, and a compact package con- as solids up to 1 mm in the cleaning
sisting of the hydrogen compressor fluid in tank sizes of 501,000 m. This
and other major equipment called the is particularly important for demand-
HyAC mini. To meet the U.S. fueling ing process lines, such as applications
protocol, the filling pressure of the within a brewery, where particles may
HyAC mini-A was raised to 87.5 MPa. be re-circulated in cleaning media be-
The HyAC mini-A is equipped with a fore completing the cleaning cycle.
remote monitoring system, and also Also, the units hygienic self-cleaning
includes compact micro-channel heat construction ensures that the flow of
exchangers called DCHE. Kobe the cleaning fluid reaches the exterior
Steel, Ltd., Tokyo, Japan surfaces of the rotary jet head, as well
www.kobelco.com as the critical interior components,
including all bushings, bearings and
This range of diaphragm inner surfaces. This minimizes the risk
pumps is extended of product contamination and ensures
Launched at this months Hannover high product quality. Alfa Laval AB,
Fair (April 2428), the hydraulic dia- Lund, Sweden
phragm pump Hydro/ 4 (photo) sup- www.alfalaval.com
plements this companys Hydro/ 2
ProMinent
and Hydro/ 3 types, thereby extend- Predict product performance
ing the application range to higher with a digital twin
capacities. The pump covers the ca- The latest release of STAR-CCM+
pacity range from 130 to 1,680 L/h at software, v12.02, includes several
7 to 25 bars absolute. The Hydro/ 4 new features to help product develop-
is equipped with a polytetrafluoroeth- ment organizations enhance and ac-
ylene (PTFE) multi-layer metering dia- celerate their ability to digitally simu-
phragm. The multi-layer diaphragm late and understand how a product
ensures safe and leakage-free me- will perform in the real world using the
tering. With material options includ- digital twin a precise virtual model
ing stainless steel, polyvinylidene of a products physical and perfor-
difluoride (PVDF) and Hastelloy C, the mance characteristics. New analysis
Hydro/ 4 can be used universally in tools combined with enhanced visual
numerous applications. As standard, realism enable STAR-CCM+ v12.02
all pump types are equipped with a to help users unlock deeper meaning
fixed-setting pressure-relief valve behind complex engineering simula-
that is integrated into the hydraulics tions. STAR-CCM+ v12.02 introduces
and a multi-layer diaphragm with a ray tracing capability that allows engi-
diaphragm-rupture warning system. neers to apply photo-realistic render-
The reproducibility of the metering is ings to their design and simulation
better than 1% in the stroke length results. In addition to providing new
range of 20 to 100%. ProMinent tools for the analysis of simulation
GmbH, Heidelberg, Germany results, STAR-CCM+ v12.02 adds
www.prominent.de capabilities to accelerate simulation Alfa Laval

Kral throughput for products that deal with A new anti-abrasive
reacting flows, such as furnaces, re- coating for insulation
formers, internal combustion engines Pittcote 16 coating (photo) is a new
and gas turbines. Siemens AG, low-temperature, anti-abrasive (LTAA)
Munich, Germany product that is designed for applica-
www.siemens.com tion with this companys Foamglas
insulation blocks, curved segments
Flow measurement at (PSG), half shells (PSH) and fitting
low temperatures covers. Pittcote 16 LTAA coating is
Components and assemblies are often a water-based, rubberized latex resin
tested in cold chambers at tempera- that provides a durable bore coat-
tures down to 40C. This company ing to insulation substrates and re-
can equip its Volumeter flowmeter duces abrasion from vibrating piping
(photo) with electronic sensors that or equipment. Due to its quick drying
are suitable for such low temperatures and brush/spray application capabili-
upon request. The upper tempera- ties, the product also reduces produc-
ture limit is 200C. For even measure- tion time and increases efficiency. The
ments in extreme cold, the special coating can be used on a wide range
advantages of the devices screw of service temperatures, from cold
measuring method offers advantages and cryogenic equipment to above
over other methods, such as gear ambient (up to 120C), allowing for
or Coriolis. In particular, the Volume- reduced inventory requirements.
ter offers a high measuring precision Pittsburgh Corning, Pittsburgh, Pa.
EM-Technik (0.1% of the measured value) and a www.pghcorning.com
measuring range of 1:100. This wide
measuring range makes it possible to This closed-system mixer
pass through the broad characteristic requires no transfer steps
curves during the functional testing of The VersaMix Multi-Shaft Mixer
hydraulic components. Kral AG, (photo) is designed for mixing pastes,
Lustenau, Austria creams and gel-type products, with
www.kral.at the capabilities of powder disper-
sion, emulsification, dissolution,
Automated switch for deagglomeration, homogenization,
multiple gas-analyzer lines heating, cooling and deaeration. All
Up to now, solenoid valves have been of these functions are achieved in a
used for switching between lines used closed system, without the need for
for measuring gases, but a consid- any transfer steps. The mixers three-
erable effort is required for servicing wing anchor, high-speed disperser
Pittsburgh Corning such arrangements in the event of a and high-shear rotor-stator arrange-
failure. This company has developed ment operate independently at dif-
an alternative a new, automated ferent speed ranges to deliver unifor-
measuring-point switch (photo). These mity in both low- and high-viscosity
point switches can be used in en- media. All product-contact surfaces
closed spaces, such as cleanrooms, are polished 316L stainless steel. The
and are located upstream of the gas mixer cover includes multiple ports
analyzers. The switch can monitor 8, for charging raw materials and the
10 or 16 measuring points. The device installation of a vacuum or pressure
clocks all active sampling boxes with transmitter, thermoprobe and tank
a pre-defined interval. In the event of light. It mates with a jacketed cone-
an alarm, the measuring points can bottom vessel that is designed for
be switched manually or individually 100% discharge through a flush dia-
in order to determine the exact loca- phragm valve. A 23-in. clearance from
tion of the gas emission. The auto- the valve outlet to the floor allows op-
mated measuring switch is equipped erators to position a bucket under the
so that eight measuring-point change- vessel to catch finished product after
over switches can be connected to the mixing cycle. Charles Ross and
each other. EM-Technik GmbH, Son Co., Hauppauge, N.Y.
Maxdorf, Germany www.mixers.com
Charles Ross and Son www.em-technik.com Mary Page Bailey and Gerald Ondrey
Facts At Your Fingertips
Gas Detection TABLE 1. COMMON GAS DETECTION TARGETS IN INDUSTRIAL SETTINGS
Department Editor: Scott Jenkins Gas name Gas properties and Exposure routes and IDLH1 level;
notes common symptoms and REL2
Detection of gases is a critical task Ammonia (NH3) Colorless gas with a pun- Inhalation, (ingestion for the aqueous 300 ppm;
in many chemical process industries gent, suffocating odor. solution), skin and eye contact TWA3 25 ppm
Often used in aqueous Irritation of eyes, nose and throat; diffi-
(CPI) facilities to avoid hazards to per- solution culty breathing; pulmonary edema
sonnel and to the environment. Gases Carbon dioxide Colorless, odorless gas. Inhalation (for liquid and solid forms, skin 40,000 ppm;
may present risks of explosion, flam- (CO2) Shipped as compressed, and eye contact) TWA 5,000
mability, toxicity, environmental pollu- liquefied gas. Solid form Headache, dizziness, paresthesia, dif- ppm
used as dry ice ficulty breathing
tion and displacement of breathable Carbon monoxide Colorless, odorless gas. Inhalation 1,200 ppm;
air. This one-page reference provides (CO) Shipped as compressed Headache, rapid breathing, weakness, TWA 35 ppm
information on common classes of liquefied gas exhaustion, dizziness, confusion
gas detectors and on commonly Chlorine (Cl2) Greenish-yellow gas with Inhalation; skin and eye contact 10 ppm;
monitored gases in industry. pungent, irritating odor Burning of eyes, nose and mouth, dis- 0.5 ppm ceiling
charge of tears, cough, nausea at any time
Chlorine dioxide Yellow to red gas (above Inhalation; skin and eye contact 5 ppm;
Gas sensor classes (ClO2) 52F) or red-brown liquid Irritation of eyes, nose, throat; cough, TWA 0.1 ppm
Gas-detection technologies can be with an unpleasant odor wheezing, bronchitis, pulmonary edema
classified according to the character- Hydrogen chloride Colorless to slightly yel- Inhalation; skin and eye contact; ingestion 50 ppm;
(HCl) low gas with pungent, ir- for solution 5 ppm ceiling
istics of the gases they detect: either ritating odor. Often found Irritation of nose, throat, larynx; cough, at any time
toxic gases or combustible gases, as aqueous solution choking; dermatitis
and most gas-detection technologies Hydrogen cyanide Colorless or pale-blue Inhalation, skin absorption, ingestion, skin 50 ppm;
fall into one of four broad categories (HCN) liquid or gas (above and/or eye contact Short-term only
78F) with a bitter, Asphyxia; weakness, exhaustion, head- 4.7 ppm
based on their mode of operation: almond-like odor. [Note: ache, nausea, vomiting; increased rate
electrochemical sensors and metal- Often used as a 96% and depth of respiration or respiration
oxide semiconductor sensors are solution in water.] slow and gasping
generally used to detect toxic gases; Hydrogen sulfide Colorless gas with strong Inhalation; skin and eye contact 100 ppm;
(H2S) odor of rotten eggs Irritation of eyes and respiratory system; 10 ppm ceiling
and infrared and catalytic sensors are apnea, coma, convulsions; conjunctivitis, at any time
used for detecting combustible and eye pain, discharge of tears, abnormal
explosive gases. visual intolerance to light, dizziness,
Electrochemical. Electrochemical headache, weakness, exhaustion
Phosphine (PH3) Colorless gas with a fish- Inhalation 50 ppm;
sensors are based on an electro- or garlic-like odor Nausea, vomiting, abdominal pain, chest TWA 0.3 ppm
chemical cell whose current increases tightness, difficulty breathing, muscle
when the molecule of interest makes pain, chills
contact with the sensing electrode. Sulfur dioxide Colorless gas with a Inhalation and skin and eye contact 100 ppm;
(SO2) characteristic, irritating, Irritation eyes, nose, throat; rhinorrhea TWA 2 ppm
The target gas may be oxidized or re- pungent odor (discharge of thin nasal mucus); choking,
duced at the working electrode, and cough; bronchoconstriction
a small, but detectable flow of elec- Nitrogen dioxide Yellowish-brown liquid Inhalation, ingestion, skin and eye contact 20 ppm;
trons is produced from the reaction (NO2) or reddish-brown gas Irritation of eyes, nose, throat; cough, 5 ppm ceiling
(above 70F) with a pun- frothy sputum, decreased pulmonary at any time
there. A measuring electrode and a gent, acrid odor. function, chronic bronchitis, breathing dif-
counter electrode are connected to ficulty; chest pain; pulmonary edema
the cell as well. 1 The term IDLH (immediately dangerous to life or health) is defined by the U.S. National Institute for Occupational Safety
Metal-oxide semiconductor (MOS). and Health (NIOSH) as exposure to airborne contaminants that is "likely to cause death or immediate or delayed permanent
adverse health effects or prevent escape from such an environment."
Metal-oxide semiconductors are 2 REL refers to recommended exposure limit, an occupational exposure limit that has been recommended by NIOSH and
based on the principle that gas ad- the Occupational Safety and Health Administration (OSHA) for adoption as a permissible exposure limit.
3 TWA is the time-weighted average, used to indicate the average exposure over a specified time period (usually 8 h,
sorption onto, and desorption from,
unless otherwise indicated)
the surface of a metal oxide changes
the conductivity of the material. When action, and the wiring resistance is of the light between the transmitter
target molecules contact a thin film changed by the temperature rise. and the receiver.
of high-surface-area sensor material, Typically, a bridge circuit is used to
the concentration of charge carriers indicate the resistance change. The Common detectable gases
(electrons or holes) changes, and the increased resistance compared to The table [1] contains information on
conductivity or resistivity is altered in a the resistance in clean air is used possible gas detection targets. n
measurable way. to indicate the gas concentration.
Catalytic. Most sensors of this type Infrared. Infrared sensors work via a References
work by catalytic oxidation, where the system of light transmitters and re- 1. National Institute of Occupational Safety and Health
(NIOSH), NIOSH Pocket Guide to Chemical Hazards, CDC,
combustible gas of interest comes ceivers. When combustible gases of www.cdc.gov/niosh/npg/default, accessed March 2017.
into contact with a catalytic surface interest come within the field of view 2. Fine, G.F. and others, Sensors, 10, pp. 5,4695,502,
(often platinum-treated wire coil) and of the receiver, a portion of the radia- 2010.
is oxidized. This releases heat of re- tion is absorbed, changing the power 3. Figaro Engineering Inc., Gas sensor technology, ac-
cessed March 2017, www.figaro.co.jp
Technology Profile
Bio-based Adipic Acid Production from Glucose
By Intratec Solutions
A
dipic acid is one of the most
Cyclohexane Two-stage oxidation Fermentation Glucose
commercially important ali-
phatic dicarboxylic acids. It
is produced on a large scale Phenol Hydrogenation + Adipic acid Fermentation Fatty acids
primarily to supply the nylon 6,6 pro- oxidation
duction chain. Other applications in-

clude the manufacture of coatings, Cyclohexene Hydration
Oxidation +
Glucose
hydrodeoxygenation
synthetic lubricants, fibers, plastics,
plasticizers and polyurethane resins. n Raw material n Pathway n Main product
FIGURE 2. Multiple production pathways exist for adipic acid

The process
In the process described in the fol-
lowing paragraphs, adipic acid is pro- is recycled to the hydrogen compres- Shifts in the hydrocarbon market
duced from glucose via a two-step sor. The reactors product stream is and growing environmental con-
catalytic process (Figure 1). expanded in a turbo generator, pro- cerns have resulted in the devel-
Glucaric acid synthesis. A glucose ducing electricity. Its low-pressure opment of alternative production
solution is mixed with process water output is directed to a knock-out routes for adipic acid from renew-
and heated before being fed to the drum in which a hydrogen-rich gas- able resources, such as sugar and
oxidation reactor. Oxygen is supplied eous phase is recovered and re- fatty acids (Figure 2).
to the reaction by feeding compressed cycled to the hydrogen compressor
air to the bottom of the reactor. The and a liquid phase, composed mostly Economic performance
overhead from the reactor is fed to of acetic acid, water and adipic acid, Using data from Q3 2013, variable
a knock-out drum, a liquid stream is is directed to a crystallizer. The out- costs (raw materials and utilities) for
recycled to the reactor and most of put from this crude crystallizer is then manufacturing fiber-grade adipic acid
the recovered gaseous material is re- filtered and fed to a rotary dryer to re- from glucose in the U.S. are estimated
cycled to the air compressor. The recover crude adipic acid. The mother to be around $1,100/ton of product,
actors bottoms product is cooled and liquor from the filter and the acetic accounting for a significant portion of
filtered, and glucaric acid is recovered acid evaporated from the dryer are the production costs.
as a solid. It is then fed to rotary dryers mixed and fed to an extractive dis- This column is based on Bio-based
to remove water. Dry glucaric acid is tillation system to remove the water Adipic Acid Production from Glucose
conveyed to the hydrodeoxygenation content from the acetic acid so it Cost Analysis, a report published
feed mixer. can be recycled to the hydrodeoxy- by Intratec. It can be found at: www.
Adipic acid synthesis. Glucaric acid genation feed mixer. Crude adipic intratec.us/analysis/adipic-acid-pro-
is dissolved in acetic acid and heated acid must still be dissolved in water duction-cost. n
before being fed to the hydrodeoxy- and then subjected to further crystal- Edited by Scott Jenkins
genation reactor. Glucaric acid reacts lization, filtering and drying to reach
with hydrogen at high pressure, yield- fiber-grade purity. Editors note: The content for this column is supplied by In-
tratec Solutions LLC (Houston; www.intratec.us) and edited by
ing adipic acid and water. The reac- Chemical Engineering. The analyses and models presented
tors overhead stream, a hydrogen- Adipic acid production pathways are prepared on the basis of publicly available and non-
rich stream, is partially condensed to Adipic acid production has been confidential information. The content represents the opinions
of Intratec only. More information about the methodology for
remove light byproducts, which are predominantly based on cyclohex- preparing analysis can be found, along with terms of use, at
burned as fuel. The gaseous stream ane and, to a lesser extent, phenol. www.intratec.us/che.
Process Offgas Acetic acid recycle 1. Oxidation reactor

water
RF 10 2. Air compressor
Glucose Offgas 3. Rotary drier
(70 wt.%) ST ST 11 4. Hydrogen compressor
5. Hydrodeoxygenation reactor
Acetic acid CW 12 6. Expander
1 CW 7. Crude adipic acid crystallization
8. Acetic acid recovery
Air Fuel 9. Crude adipic acid purification
8 Waste
2 water 10. Refrigeration system
5
RF 11. Steam boiler
12. Cooling tower
H2 7 9
Water recycle 3 4 6 CW Cooling water
Adipic
acid ST Steam
Hydrogen recycle RF Refrigerant
FIGURE 1. The production of bio-based adipic acid from glucose via a two-step catalytic process is shown here
3D Level Sensor Visualizes Material in Silo Under Pressure - how to safeguard high
Get x-ray vision! pressure processes
BinMasters 3D Scan- High Pressure ap-
ner is the ONLY level plications require
sensor to measure and special overpres-
map multiple points sure protection due
and create a 3D visual to the demanding
of the topography of process conditions
solids stored in silos. including pres-
Accounts for surface sures up to several
variations in lump thousand bar and
materials, granules, temperatures over
powders, akes, or 300 C which mainly occur in autoclaves. Related com-
pellets for accurate pressors face similar pressures.
inventory VOLUME of 1% to 3% of total stored volume.
REMBE HPRD rupture discs protect various high pressure
Models for high temperatures or with a Teon coating for
processes around the world. They were recently ap-
clingy materials. Multiple scanner systems for accuracy in
proached by one of the leading multinational companies
very large vessels. MultiVison software monitors all silos
to protect their polymer plant in Belgium and help to
with automated alerts. Minimal maintenance and works in
bring them in line with European regulations on pressure
high dust!
equipment.
BinMaster
REMBE GmbH Safety + Control
www.binmaster.com/products/info/40-3d
www.rembe.de
Circle 01 on p. 78 or go to adlinks.chemengonline.com/66427-01 Circle 02 on p. 78 or go to adlinks.chemengonline.com/66427-02
Dry Screw Vacuum Pumps for Solvent Handling Step up to the Vari-Flow Distribution Valve
Customers Internal Guide & Support
depend on System:
Tuthills experts The Vari-Flow Distri-
for sizing dry bution Valve has been
screw vacuum designed with a superior
pumps used in internal guide system that
solvent vacuum supports the stem and disc
systems. Tuthill providing support needed
offers the SDV series with variable pitch rotors for to allow the valve to be
reduced power consumption and lower exhaust tempera- used for balancing ow.
tures. Optional PTFE internal coating is available. The
Maintenance Free Opera-
KDP series with constant pitch rotors offers simplicity and
tion:
reliability, along with PFA coated internals standard. You
Manufactured from 304 stainless steel and UHMW plas-
can trust Tuthills experience and knowledge to identify
tic, which eliminates corrosion and maintenance concerns.
if a dry screw pump is the right choice for your applica-
Bushing assembly replaces easily from exterior, eliminat-
tion. With its environmentally friendly design and Tuthills
ing costly downtime.
complete solution offering, the decision to choose Tuthill
is easy. Positive Shutoff:
An improved gasket system allows complete (positive)
shut-off of the water stream without the persistent leaking
Tuthill Vacuum & Blower Systems associated with conventional valves.
https://www.tuthillvacuumblower.com/dam/2835.pdf Vari-Flow Products
www.industrialcoolingtowerservices.com/variowvalve.cfm

Cover Story
Part 1
Batch Drying With

Vacuum Contact Dryers
Drying is a demanding unit operation where solvents need to be removed without altering
product chemistry. Vacuum dryers are essential pieces of equipment for accomplishing this task
D
Eberhard rying solids is a de- Filling
Tritschler manding task that
Mixing/recondensing of solvents
Ekato Systems GmbH requires both knowl-
edge of process tech- Evaporation of Evaporation of
Heating free solvent bound solvent Cooling
nology and a sound mechani-
Discharge
cal design of the equipment
IN BRIEF used. This article provides an FIGURE 1. Batch drying processes typically consist of the components and
VACUUM DRYING overview of batch-drying prin- steps shown here
ciples and possible options for vertical vac- material without changing its original chemi-
BATCH DRYING
uum-contact dryers. cal composition. In essence, there must be
PROCESS
Most solids in the chemical process indus- no changes to the molecular structure dur-
EQUIPMENT OVERVIEW tries (CPI) are recovered by precipitation or ing the drying process and no derivatives
VACUUM DRYER DESIGN crystallization. The suspended solids are me- formed due to the drying process.
chanically separated by filtering or centrifug- A vacuum contact dryer is built to evapo-
DUST FILTER
ing in the first instance. In most solid-liquid- rate solvents from a solid by the use of the
SOLVENT-RECOVERY separation processes, thermal evaporation following physical and mechanical param-
SYSTEM does not compare favorably with mechanical eters: temperature; low pressure; and me-
PROCESS CONTROLS
separation by filtration or centrifugation with chanical fluidization by agitation.
respect to energy efficiency. However, when In most cases, vacuum contact dryers are
DRYING PROCESS STEPS it comes to the final moisture content, ther- restricted by the requirement that they not
CONCLUDING REMARKS mal evaporation is often the follow-up step to influence the chemistry of the product. How-
mechanical dewatering methods in order to ever, special processes are possible, where
achieve the desired dryness. the application of high temperature will initi-
The residual moisture content of the solids ate or control a chemical reaction.
after filtration or centrifugation is influenced The degree of residual moisture in the fin-
by the properties of the solids crystal struc- ished product is strictly related to the use
ture. A typical filtration cake can show resid- of the product and its specifications. Ex-
ual moisture content of between 5 and 45%. amples include the following: less than 5%
To dry a wet cake to lower values, thermal moisture for waste material for disposal;
evaporation is an effective way to achieve a less than 3% in foodstuffs for storage con-
true dry solids powder. siderations; less than 1% in herbal extracts;
For some products, continuous drying pro- and less than 0.1% in active pharmaceutical
cesses, such as belt and conveyor drying or ingredients (APIs).
spray drying, are suitable methods to achieve A vacuum contact dryer can achieve these
a dry powder in a single pass. While continu- values for the separation of solids from sol-
ous systems are not a subject of this article, vents and there are cases where the solids,
more information can be found in Part 2 of the solvents or both, are valuable products.
this Feature Report, Optimizing Analysis for
Spray Drying Processes (p. 43). Batch drying process
Almost all batch drying processes consist
Vacuum drying of the process steps mentioned in Figure 1.
During any drying process, all additives and Whether the steps are performed in a non-
solvents have to be removed from the solid agitated tray or in an agitated vessel, the con-
cepts discussed here for evaporation and Dust filter
re-condensing and collecting the solvents are
the same.
Each process step in batch drying has in-
dividual issues that require special attention:
Filling. During filling, factors such as the use
of gravity or force (pumping), as well as the
need for a contamination-free transfer into
the dryer will have to be addressed.
Heating source
Mixing. In order to create an even tem- Solvent recovery system
perature and solvent-concentration dis-
tribution in the bulk material, as well as to
support the outflow, mixing is mandatory in
the dryer. However, the influence of shear
forces created by the mixing action on the
solids needs to be addressed. Vacuum dryer
CIP system
Re-condensing. Whether the purpose of
the drying is to retain the dry power and
discard the solvent, or vice-versa, is deter- Evaporation of bound solvent. Some sol- FIGURE 2. Vacuum drying
mined by the user. Re-condensing and col- vents tend to stick to the solid particles by systems require several
pieces of key equipment
lection of the solvents is a demanding task physical bridging, or to hide in the pores of
in the process. the particle structure, while others dont. In
Evaporation of free solvent. The solvent order to predict required process times, de-
selection dictates the evaporation condi- tailed knowledge of the separation behavior
tions (enthalpy) and the maximum tempera- is critical.
ture limits of the solids dictates the thermal Cooling. For safe discharge, it might be
limitations for the drying system. required to cool the solids to very low tem-
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TABLE 1. EXAMPLES FOR IDENTIFYING PROCESS LIMITATIONS a closed loop is the appropriate method
for transporting the energy from the heat
Product Process Solvent Vacuum Max. temperature
level source to the dryer vessel. For thermal flu-
ids, water, water-glycol mixes or thermal oils
Polymers Post treatment Water Med. (50 High (300C)
mbar abs) are common.
For its high specific-heat capacity, water
Pigments/flame Vacuum drying Water, organics Med. (50 Average (80100C)
retardants mbar abs) is the first choice as a thermal fluid when the
temperature needs to stay below 150C. At
API Post drying Water, organics Low (8 Low (40C)
mbar abs) process temperatures above 150C, ther-
mal oil becomes more feasible, since oil
shows only a marginal pressure rise at el-
peratures prior to discharge. Since the heat evated temperatures.
removal from a dry power is subject to even Whether the closed loop is driven by one
lower heat-transfer coefficients, the cooling heat exchanger for heating and one heat ex-
step might be time consuming. changer for cooling, or the system is fed by a
Discharge. While fluids or suspensions drain centralized plant heating and cooling system
well from a vessel, draining a dry powder can is to be decided based on the site condi-
be a challenge. Residues after draining are tions. Proper sizing is important.
lost in most instances and reduce the cost Prior to any equipment selection, the physi-
efficiency of the dryer. cal limitations for the process need to be de-
In addition to the aforementioned basic refined by the process owner. Each and every
quirements, supplemental codes and stan- process has special demands, including (but
dards, such local laws, pressure vessel regu- not limited to) the three examples in Table 1.
lations, good manufacturing practice (GMP)
rules, pharmaceutical standards, U.S. Oc- Vacuum dryer design
cupational Safety and Health Administration The majority of commercially available vac-
(OSHA) requirements and explosion protec- uum contact dryers are built according to the
tion measures have to be considered. same principle: a jacketed vessel either
horizontal or vertical with a wall-wiping
Equipment overview agitator. Vertically oriented dryers can take
The following section is intended to identify advantage of gravity to influence product
the key components of a vacuum drying sys- flow (Figure 3). Vertical vacuum-contact dry-
tem (Figure 2). ers include the following:
Heat source. With respect to the heating An upright cylindrical vessel with a filling-
source for the dryer, available site utilities, to-height diameter ratio designed for bulk
as well as product specifications have to be mixing
considered. While a supplier of aluminum pig- A cone bottom to support the outflow of
ments might ban water as a heating fluid for solids
fire hazard reasons, an API producer might A jacketed to suit the selected heating
avoid thermal oil to avoid contamination risks. system
Both are secondary aspects, not directly re- A top-entry agitator, designed for solids
lated to the physical operation of heating. applications (re-starting in settled solids)
The base specification for a dryer heating Valves and safety applications to operate
system should consider the following: a pressure vessel
Provide a sufficient amount of heat Solids impellers circulate the entire con-
(Joules) in an energy efficient way tents of the vessel from the gravity filling until
Provide measures to keep a constant the gravity discharge. The impellers can be
temperature in the system hydrofoil type, designed to create maximum
The correct heating power and capacity flow with the lowest possible power input.
calculation has to consider the following: Energy balance is important. Mixing power
Initial heating of all wetted components by the impeller equals the power into the pro-
(equipment) within a reasonable amount cess. In a temperature-sensitive process, ex-
of time cessive mixing power input might disturb the
Provide sufficient energy to heat the prod- fragile temperature balance in the product.
uct load to the operating temperature The key feature of all agitators in a vacuum
Provide sufficient energy to evaporate the contact dryer is an agitator system that op-
solvent load at the given conditions erates with minimum wall clearances and
Compensate for energy losses wipes the full wetted surface of the vessel.
Maintain temperature Wall clearances from 5 to 15 mm are com-
In most cases, circulating a clear fluid in mon and feasible, and require both a pre-
cisely fabricated vessel and a deflec- ing systems that are properly designed
tion-free balanced impeller. to protect the solvent-recovery system
Since the process is typically operated from the dust.
under vacuum, the vessel must be fabri- Two types of commercially available
cated according to the American Society filter elements are discussed here, but
of Mechanical Engineers (ASME) Boiler others experience might include many
and Pressure Vessel Code (BPVC), and more systems.
must also follow local laws and regula- The dust-loaded area of the dryer is
tions, as applicable. separated from the solvent recovery line
by a gas-tight filter plate. This filter plate
Dust filter carries the filter elements. One possibil-
By heating a wet solid in the closed ity is a fabric bag filter mounted on a
vessel, evaporation will start. The sol- wire cage, while the other is a sintered
vents will be condensed in an external metal or wire mesh (10 m) cartridge
solvent-recovery system. This migration made of metal wire or metal fibers
of solvents will create a strong gas flow The selection of one of these filter
that may cause dust formation as the systems is based on owner preference
solids dry. and on the overall operating conditions
Commercially available solvent-re- (including temperature). While the fabric
covery systems are built for heavy duty bag filters are disposable and low in re-
services, but not for high amounts of placement cost, the metal cartridge is re- FIGURE 3. Vertical solids dryers can
dust. In order to prevent the plugging useable with a high lifetime expectation. take advantage of gravitational forces for
of lines or simply to keep the solids In both cases, proper sizing of the filter solids flow
where they belong, in the dryer vessel is critical. An undersized filter will lead to
a dust filter is installed on top of the an excess pressure drop in the solvent-
dryer vessel. recovery line, with effects on the total
Modern dryers feature heated filter evaporation regime.
domes with automatic blowback clean-
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TABLE 2. TYPICAL EVAPORATION TEMPERATURES FOR WATER insulating the vessel is recommended when
Water Pressure, mbar abs Boiling temperature, C
the system is installed at higher ambient
temperatures.
1,013 100
With respect to the cooling methods,
100 45 again the circulation of a clear fluid is one of
10 5 the first choices. Based on commonly used
solvents and the vacuum level achieved,
TABLE 3. TYPICAL EVAPORATION TEMPERATURES FOR ETHANOL anything from water (at 8C) to brine (at
15C) might be required. One item needs
Ethanol Pressure, mbar abs Boiling temperature, C
to be considered: water at 25C should not
1,013 82
be considered cold.
100 32 Collecting the solvents is the most precise
10 5 method for back-calculating the residual
moisture in the dry product. This can be
TABLE 4. TYPICAL DRYING BEHAVIORS done simply by measuring the solvent vol-
ume. A small amount of solvents, however,
System Step 1 Step 2 Step 3
might escape even a properly designed con-
Pigment drying Evaporate surface Transition Evaporate crystal denser. To catch the saturated solvents, a
moisture moisture bound in the
capillary second condenser in the exhaust line of the
vacuum pump might be required.
Comment High solvent load, low Dust emission starts Long duration, low
dust emission solvent load, dust
formation Process controls
All of the components mentioned in this ar-
Solvent-recovery system ticle require safe and precise operation. The
As the vacuum contact dryer evaporates large number of signals to be processed and
the solvents, the solvent-recovery system valves to be handled does not allow manual
needs to re-condense the solvent, usually operation of such a system, except situa-
at the same rate. There are many ways to tions involving small-scale tests in a labora-
achieve this objective. This article covers one tory environment. Automatic process control
method that has shown some advantages systems that focus on a proper temperature
when it comes to collecting the solvent for and vacuum regime are mandatory for in-
further use (Figure 4). dustrial vacuum drying.
A robust vacuum pump (liquid-ring pump
or dry-running pump) creates the initial low Drying process steps
pressure that will activate the process. Design As noted earlier in the article, an effective
criteria for the pump includes the following: drying process requires knowledge of the full
Evacuate the total system volume in a picture of the process, including filling, mix-
reasonable time ing, re-condensing, evaporation of free sol-
Maintain the vacuum level under changing vent, evaporation of bound solvent, cooling
process conditions and discharge of products
Compensate for air leakage across the full Filling. There are many ways of transferring a
system solvent-loaded wet cake into a dryer vessel.
Compensate for inert gas volumes intro- This could be the subject of an article on its
duced during the process own, covering all aspects such as contami-
In essence, the vacuum pump has to nation, operator exposure levels, explosion
keep the system running while also covering risks and dosing the correct amount. Some
FIGURE 4. The solvent-recov-
ery system recondenses the
for losses. dryers provide a wide opening at the top of
solvents as the dryer evapo- The key component of the solvent-recov- the dryer vessel where valves, dosing or con-
rates them ery system is the heat exchanger or conveying systems, including (but not limited to)
denser that is installed on the low-vacuum material-containment apparatus, can be in-
side of the pump. Properly designed and stalled. Gravity will support the filling process.
activated with the proper cooling fluid, sol- Mixing. During the filling process, the mixer
vents evaporated in the hot dryer vessel will may or may not run. However, it has to be
migrate to the cold surface of the heat ex- designed for re-starting in settled solids at
changer and will be re-condensed. any time during the process. Stalling dur-
Condensation on the vacuum side of the ing a drying process should be avoided. In
pump will result in a huge draft the con- some rare cases, however, stopping the agi-
denser acts as a vacuum pump. The liq- tator is even required to overcome a certain
uefied solvents are collected in a collection process condition. In essence, an off-the-
vessel for further use or transfer. Cooling or shelf agitator will not do the job. Dryer agi-
tators have to be designed for the purpose. 1000
The degree of mixing might or might not af-
fect the drying time. It is the task of the scale-
up engineer to predict the influence of the
Pressure, mbar abs

mixing on the drying behavior. Engineers must 100
gain this information in a small-scale test.
Re-condensing. Evaporation starts when Water
the solvent vapor pressure exceeds the
pressure in the vessel or the product tem- 10
Ethanol
perature exceeds the boiling temperature of
the solvent.
Since the heat transfer into a mixed solids
bed is difficult (because of low overall heat- 1
0 20 40 60 80 100
transfer coefficients of about 50 W/mK), Boiling temperature, oC
additional measures are required to increase
the system efficiency. Often the dry product reaching the goal of 5% solvent by weight. FIGURE 5. Solvent evapora-
shows temperature sensitivity, limiting the al- Based on the results of this chart, the fol- tion behaviors can be plotted
in graphs like the one shown
lowable heating fluid temperature. lowing parameters affecting the hardware here
In order to compensate for both, the are calculated:
limitations in heat transfer and heating tem- Required power consumption of the heat-
perature, working under vacuum is advised. ing system (amount of evaporation heat in
By lowering the pressure in the vessel, the relation to the time required)
boiling temperature of solvents drops. Typi- Required dust filter sizing, with respect to
cal evaporation temperatures for water and the solvent load over the evaporation time
ethanol are shown in Tables 2 and 3. Required vacuum condenser sizing,
Water has a vapor pressure of 1,013 mbar with respect to the solvent load over the
abs (~760 torr) at 100C, so its vapor pres- evaporation time
sure would exceed atmospheric pressure Each and every drying chart looks different
at temperatures higher than 100C and the for the great number of drying applications.
water starts boiling (Figure 5). However, they all give an indication about
If a desired solid product is water-loaded, typical drying behaviors and are divided into
but melts above 40C, it is advisable to en- three sections (Table 4).
sure that the heating-system temperature Discharge. When the process temperature
does not exceed 40C. The vapor pressure is equal to the heating temperature, this is
of water at 39C is 70 mbar abs. To avoid an indication that energy is no longer being
melting during the drying process, the pres- spent for evaporation, and the drying pro-
sure inside the vessel has to be set to less cess can stop. However, safety consider-
than 70 mbar abs. ations might not allow the discharge of a
Drying curve. Once the theoretical param- hot solid. In many cases, cooling prior to
eters have been set, a small-scale test is discharge to lower temperatures is manda-
recommended to gain sufficient information tory. Some dryer systems have the ability
about the exact drying behavior of the prod- to change the heating system to a cooling
uct. The following are characteristics for typi- mode. While the heat transfer for heating FIGURE 6. Drying curves
show the progression of sol-
cal small-scale testing of drying behavior: already has very low values, the values for vent content in the solid mate-
3-L scale: Yes/No-type testing with lim- cooling a dry powder are even lower. Cool- rial over the drying time
ited data collection for scaleup Moisture
25-L scale: best for free-flowing products; 45,00
results allow safe scaleup to plant size Line:
40,00
50100-L test: best for difficult-flowing loss of solvent based on
receiving vessel level
products; results allow safe scaleup to 35,00
Process moisture, wt. %
production scale 30,00 Dots:

loss of solvent by sample
During a drying test, in the first instance, 25,00 taking and analyzing moisture
proof that the agitator is suitable to move the
20,00
product is mandatory. All process-related
parameters must be collected in order to 15,00
generate the drying chart, a plot that shows 10,00
y = 42,725e-0.019x
the progression of the solvent content over 5,00 R2 = 0,9846
the drying time (Figure 6). y = -0,0132x + 6,9559
0,00 R2 = 0,9398
For this example process, the solvent 0 20 40 60 80 100 120 140 160
evaporates at an almost constant pace until Time, min.

ing the dry solids will consume additional the values deviate from one another
production time. In addition, the stain- A factor to account for the influence of
less-steel mass of the dryer equipment agitation speed on the evaporation
also needs to be cooled. In cases where If all data are available, safe scaleup by
time is of the essence, it might be benefi- a factor of 200 is readily achievable.
cial to separate the functions and transfer
the hot solids by closed pipe into a des- Concluding remarks
ignated cooling vessel directly below the The information included here describes
dryer. This procedure saves the energy the basic concept of a vacuum contact-
required to cool the equipment mass. drying system. This type of system can
Maximum yield after discharge is im- be applied to many chemical applica-
portant for the cost balance of the drying tions by designing the components ac-
system. In a single-product manufactur- cordingly. The following are some of the
ing process, leaving residues in the drying typical situations:
vessel for the next batch may be permit- Selection of wetted parts with respect
ted. However, in a typical pharmaceutical to corrosion (most commercially avail-
or fine chemicals process, cross-contam- able metals)
ination of products is banned. Designing the components for GMP
With a cleverly designed vessel and a standards (food and pharmaceutical
flexible agitator, the equipment can be industries)
made to suit the flow characteristics of the Designing the components for critical
product. A vertical vessel will, by nature, solvents, such as organic solvents
drain better than a horizontal drying vessel. Designing the components for severe
A cone bottom supports outflow far better site conditions (outdoor and weather
than a flat or dished bottom. The agitator protected)
must be in a position to rotate at elevated Designing the components for high
speeds, including the changing the direc- demands on cleanability (cleanroom
tion of rotation for discharge. Also, surface environment)
polishing and surface linings can help to Designing liquid cleaning systems
reduce friction as the solid product flows. (clean-in-place; CIP) for the dryer vessel
Scaleup. Scaling up a drying process Designing the components for out-of-
requires both small-scale testing capa- specification applications (high tem-
bilities and scaleup experience. Once peratures and pressures)
successfully dried at a 25-, 50- or 100-L Aside from plant experience and knowl-
scale, scaleup rules can be used to pre- edge of the process, cooperation with a ca-
dict the following: pable dryer company opens a wide range
Drying time of possibilities beyond vacuum contact dry-
Solvent load, energy demand ing. Applications include solvent extraction
Residues after discharge from herbs and spices; all-in-one reaction
Particle size changes due to shear on systems for paints and pigments; food pas-
the product teurization and drying; and all-in-one chem-
Wear of the agitator parts due to ex- ical reactor/dryers. n
posure to the product Edited by Scott Jenkins
As a basic rule, a safe scaleup requires
that the geometry of the small-scale test Author
dryer is geometrically similar to the pro- Eberhard Tritschler is product manager
duction-size dryer. for sales at Ekato Systems GmbH (Kp-
pelemattweg 2, 79650 Schopfheim, Ger-
Scaleup works best when the trials many; Phone: +49 7622-6907-808;
have been carried out under identical Email: eberhard.tritschler@ekato.com;
physical parameters (such as pressure Website: www.ekato.com). Tritschler has
served in sales and application engineer-
and temperature) as the full-scale pro- ing at Ekato Systems since 2005, and
cess. If this is not possible, correction prior to that, worked in sales and appli-
cation engineering at several other Ekato
factors have to be applied to the scaleup divisions. Tritschler holds a bachelor's degree in mechanical
formula. The scaleup rules consider the engineering from the Technical School of Engineering in Lr-
following items: rach Germany, and has also earned a degree in business ad-
ministration from the HWK School in Schopfheim, Germany.
The ratio of volume-to-heated-surface- Aside from his day-to-day business duties in the sales organi-
area of the small-scale dryer to the zation of Ekato Systems, Tritschler also speaks at customer
full-scale dryer seminars, tradeshows and business schools. He has special
expertise in the mechanical aspects of vacuum contact drying,
A temperature correction factor in as well as extractions and all-in-one reactions in batch-type
moving from small scale to full scale, if mixing vessels.

Part 2
Optimizing Analysis
for Spray-Drying
Precise control over spray-drying processes can be enabled by modern measurement
approaches that provide information on particle size and shape in realtime
Daisuke
Sasakura and
Fumiaki Sato
Malvern Instruments
Hayato Kato,
Shinya Kawaguci
and Yuichi
Misumi
Preci Co. Ltd.
FIGURE 1. Atomization technolgy is critical for spray drying processes. These photos show rotary atomizers (left), two-fluid IN BRIEF
nozzles (middle) and pressure nozzles (right) SPRAY DRYING
ADVANTAGES
T
he process of spray drying is ex- powder; subsequent classification ensures
ATOMIZATION
tremely valuable to a wide range of a closely defined particle size distribution. A TECHNOLOGY
solid-product manufacturers due spray drying process can be operated as ei-
to its ability to produce particles ther an open system, in which filtered air exits PARTICLE SIZE AND
with precisely controlled size and shape. to the atmosphere, or in a closed loop under SHAPE
Cutting-edge spray drying technology is inert gas, with solvent recovery, depending on LASER DIFFRACTION
used in industries ranging from food and the characteristics of the powder being pro-
CONTINUOUS PARTICLE
pharmaceuticals, to industrial materials, duced and of the original slurry or solution.
SIZING
metal powders and chemicals. Spray dry- Spray drying offers a number of significant
ing technology is typically selected for its advantages relative to other powder-produc- INCLUDING PARTICLE
ability to deliver standardized particles, so tion methods that give it broad commercial SHAPE
optimizing analytical strategies for process appeal. First, it produces highly spherical A MODERN APPROACH
monitoring is crucial to its successful imple- particles that consequently tend to have
mentation. Methods for monitoring spray excellent fluidity. It also delivers particles or
drying have developed significantly in re- granules with a sharp, stable and closely
cent years, with new technologies making defined particle-size distribution, offering
it easier to achieve precise control. In this a highly consistent output. Furthermore,
article, we look at those techniques that spray-drying processes can be operated
are proving particularly valuable, focusing continuously, minimizing the manual input
on online particle sizing and automated im- and potential for variability associated with
aging, a technology that quantifies particle batch processing (For more on batch dry-
shape, as well as size. ing, see part 1, Batch Drying with Vacuum
Contact Dryers, p. 36). These benefits bring
Spray drying advantages value in the manufacture of products as di-
Spray drying produces a dry powder from a verse as milk powder, vitamins, antibiotics,
liquid solution or slurry. The liquid is sprayed cosmetics, pigments, ceramics and metal
into a drying chamber in which air, or an inert powders including steel and rare-earth-
gas, drives off the solvent to leave a dried metal-based products.

produced. Reducing pressure increases the
median particle size of the finished powder,
OOS
while increasing it has the opposite effect.
Once the most suitable process technol-
Realistic process behavior ogy has been selected, optimization of the
Size
and fluctuations (example)

spray-drying process relies on the effective
Max manipulation of processing parameters and
of the properties of the feed solution or slurry.
Important feed characteristics include the
Min OOS
following: concentration, viscosity, specific
T = (sampling timing) T T T T gravity, additive content and inclusion, and
Process running time, T primary particle-size distribution. All of these
characteristics help determine the morphol-
FIGURE 2. This graph illus- Atomization technology ogy of the finished particles.
trates the benefits of improved In order to tailor the properties of spray-dried Potentially influential process parameters
control over spray drying
processes, including reduction materials to a specific application, it is im- include the following: the inlet and outlet
of out-of-specification (OOS) portant to select the most appropriate at- temperature of the dryer, the feedrate of the
material omization technology, and then to optimize liquid, and the air flowrate through the dryer
the process parameters that are available and nozzle, depending on the atomization
to exert control. Understanding the differ- technology used.
ent commercially available atomizing equip- Timely and informative particle character-
ment, and their method of operation, is a ization information drives the comprehen-
useful first step (Figure 1). sive optimization of these interacting pro-
Rotary atomizer. A rotary atomizer applies cess parameters.
the shear needed to break up the liquid solu-
tion into droplets via a rotating disc. Droplet Particle size and shape
size is controlled by the size and shape of The primary metric used to specify the prop-
the disc and, once the mechanical design erties of spray-dried particles is size, since
is fixed, by varying the speed of rotation. this has a defining influence on performance
This technology is most suitable for produc- and typically forms the basis of a product
ing particles ranging from 20 to 200 m in specification. The morphology of a particle
size, with the resulting products having high is directly linked to the fluidity of the associ-
sphericity and narrow particle-size distribu- ated powder, a prized characteristic of spray
tions compared to products generated with dried products. Generally speaking, smaller
other spray-drying equipment. particles flow less easily than those that are
Two-fluid nozzle. An alternative option for larger because interparticle forces of attrac-
atomization within a spray-drying process is tion increase with decreasing particle size.
a two-fluid nozzle. With this technology, the However, particle shape can also have a
energy required for liquid breakup comes marked impact. Irregular-shaped particles
from a flow of compressed gas, which is used can inhibit flow as a result of inter-particle
to drive two-phase flow through the nozzle. friction or interlocking; particles with a regu-
Droplet size is controlled by manipulating the lar shape more easily slip past one another,
compressed gas pressure (flowrate). An ad- thereby flowing more freely. When it comes
vantage of two-fluid nozzles is that they pro- to controlling spray-drying processes, par-
duce very fine particles, from around 1 to 20 ticle size measurement, though vital, is not
m, and offer a process with a small physical all that is required. Particle shape data can
footprint. However, a large quantity of com- also be extremely valuable.
pressed gas is required for operation.
Pressure nozzle. A pressure nozzle is an- Laser diffraction
other atomization technology used routinely Laser diffraction is used as a method for
in spray drying. A pressure nozzle atom- measuring particle size, and is usually the
izes the liquid simply by forcing it through preferred option in the majority of spray-
an orifice under high pressure. This tech- drying applications because it offers a num-
nology offers low operating costs and, via ber of important advantages over alternative
orifice selection, allows substantial scope methods. Laser diffraction is an ensemble
to vary the size of the granules produced. particle-sizing technique, generating volume-
Pressure plays an important role in defining based results for the whole sample rather
the atomization process, thereby directly im- than building up a size distribution from mea-
pacting the size of the droplets and particles surements of individual particles. As a result,
it is inherently fast. Laboratory-based mea- "Black box"
surements take less than one minute.
Laser diffraction generates particle-size Manufacturing
Raw material equipment Final product
distribution data from measurements of an-
gular variations in the intensity of light scat-
Analysis at lab
tered by a dispersed sample as it passes Analysis at lab "Prediction" "Prediction"
through a laser beam. Large particles scat-
ter intensely at relatively narrow angles to
the incident beam, whereas smaller particles "Not black box"
produce a lower intensity signal but at much
wider angles. Laser diffraction analyzers re- Manufacturing
Raw material equipment Final product
cord the angular dependence of the intensity
of scattered light using a detector array, and
from it calculate the particle-size distribution In-, On-, at-line
of the sample using an appropriate theory of particle analysis
light behavior typically the Mie theory.
The technique has a measurement range developed in a laboratory can be easily FIGURE 3. Realtime, continu-
of approximately 0.01 m to 3.5 mm, com- transferred into the manufacturing environ- ous monitoring enables the
assessment of quality of
fortably covering the size range of interest ment. Once a particle size specification is spray-dried products
for many spray-drying applications. Laser in place, realtime measurement helps to
diffraction can report over 100 class sizes, improve process control, making it easier
delivering excellent resolution for the precise to ensure that the process consistently pro-
detection of variations in particle-size distri- duces particles of the required quality. Fig-
butions. This technique can be automated to ure 2 shows how the data made available
reduce requirements for manual input to a by continuous realtime measurement allow
minimum, and to keep maintenance require- operators to robustly track process fluctua-
ments for laboratory systems to a minimum, tions and instantly see when the product is
while simultaneously increasing repeatability drifting out of specification (OOS). As a re-
and reproducibility. sult, they can adjust the process to rectify
a problem. This level of insight is not acces-
Continuous particle sizing sible to operators applying manual analysis,
The inherent speed of laser diffraction and an approach that can easily result in OOS
its amenability to automation have led to the material being included in the final product.
techniques successful commercialization as Furthermore, as well as improving manual
in- or on-line technology for continuous real- control, automated measurement provides
time particle sizing. Alternative realtime sizing an essential platform for fully automated
techniques include spatial particle velocim- closed-loop control, opening up a route to
etry, which determines the size of particles further efficiency gains. FIGURE 4. This process op-
present from measurements of the duration Figure 3 summarizes the fundamental shift timization test used a rotary
atomizer for the spray drying
for which they interrupt a laser beam. As al- in process operation that realtime measure- process and shows the effect
ready established, particle size is of crucial ment delivers. In simple terms, continuous of speed on resulting particle
importance in the spray drying process, so measurement makes it possible to assess size. The data suggest that
the availability of robust systems for realtime the quality of spray-dried particles as they a speed of between 6,000
or 8,000 rpm is sufficient to
monitoring can substantially enhance op- are being produced, rather than post-man- achieve the desired particle
tions for process optimization. ufacture, prompting responsive, remedial size of less than 50 m
An on-line laser diffraction analyzer system 1.6
can be easily integrated into the process and 1.4
will then automatically measure particle size, Alumina, water and PVA
% of particles at given size
1.2
providing a continuous stream of analytical
data with no manual intervention. Eliminating 1.0
the operator-to-operator variability associated 0.8

with manual analysis and sampling improves 0.6
repeatability and reproducibility, and the rate
0.4
at which on-line systems analyze data typi-
cally on the order of four complete particle- 0.2
size distributions per second is sufficiently 0.0
fast to track even rapidly changing processes. 10 100
CE diameter (m)
Because laser diffraction technology can Blue, 12,000 rpm, Dv50 = 36 um: Green; 1,000 rpm, Dv50=32 um
be applied from lab to line, specifications Black; 8,000 rpm, Dv50 = 53 um: Red; 6,000 rpm, Dv50=56 um

THE IMPACT OF SOLUTION VISCOSITY ON PARTICLE SIZE
The amount of shear applied to the liquid feed during atomization in a 2.4
spray-drying process is set by the design of the atomization technol- 2.2 Batch 1
ogy and by the process parameters, such as pressure. However, the 2.0
Batch 2
1.8
effect of that applied shear depends on the viscosity of the liquid. With 1.6
higher-viscosity solutions, the shear has less impact than with a lower- 1.4
viscosity feed. This means that, in the absence of any other change, an 1.2
%
increase in viscosity will result in an increase in droplet size. An alterna- 1.0
0.8
tive way of looking at this is that solutions of higher viscosity require
0.6
greater energy input to achieve successful atomization for an equiva- 0.4
lent droplet size. The example discussed here shows clearly how a 0.2
viscosity change can impact droplet formation and, consequently, can 0.0
0.1 1 10 100 1000 10000
affect the morphology of the resulting powder particles. CE diameter, m
Observing the impact of viscosity on the proper- TABLE 1. MATERIAL DIFFERENCES AND SLURRY VISCOSITY
ties of spray dried particles. Because spray-dried
Batch Dv50, m Slurry viscosity, mPas
materials are prized for their precisely defined proper-
ties, reproducibility is critical to the value of products 1 50 2,200
manufactured. The graph here shows data for two
2 39 350
batches produced under identical spray-drying condi-
tions. The particle size Dv50 for the resulting granules Differences in the material have a significant effect on the slurry viscosity, and the size of the product
for the two batches are 52 and 39 m, respectively.
Investigations into the reason for the observed difference in performance highlighted a marked difference in the viscosity of the slurry used
to produce each batch (Table 1). Though the stock solutions for both batches were produced by milling for identical periods of time using
identically sized balls within the mill, the ball-mill media material and weight were changed between the two runs. This led to a substantial
difference in the viscosity of the two stock solutions. The observed change in particle size is attributed to this difference. Establishing control
over the ball-mill charge conditions corrected this issue and delivered the consistent viscosity required to ensure reproducible manufacture.
action to address an issue. Realtime sands of individual particles in minutes

analysis directly enables better process and is a powerful technique for particle
control either automated or manual characterization. The resulting images
thereby increasing throughput, reli- are used to calculate number-based
ability and reproducibility, while at the particle size and shape distributions,
same time saving time and money by providing detailed, statistically relevant
eliminating any requirement for manual morphological analysis. Automated
measurements and control. imaging offers the major advantage of
allowing the user to view the particles
Including particle shape produced and, compared with manual
As mentioned previously, beyond size, microscopy, is faster and far less sub-
it is shape that defines the value of jective. The measurement range varies
spray-dried products, and that is con- from approximately 1 m to 10 mm.
FIGURE 5. Shape data show that although sequently a crucial consideration when When it comes to optimizing spray-
6,000 and 8,000 rpm are both sufficient selecting instrumentation for analysis. drying processes, automated imaging
for the production of appropriately sized
particle, the faster speed ensures more Automated imaging captures micro- is highly complementary to laser diffrac-
spherical particles scope-quality images of tens of thou- tion. It enables shape to be optimized
along with size, for example, to access
100 premium performance. Automated im-
90 aging can also be used for troubleshoot-
Alumina, water and PVA ing. The ability to quantify shape allows
80
70
for the more robust differentiation of
particles and can elucidate differences
60
in performance between similarly sized
%
50
products. Furthermore, the calculations
40 that underpin laser diffraction analysis
30 assume that the measured particles are
20 spherical, so results can be affected by
10 changes in particle shape. Automated
0 imaging makes it straightforward to
0.7 0.8 0.9 1.0 confirm that samples are adequately
HS circularity
Blue, 12,000 rpm, Dv50 = 36 um: Green; 1,000 rpm, Dv50=32 um dispersed prior to laser diffraction analy-
Black; 8,000 rpm, Dv50 = 53 um: Red; 6,000 rpm, Dv50=56 um sis so that primary particles, rather than
agglomerates, are measured, and detects erating conditions of interest to determine
changes in shape that may skew the particle those required to produce the target Dv50
size data generated. (median particle size) and the time taken for
The following real-world examples illus- the process to stabilize. The target Dv50 in
trate how laser diffraction and imaging in this case was 5565 m, but the level of
combination support the optimization of fines in the product was also a concern. The
spray-drying processes. ability of the on-line system to accurately
Case 1: Optimizing process conditions measure down to around 0.1 m was there-
with respect to particle size and shape. fore an important benefit.
Rotary atomizer technology was selected for Figure 6 shows that as the speed of rota-
the production of alumina particles and tests tion of the disk is stepped down, the particle
were then carried out to determine
the optimum speed of rotation of the
disk. The feed solution for the pro-
cess was a mixture of alumina par-
ticles, water and polyvinyl alcohol
(PVA), which was added as a binder Introducing the improved
within the suspension. In an initial
test series, rotary speed was varied
in the range 6,000 to 12,000 rpm
Sentry Saf-T-Vise
and the size of the resulting particles
was compared to the target speci-
corrosion monitoring
fication, which defined the required
Dv50 as being greater than 50 m.
products and services
From these results, a speed of rota-
tion of either 6,000 or 8,000 rpm was
identified as being suitable (Figure
4). A rotational speed of 6,000 rpm
The safest choice under pressure
is preferable from the perspective
of energy consumption. However,
shape analysis reveals that in fact, Sentry Saf-T-Vise Corrosion Monitoring
these two speeds are not equally products enable chemical engineers and
suitable in terms of the particle mor- field technicians to maximize production,
phology of the resulting particles. mitigate materials failure in pipelines while
Shape data show that the higher optimizing chemical usage. This patented
speed of rotation (8,000 rpm, rather
technology far exceeds the rest for operator
than 6,000 rpm) produces more
safety and ease-of-use even in extreme high
spherical particles that, because of
pressure conditions. The Saf-T-Vise portfolio
their shape, are likely to have su-
perior fluidity (Figure 5). Here then, has been redesigned and economically
shape data provide additional, valu- priced to accommodate pressure ratings
able insight into the liquid breakup up to 10,000 psi without any sacrifice to
process and its result, supporting safety. Its our contribution to the economic
process optimization to a more suit- recovery of the oil & gas industry.
able conclusion.
Case 2: Studying process dynam-
ics to define production condi-
tions. A further study of the impact
of disk-rotation speed on the size
of spray-dried particles produced
using a similar alumina-water-PVA
suspension to the one tested in
Case 1 was carried out using re-
altime size-monitoring technology,
an on-line laser diffraction particle Visit sentry-equip.com /corrosion to learn more.
size analyzer. Here, tests at differ-
2017 Sentry Equipment Corp. All rights reserved. All trademarks are the property of Sentry
ent speeds of rotation were carried
Equipment Corp.
out over a relatively short timescale,
simply by stepping through the op- Circle 25 on p. 78 or go to adlinks.chemengonline.com/66427-25

10,000rpm 8,000rpm 6,000rpm they are produced, to drive rigorous process
optimization and, ultimately, automated pro-
cess control. Beyond size measurement, au-
tomated imaging delivers statistically relevant
shape distribution data in minutes, providing
Transmission further insight for precise control of the prop-
120 um
erties of spray dried powders. Together, these
DV90 techniques support the effective application of
spray drying technology and its exploitation to
manufacture consistent products with well-de-
90 um fined properties and high value. n
Edited by Scott Jenkins
"Sweet spot" Dv50 References
1. Malvern Instruments Ltd., The Enduring Appeal of Laser Diffraction
Particle Size Analysis, Whitepaper, Malvern, www.malvern.com/en/
60 um support/resource-center/Whitepapers/WP110325EnduringAp-
pealLaserDiff.aspx, 2016.
2. Malvern Instruments Ltd., Real-time Particle Sizing for Granula-
Dv10 tion Control, Whitepaper, Malvern, www.malvern.com/en/support/
resource-center/Whitepapers/WP130226RealTimeParticleFor-
Granulat.aspx, 2016.
Authors
11:20 12:20 13:20 14:20 Daisuke Sasakura is a product specialist for
cross-product marketing at Malvern Instru-
ments (Enigma Business Park, Grovewood
FIGURE 6. Realtime measure- size of the resulting droplets increases, as ex- Road, Malvern WR14 1XZ U.K.; Phone: +44
ment makes it possible to pected. However, after each change, it takes 1684 892456; Email: salesinfo@malvern.com;
instantly observe the effect Website: www.malvern.com). Prior to his cur-
of decreasing the speed of a certain amount of time for the particle size rent position Sasakura served as product spe-
rotation of the atomizing to steady at a new a value. The realtime data cialist for analytical imaging at Malvern from
disk and the time taken for accelerate the assessment of different oper- 2011 to 2015. He holds a Ph.D. in analytical
the process to re-establish a science and vibrational spectroscopy from
steady state. (The green line
ating conditions but, at the same time, clearly Showa Pharmaceutical University.
represents Dv10, blue line is highlight the need to run for around 30 min- Fumiaki Sato is a product specialist for pro-
Dv50, orange is Dv90, red is utes to generate robust particle size informa- cess systems at Malvern Instruments. Sato
transmission) tion at each new speed. Equally importantly, has been with the company since 2013.
these data provide information as to when
a process change in a manufacturing plant
will feed through to a changed product that
can be securely collected as in-specification
material. The sweet spot for this process
is found to be a speed of rotation of 8,000 Hayato Kato is the CEO of Preci Co. Ltd. (2-
11-6 Taito, Taito-ku, Tokyo 110-0016 Japan;
rpm, which produces particles with the re- Phone: +81 3-3839-4540; Website: www.
quired Dv50 and an acceptable level of fines preci.co.jp.). Prior to becoming CEO, Kato
as quantified by Dv10 data (Table 2). served as strategic officer at Preci from 2008
to 2012. Kato holds a master's in business
administration in international business from
A modern approach Tsukuba University.
Spray-dried powders are prized for their fluid-
ity, shape and tight particle size distribution. Shinya Kawaguchi is chief of the Powder
Producing standardized, spherical particles is Technical Center at Preci Co Ltd. Prior to that,
Kawaguchi was manager of the sales team for
crucial and relies on exerting effective process the drying machinery department at Preci
control. Timely, relevant particle characterization from 2013 to 2016 and has worked for Preci
is essential. Commercial realtime particle sizing since 2012. Kawaguchi holds a bachelor's
degree from the Tokyo University of Science
technology makes it possible to continuously
monitor the quality of spray-dried powders, as
Yuichi Misumi is an application specialist in
TABLE 2. ATOMIZATION DISK ROTATION SPEEDS AND PARTICLE PROPERTIES powder manufacturing at Preci Co Ltd., and
10,000 rpm 8,000 rpm 6,000 rpm has been with the company since 2011.
Dv10 (m) 23.57 32.22 38.98

Dv50 (m) 44.71 61.38 71.78
Dv90 (m) 80.44 112.45 122.68
Span 1.27 1.31 1.17

Feature Report
Part 1
Crossflow Membrane
Filtration Essentials
Several aspects of crossflow membrane filtration , including process design, equipment
selection and control, are detailed here
A
membrane, also re- Feed Alan Gabelman
ferred to as a semi- Gabelman Process
Retentate
permeable mem- Solutions
brane, is a thin layer
of material that selectively
passes one or more com-
ponents of a feed solution or IN BRIEF
slurry, while retaining the oth- Permeate ADVANTAGES AND
ers. Biological membranes DISADVANTAGES
have existed since the dawn BATCH PROCESS
of time, but synthetic mem- Circulation pump FLOWSHEET
branes are of greater indus-
MF AND UF BASICS
trial importance. These were
first employed commercially FIGURE 1. Crossflow membrane filtration (CMF) differs from conventional filtration
in that feed flow is parallel to, rather than perpendicular to, the filtration surface
PRESSURE EFFECTS AND
in crossflow filtration opera- POLARIZATION
tions in the 1960s, and growth DESIGN
in the ensuing years was remarkably fast. sion that do lead to retention of dissolved CONSIDERATIONS
Today, crossflow membrane filtration (CMF) species, including adsorption onto the mem-
is a major unit operation that is pervasive in brane surface or the undissolved solids MEMBRANE MATERIALS
numerous industries. themselves. The relatively large pores char- MODULE
The concept is illustrated in Figure 1. Un- acteristic of microfiltration membranes are CONFIGURATIONS
like conventional filtration [1], feed flow is known as macropores. DIAFILTRATION
parallel to, rather than perpendicular to, the Like microfiltration, ultrafiltration (UF) oper-
filtration surface. During a given pass, only ates using traditional size exclusion, but with CONTINUOUS
a small portion of the feed permeates the smaller mesopores rather than macropores. OPERATION
membrane and becomes permeate, while While both UF and MF are used to remove MEMBRANE FOULING
a much larger portion is retained as reten- undissolved solids, UF membranes are also AND CLEANING
tate. Most of the retentate is returned for capable of separating large and small mol-
multiple passes, by the action of the circula- ecules in solution. UF membranes are de-
tion pump. This allows a high linear velocity, scribed by their nominal molecular weight
which imparts a shear to the membrane that (MW) cutoff (NMWC), which is a rough in-
helps to keep the filtration surface clean. The dication of the smallest molecule that the
valuable stream may be the permeate, the membrane will retain. However, because
retentate, or both.
As shown in Table 1, membrane pore size TABLE 1. CROSSFLOW MEMBRANE FILTRATION PROCESSES
varies considerably, with separation capa- Membrane process Separation Separation Transport regime
bilities from angstroms () to several microns mechanism capability
(m) in particle size. The relatively coarse Microfiltration Size exclusion 0.110 m Macropores
microfiltration (MF) membranes are used to Ultrafiltration Size exclusion MW 1,000500,000 Mesopores
g/mol
separate liquids from undissolved solids by Nanofiltration Size exclusion, elec- MW 100-1,000 g/mol Micropores
size exclusion, as in traditional filtration pro- trostatic exclusion
cesses. In principle, the liquid composition Reverse osmosis Solution/diffusion MW <100 g/mol Molecular
does not change, although in some cases Gas separation Solution/diffusion Molecular size Molecular
there are phenomena other than size exclu- ~0.0001 m

From CIP system tion area, or flux, obtained in the pilot
Diafiltration
water plant. Other advantages of CMF are:
Feed mild processing conditions (temper-
Steam (for ature, pressure); high product yield;
cleaning) Membrane module ability to operate as a closed system,
Feed/ reducing risk to personnel and the
retentate
tank environment when handling hazard-
Permeate ous materials; and the ability to tai-
CWR
lor membrane properties to match
Heat specific user requirements.
exchanger
On the downside, the capital cost
Drain Circulation pump of membrane plants is relatively high,
CIP: clean in place PI: pressure indicator
CWR: cooling water return PIC: pressure indicator-controller especially if exotic membrane mate-
CWS: cooling water supply T: steam trap rials are required. In addition, many
FI: flow indicator TI: temperature indicator
LIC: level indicator-controller TIC: temperature indicator-controller polymeric membranes are subject
FIGURE 2. Batch or semi-continuous crossflow membrane filtration processes can vary widely in com- to swelling in the presence of high
plexity, depending on the application
concentrations of organic com-
permeability depends on more than ions and surrounding water mol- pounds, and cannot be operated
just molecular size, exclusion of all ecules leads to hydrated structures at high temperatures. These chal-
molecules above a certain NMWC is that dissolve and diffuse much more lenges can be met with inorganic
unlikely. As a rule of thumb, for com- slowly than free water molecules. For materials or high-performance poly-
plete removal of molecules of a given this reason, the free water passes mers, but the cost is higher. Other
size, a membrane rated one-tenth through, while the ions are largely disadvantages include formation of
that size should be selected. Ultrafil- rejected. RO membranes are non- a polarization layer on the mem-
tration membranes are available with porous, meaning there are no dis- brane surface, which reduces flux;
NMWCs of 1,000 to 500,000. tinct pores that accommodate fluid fouling, requiring periodic clean-
This article focuses on MF and flow. The openings are the interstitial ing; and in some cases, significant
UF, except for a brief mention of the spaces between the polymer chains, dilution when retained species are
other processes listed in Table 1. and the transport regime is known washed to increase product yield or
Nanofiltration membranes contain as molecular because the size of remove contaminants a process
micropores that are tight enough these openings is of the same order known as diafiltration.
to separate very small molecules, of magnitude as the small molecules
such as monosaccharides from di- (nominally, molecular weight less Batch process flowsheet
saccharides. For neutral molecules, than 100 g/mol) that pass through A process flowsheet for a batch or
the principle is size exclusion, the these membranes. semi-continuous membrane filtration
same as in UF and MF, with NMWCs Finally, the tightest membranes are process (continuous processes are
of 1001,000. However, nanofiltra- those used for gas separations for discussed later) is shown in Figure
tion membranes can be functional- example, separation of air into nitro- 2. Please note that this is just an ex-
ized with charged groups, making gen and oxygen. These non-porous ample. Like any chemical engineer-
electrostatic interactions an impor- membranes also fall into the molecu- ing unit operation, CMF processes
tant factor in performance. Such lar transport regime, and pass mol- vary widely in complexity, ranging
membranes are used, for example, ecules on the order of 0.0001 m from completely manual to highly au-
to repel anions in wastewater treat- in size. tomated. In a batch process, reten-
ment applications. Nanofiltration is a tate is circulated through the mem-
relatively new classification before Advantages and disadvantages brane module then back to the feed/
the term was coined, these prod- The main advantage of crossflow retentate tank, where the volume
ucts were considered loose reverse membrane filtration is the shear im- gradually decreases, and the con-
osmosis membranes. parted to the filtration surface, which centration of the retained species
Reverse osmosis membranes reduces fouling by particulate matter increases, as permeate is removed.
were the first to see large-scale in- or retained molecules. Another ad- In a semi-continuous process, fresh
dustrial use, primarily for desalination vantage is ease of scaleup, which is feed is added to the tank at the
of seawater. Unlike the membrane linear and straightforward. Pilot work same rate permeate is withdrawn,
processes discussed so far, the sep- is done with one or a few modules so that the retentate concentration
aration mechanism is solution/diffu- identical to those to be used in pro- still increases while the tank level
sion, meaning molecules dissolve in duction, which minimizes scaleup remains constant.
the polymeric membrane, then pass risk. The required number of pro- The pressure driving force, known
through by diffusion. In desalina- duction modules is easily calculated as transmembrane pressure (TMP),
tion, the most common application, from the target production rate and is generated by the combined ac-
the electrostatic attraction between the permeate flowrate per unit filtration of the circulation pump and the
Pp
to Figure 3, this pressure drop due
to bulk fluid flow is expressed as in
Equation (1) below:
Pin Pout
Pb = Pin Pout (1)
FIGURE 3. The pressure profile within a CFM module is an important factor to consider. Here, Pin is the
feed/retentate pressure at the module inlet, Pout is the feed/retentate pressure at the module outlet and This is not to be confused with trans-
Pp is the permeate pressure membrane pressure, which is the dif-
throttling valve downstream of the materials that are more difficult to ference between the average feed/
module. These must be balanced handle. A partial list of applications of retentate and permeate pressures,
to maintain a stable operation. For crossflow membrane microfiltration as shown in Equation (2):
example, throttling the valve will in- (CMMF) is given in Table 2.
crease the transmembrane pressure, In addition to the general advan- Ptm = [(Pin + Pout)/2] Pp (2)
which tends to increase the flux (up tages of CMF cited previously, CMMF
to a point this is discussed further offers a permeate that is completely Often, the permeate pressure is
later in the article). At the same time, solids-free, and typically more clear close to atmospheric, just high
the flowrate will decrease, and the than filtrates from conventional filters enough to overcome the friction loss
reduced shearing action will result in [1] or centrifuges [2]. Moreover, no fil- in the downstream piping. Intuition
a lower flux. ter aids or other processing aids are tells us that a higher TMP results in
Note that in Figure 2, the pump needed. Disadvantages are the inabil- a higher flux, and this is generally
discharge is cooled. This may seem ity to produce a cake, as well as pos- the case, up to a point. However,
counterintuitive, because in most sible pluggage of membrane pores above some threshold value typi-
cases, a higher temperature results with compressible solids. However, if cally about 1 bar a polarization
in a lower viscosity, and in turn, a macromolecules are not needed, the or gel layer forms on the membrane
higher filtration rate. However, the latter issue can be overcome with the surface [3]. This layer is composed
circulation pumps used in crossflow use of a coarse ultrafiltration mem- of undissolved solids and retained
membrane units are rather large, brane, with pores large enough to molecules in the feed. Moreover, be-
and generate a significant amount pass all but the largest dissolved mol- cause retained species concentrate
of heat. For this reason, cooling may ecules, yet sufficiently small to exclude near the membrane surface, precipi-
be needed to avoid damage to the undissolved solids. This technique is tated components may be present if
product, or in the case of common used, for example, in the filtration of their solubility limit is reached.
polymeric membranes, remain below apple juice. Once the polarization layer is es-
the maximum allowable operating Operating pressures in ultrafiltra- tablished, a further increase in TMP
temperature. This is especially true in tion are higher than in CMMF, but still does not increase the flux, and may
a batch process when the retentate relatively low. If undissolved solids are even reduce it. In addition, the polar-
volume becomes small. Cleaning is not present, volume reductions of 30 ization layer actually does the filtra-
done without the need for disassem- or higher are possible, much higher tion, and the membrane itself has little
bly, a feature known as clean in place than those achievable with CMMF. effect on the permeate composition.
(CIP), which is common in food and The limitation may be the retentate To minimize the effect of the polariza-
pharmaceutical applications. The in- viscosity, the solubility limit of one or
dicated ability to recycle permeate to more components or the practical
TABLE 2. PARTIAL LIST OF
the feed/retentate tank is useful dur- problem of equipment holdup that CMMF APPLICATIONS
ing certain portions of the CIP cycle. is, enough retentate is needed to fill Removal of cells or cell fragments from fermen-
the pipes and avoid pump cavita- tation broth
MF and UF basics tion. Ultrafiltration is widely used in Removal of microorganisms from potable water
Microfiltration membranes, which are the food industry for example, to Removal of microorganisms from milk
Removal of fat from milk
used to produce clear permeate from concentrate proteins in skim milk or Removal of haze from gelatin
slurries containing solids as large as cheese whey. The process is also Removal of m-size particles from a variety of
10 m, typically have ratings of 0.1, commonly used in drug purification liquid streams
Concentration of fine solids
0.2, 0.45 or 0.65 m. Required trans- and other pharmaceutical applica- Pretreatment for ultrafiltration, nanofiltration or
membrane pressure is low, usually tions, as well as water purification and reverse osmosis
1050 psi as explained later, higher chemical recovery in the textile, paper Sterilization in the pharmaceutical industry
is not necessarily better. Volume re- and waste-treatment industries. Purification of therapeutic proteins and other
pharmaceuticals
duction is typically 512, correspond- Clarification of beverages (such as beer, wine or
ing to undissolved solids of 100700 Pressure effects and polarization fruit and vegetable juices)
g/L in the retentate. Greater volume As with normal pipe flow, friction Purification of fluids for semiconductor
reduction and higher retentate solids causes a loss in pressure from the manufacturing
Separation of radioactive solids from liquid
are achieved with rigid, incompress- inlet to the outlet of the module on waste in nuclear power plants
ible solids than with soft or gel-like the feed/retentate side. Referring

300
Feed/retentate
consideration of the heat gener-
5 m/s ated by the circulation pump. As
250
Diffusion Convection discussed below, membranes made
Gel from inorganic materials and certain
200
Membrane polymers allow operation at temper-
atures well above the limits of tradi-
Flux, LMH
150 tional polymeric membranes. How-

Permeate
ever, the rate of membrane fouling
2 m/s
100 may also increase with temperature,
Ceramic (-alumina) membrane, 0.2 m and this can negate some or all of
50 Volume concentration factor: 1 the benefit. In addition to the change
Temperature: 60oC
with temperature, any increase
0 in viscosity with retained species
0 5 10 15 20 25 30 35 40 45 50 concentration must also be taken
TMP, psi
into account.
FIGURE 4. The flux (in liters of permeate per square meter of membrane area per hour, or LMH) versus
transmembrane pressure (TMP) for microfiltration of corn starch hydrolysate at two different linear veloci- Fluid composition. The starting
ties is shown [4] concentration and solubility of re-
tained molecules clearly have an
tion layer and maximize the flux, TMP from the polarization layer are equal, impact on design for example,
should be kept relatively low typi- and the polarization layer is stable. they affect the achievable retentate
cally 1015 psi for MF, and up to 50 An increase in pressure causes an concentration and, barring other
psi for UF. For applications that are increase in the rate of convective limitations, volume reduction. If un-
particularly sensitive to fouling, much transport to the layer, which leads to dissolved solids are present, not
lower TMP values are used, as low an increase in the retained species only is their concentration impor-
as 12 psi. These low TMPs require concentration, and in turn, increased tant, but also the nature of those
backpressure on the permeate side, rate of diffusion back into the bulk. A solids. As with conventional filtra-
an exception to the general practice new steady state is established, and tion, rigid, spherical particles are
of operating with the permeate near the net result is no change in flux, more easily removed than ones that
atmospheric pressure. consistent with Figure 4. are soft, gelatinous or odd-shaped.
Evidence of the polarization layer Interactions between the feed and
is clear in Figure 4, which shows Design considerations the membrane material also war-
flux versus TMP for microfiltration Important design considerations rant consideration. For instance,
of corn starch hydrolysate at two include not only most or all of the components of interest can be lost
different linear velocities [4]. These considerations pertinent to the de- if adsorbed onto the membrane sur-
data were collected at a concentra- sign of traditional filter or centrifuge face. In this case, the designer must
tion factor of one, meaning all per- operations, but also some that either select a membrane material
meate was recycled. At low values are unique to membrane systems. with little affinity for the solute, or
of TMP, the flux increases linearly Key factors are described in the if possible, change the processing
with TMP, as one might expect. following paragraphs. conditions (for example, pH) to re-
However, the curves begin to level Productivity target (usually ex- duce affinity.
off at about 25 psi, and above 30 pressed as annual throughput). As Fouling tendency. Membrane clean-
psi there is no increase in flux upon with any chemical engineering unit ing adds cost, attributable not only
further increase in TMP. Note that operation, this figure forms the basis to the required chemicals, but more
the maximum flux is higher at the of membrane process design and importantly, to the associated down-
higher linear velocity, because the economics. For example, through- time. Membrane materials, operat-
higher shear reduces the thickness put drives the choice of batch or ing conditions, cleaning protocol,
of the polarization layer, and in turn, continuous processing, with larger and where possible, feed proper-
the resistance to flow. volumes making the latter more cost ties, must be selected to minimize
Membrane operation with an es- effective. Once the permeate flux is fouling, and in turn, cleaning time
tablished polarization layer is illus- known from pilot work, the mem- and frequency. While the feed com-
trated in the inset in Figure 4. The brane area needed to reach the pro- position gives some clues about ex-
retained species is transported from ductivity target is a straightforward pected fouling tendency, longterm
the bulk feed/retentate to the polar- calculation, as mentioned above. pilot testing is needed to develop a
ization layer by convection. The con- Fluid physical properties (espe- full understanding.
centration of the retained species cially viscosity). In most cases, Modules. The module specifica-
in the polarization layer increases, flux decreases with increasing vis- tions are a key part of membrane
and this gradient drives diffusion cosity. For this reason, membrane system design. Available mod-
back into the bulk. At steady state, processes are sometimes operated ule configurations are discussed
the rates of transport to and away at elevated temperatures, with due in subsequent sections of the ar-
S. Koseoglu, Filtration and Membrane World LLC
TABLE 3. FACTORS INFLUENCING MEMBRANE FLUX

Factor General effect
Temperature Higher temperature leads to higher flux, but rate of fouling may also increase
Undissolved solids Flux tends to decline with increasing solids content
concentration
Nature of undissolved Flux and achievable volume reduction are higher with rigid, spherical solids than
solids with soft, gelatinous or odd-shaped ones
Dissolved solids Flux tends to decline with increasing solids content, at least partly due to higher
concentration viscosity
Viscosity Higher viscosity results in lower flux
Transmembrane Flux increases with TMP up to a point, then further TMP increases have little effect
pressure (TMP)
Linear velocity Flux increases with linear velocity, but again up to a point
Pore size Flux is usually higher with larger pores. One notable exception is with soft particu-
late matter, which may plug larger pores but are excluded from smaller ones
Porosity A higher porosity leads to a greater flux, but mechanical strength is insufficient
when porosity is too high
Membrane thickness A greater thickness results in a lower flux
FIGURE 5: Asymmetric membranes, such as the
ticle. Specifications include module lower packing efficiency. one shown in this electron micrograph, are char-
length, diameter, size and location Flux. Clearly, an important number in acterized by a thin selective layer on top of a more
open support layer
of ports, internal dimensions, mate- membrane system design is the flux,
rials of construction, and of course, usually expressed as liters of perme- were made from cellulose acetate,
membrane filtration area. Key operate per square meter of membrane and this polymer is still used. How-
ating specifications are temperature, area per hour (LMH), or gallons per ever, its chemical resistance is lim-
transmembrane pressure and linear square foot per day (GFD). A similar ited, pH tolerance is only in the range
velocity. The latter is typically 12 and performance measure is permeability, from about 2 to 9, and the maximum
57 m/s for polymeric and inorganic or flux per unit transmembrane pres- allowable temperature is relatively
membranes, respectively. The ben- sure for example, LMH per bar. low at 35C. Since the advent of
efit of the increase in flux with linear Factors influencing flux and perme- membrane filtration on an industrial
velocity (shown, for example, in Fig- ability are listed in Table 3. The goal of scale, there have been considerable
ure 4) is at least partially offset by the pilot testing is to quantify these effects, advances in polymer technology.
higher pumping cost. Thin channels particularly those of transmembrane Today, there are a variety of robust
offer higher membrane area per unit pressure, linear velocity and retained polymeric membranes that can oper-
volume (that is, packing efficiency), species concentration. ate at pH values ranging from 1 to 14,
but these are not suitable for streams and in some cases, at temperatures
with high viscosity or undissolved Membrane materials of 120C or even higher. Examples
solids content. Those situations re- In the early days of crossflow mem- include polysulfone (PS), polyether-
quire wider channels, and in turn, brane filtration, most membranes sulfone (PES), polyvinylidene fluo-

Courtesy of Koch Membrane Systems, Inc. (www.kochmembrane.com) and used by the publisher with permission
Water
FIGURE 7. The ability to backwash hollow-fiber

membrane modules provides more effective
cleaning
and the tube wall is the membrane.

Feed enters the tubes at the bot-
tom, retentate leaves at the top,
and permeate passes through the
FIGURE 6. The hollow-fiber membrane configuration is shown as follows: (a): fiber cutaway displaying tube walls, then exits through the
asymmetric pore structure; (b): module containing polysulfone fibers encased in a shell that is also poly- shellside. Fibers are available in di-
sulfone; (c) commercial unit using the modules shown in (b) ameters of 0.256 mm, but 13 mm
ride (PVDF), polyacrylonitrile (PAN), bases and other corrosive chemi- fibers are most common. A typical
polyamides, polytetrafluoroethylene cals, as well as high temperatures module is 1020 cm in diameter by
(PTFE) and polypropylene (PP). and pressures. Such membranes 11.6 m in length. The single fiber
Most of these membranes are are particularly useful for high-foul- cutaway in Figure 6a clearly shows
asymmetric, characterized by a ing applications that require aggres- the asymmetric nature of the pores
thin selective layer on top of a more sive cleaning. Inorganic membranes in the tube wall. The module shown
open support layer (Figure 5). The are more expensive, but they last in Figure 6b contains polysulfone
tight selective layer, also called the longer than polymeric ones, justify- fibers encased in a shell that is also
dense, active or skin layer, does the ing the higher cost in some cases. polysulfone, and a commercial unit
actual filtration. Once this is done, a Additional detail is given in the dis- using these modules is depicted in
tight structure is no longer needed, cussion of membrane modules Figure 6c.
and use of an open support mini- presented below. Selection crite- The main advantage of the hol-
mizes the resistance to flow, while ria for the membrane material are low-fiber configuration is the abil-
still providing the required mechani- cost, compatibility with the pro- ity to tightly pack the fibers, allow-
cal integrity. A sublayer of intermedi- cess stream, any interactions (for ing a high membrane area per unit
ate pore size is also used in some example, adsorption) with feed volume, as high as 16,000 m2/m3.
cases. There are also symmetric components, ability to clean and Another advantage is the ability to
membranes that contain pores with expected lifetime. backwash for more effective clean-
a uniform cross-section. These offer ing. Backwash, shown schemati-
greater mechanical strength and Module configurations cally in Figure 7, entails forcing water
longer life than asymmetric mem- Available module configurations through the membrane in the direc-
branes, but the flux is lower. are described in the following para- tion opposite to normal flow (that
Inorganic membranes are also graphs, and a summary is presented is, from the permeate to the feed/
available. These include ceramics, in Table 4. retentate side), to dislodge foulants
such as -alumina, zirconia and Hollow fiber. This module contains from the membrane surface. These
metal oxides (notably, titanium di- a bundle of polymeric tubes, also advantages make the hollow-fiber
oxide), sintered stainless steel and called hollow fibers, potted at both design an economical option for
graphite. Inorganic membranes are ends and encased in a shell. The many applications, especially in the
more robust than most polymers, geometry is analogous to that of food and pharmaceutical industries.
able to withstand strong acids, a shell-and-tube heat exchanger, For example, hollow fibers are used
in over 90% of the 1,500 wine filtra-
tion plants throughout the world. Spiral membrane configuration
A disadvantage of hollow-fiber Permeate collection holes Retentate
modules is their greater fouling ten-
dency compared to other module Feed solution (in) Permeate
(out)
configurations. In addition, fiber Retentate
pluggage can occur if large solids are Permeate
(out)
present, a problem that can some- Anti-
telescoping
times be resolved by prefiltration of Feed solution (in) device
the feed. If a larger fiber diameter Feed flow (across feed channel spacer)
must be used, there is a penalty in Membrane
Permeate collection material Covering
membrane area per unit volume. Fi- Permeate flow (after passage
Membrane
nally, hollow fibers are not suitable for Feed channel spacer through membrane into permeable
collection material)
streams with high viscosity or undis- FIGURE 8. Spiral-wound modules are commonly used for water filtration
solved solids content. Those appli-
cations are a better fit for a tubular rated by a porous spacer. These and the fourth side is attached to
module, discussed below. spaces provide a path for the per- the central tube. Typical channel
Spiral wound. As shown in Figure meate, which flows around the spi- width, module diameter and length
8, this design consists of one or ral to the central core, then exits are 0.250.5 mm, 1040 cm and
(usually) more membrane envelopes the module. The spaces between 11.5 m, respectively.
wound around a perforated central adjacent envelopes, separated by Spiral-wound modules are com-
core. Each envelope contains two grids, serve as flow channels for monly used for water purification,
rectangular membrane sheets fac- the feed/retentate. Each envelope is and the high volume drives the cost
ing away from each other, sepa- sealed with adhesive on three sides, down for other applications as well.
TABLE 4. MODULE CONFIGURATIONS

Configuration Description Advantages Disadvantages Additional comments
Hollow fiber Fiber bundle potted at both High filtration area per unit High tendency to foul Often an economical option for
(Figure 6) ends, encased in a shell volume Fibers can plug low-viscosity, low-solids feeds
Can be backwashed Not recommended for high viscosities
or undissolved solids contents
Spiral wound Membrane envelope(s) wound Prevalence in water purification Not suitable for fibrous solids Most common and economic
(Figure 8) around a central permeate drives cost down for other ap- Not recommended for high viscosities configuration in use today. Often
collection tube plications as well or undissolved solids contents a good choice for low-viscosity
Low energy consumption Flow channels can plug feeds with low levels of non-
High filtration area per unit Not recommended for high-value fibrous solids
volume products because modules do not
drain completely
Complex design and structure
Cannot be backwashed
Tubular Active layer is deposited onto Resistant to fouling because Low packing density leads to high cost Good choice for streams with
(Figure 9) a porous tubular support, of good fluid hydrodynamics per unit area high viscosity, elevated concen-
which is situated in a pres- (turbulent flow) High energy consumption tration of large solids, or high
sure vessel housing Easy to clean Usually cannot be backwashed fouling tendency
Able to handle high viscosities,
high undissolved solids con-
tents and large particles
Plate and frame Flat sheet membranes as- Baffles can be used to achieve Low area per unit volume In general, these are being re-
(Figure 10) sembled in a plate-and-frame high fluid velocities at lower High cost of frames drives overall placed by other configurations
device reminiscent of a filter circulation rates than with cost up
press other designs
Can be built with wide plate
spacing, to accommodate
high viscosities or undissolved
solids levels
Ceramic Porous ceramic monolith con- Can withstand high tempera- Low area per unit volume Ultimate in tolerance of severe
(Figure 11) taining parallel flow channels, tures. High capital cost (but may be justified process conditions and resistance
with active layer deposited Highly resistant to chemical by longer life) to chemical attack
onto the channel surface attack High pumping cost
Handle high linear velocities
without excessive abrasion
Long membrane life
Sintered Sintered stainless-steel tubes Same as for ceramics, but with Available pore sizes are limited A lower-cost alternative to
stainless steel with TiO2 active layer depos- lower cost Stainless steel is vulnerable to chloride ceramics for some applications
(Figure 12) ited onto the surface, encased No seals to fail because chan- stress corrosion
in a stainless-steel shell nels are welded in place TiO2 active layer may be subject to
abrasion

sistance to fouling, attributable to

good fluid dynamics (turbulent flow);
ease of cleaning; and simple mod-
ule design and structure. Disadvan-
tages are low packing density, and
in turn, low area per unit volume;
high energy consumption; and the
inability to backwash. Applications
of tubular modules include waste-
water treatment, paint recovery and
juice clarification.
Plate-and-frame modules. This is
one of the earliest designs. These
modules contain a series of flat
membrane sheets, usually disk-
shaped, arranged in a plate-and-
frame assembly. As shown in Figure
FIGURE 9. Tubular modules employ a shell-and-tube design, as shown in (a), a module containing PVDF 10a, the membrane side of each
tubes and a polysulfone shell; (b) shows a commercial unit using the modules shown in (a)
sheet faces a feed channel, with
Additional advantages are lower It is the most economical choice for the space between the opposite
energy consumption compared many applications, particularly water sides providing a flow path for per-
to other designs, and like hollow- purification, as mentioned previously. meate. This assembly, reminiscent
fiber modules, high area per unit Tubular. Like the hollow-fiber design, of a traditional filter press, is situ-
volume. On the downside, spiral- tubular modules have a shell-and- ated between two end plates, with
wound units are not suitable if fi- tube geometry, but the tubes are gaskets placed as needed to direct
brous solids are present, because larger, with the inner diameter rang- flow. A commercial unit is shown
these will clog the grids. Prefiltra- ing from 2.5 to 25 mm. The tubes in Figure 10b.
tion is recommended to remove consist of a porous support, such Feed channels can be narrow, for
particles larger than one twentieth as fiberglass-reinforced epoxy, with non-viscous, low-solids feeds, or
of the channel width (1/20 rule). the active layer formed on the in- wide, to accommodate more diffi-
Moreover, as with hollow-fiber side surface. The shell is made from cult process materials. In addition,
modules, process streams with stainless steel or a hard polymer. A baffles can be used to reach high
high viscosity or high undissolved single module and an industrial unit velocities at low pumping rates.
solids content are better suited are shown in Figure 9. On the downside, the low area per
for tubular modules. Because spi- Tubular modules are chosen for unit volume and high cost of frames
ral-wound modules are difficult to feeds that are difficult to handle, have led to a decline in the popular-
drain completely, the hollow-fiber and are not suitable for hollow fiber ity of plate-and-frame modules.
design is preferred for valuable or spiral wound designs. These in- Ceramics. A ceramic module con-
products. Finally, the design and clude feeds with high viscosity, high sists of a porous ceramic material,
structure of spiral-wound mod- undissolved solids content, large called a monolith, through which
ules are complex, and they cannot particles (up to 2.5 mm; prefiltration: parallel flow channels have been
be backwashed. 1/10), or highly compressible or ge- formed. The separation is performed
Despite these disadvantages, the latinous solids. Advantages in ad- by a thin active layer of smaller par-
spiral-wound module is the most dition to the ability to handle these ticles deposited onto the inside
common configuration in use today. challenging streams are high re- surface of the channels. Channel
diameters are 26 mm, and pore
Feed sizes extend from 40 (NMWC =
~1,000) to the m range. The active
layer is usually -alumina, zirconia
Membrane or titanium dioxide, while the mono-
lith is typically -alumina or other
metal oxide.
Examples of ceramic modules are
shown in Figure 11. As with hollow-
Retentate
fiber and tubular designs, a shell-
and-tube geometry is used. The
Permeate
(a) (b)
Alfa Laval
cylindrical inserts in the photograph
FIGURE 10. A plate-and-frame membrane module is shown schematically (a); and as an are known as elements; a common
industrial unit (b) design is 19 channels per element.
Atech Innovations Gmbh
is delivered in the direction opposite product. Pulse frequency and du-
to normal flow that is, from the ration vary, but typical settings are
permeate to the feed/retentate side. once every 25 min for 0.5 s.
This improves flux by dislodging fou- Additional advantages of ceramic
lants from the membrane surface. modules are higher abrasion resis-
The concept is like backwashing, tance than polymers, allowing op-
discussed earlier, but backwash- eration at a higher linear velocity;
ing uses an extended flow of water and membrane life up to 10 years,
during cleaning, while back-pulsing compared to 1 to 2 years for a typi-
involves periodic pulses of perme- cal polymeric membrane. The main
ate that are delivered while running disadvantage of ceramics is their
FIGURE 11. Ceramic modules such as these can

withstand higher temperatures and more aggres-
sive chemicals than polymeric modules
In operation, permeate coming

through the active layer flows by
gravity to the bottom of each mono-
lith, then into the shell space and Perfection is
out the exit port. Meanwhile, feed/
retentate transverses the length of
Better Dispersion and Control
the channel, then leaves.
Ceramic modules can withstand
temperatures of 150C or more,
much higher than the maximum of
5055C for many polymers. This is
useful for viscous feeds, and allows
high-temperature cleaning in heavily
fouling applications. Moreover, ce-
ramics are highly resistant to chemi-
cal attack, permitting their use with
process streams that attack poly-
mers. An example is the use of ce-
ramic modules to remove wax from
citrus oils, which are highly corro-
sive to most polymeric membranes
[5]. Their chemical resistance also
allows ceramics to be aggressively
cleaned with strong acids, bases or
other harsh chemicals.
Another advantage of ceramic
Perfecting Particle Size
The Sturtevant Micronizer jet mill reduces the
modules is the ability to back-pulse,
particle size of pesticides, herbicides, fungicides,
also called blowback. With this tech- insecticides and dry chemicals to narrow particle
nique, a periodic pulse of permeate size distributions of 0.25 microns or larger without
heat buildup.
Graver Technologies
Better control properties - dispersion & reactivity
Particle-on-particle impact, no heat generation
Simple design, easy to clean
Abrasion resistant for long life
348 Circuit Street Hanover, MA 02339
Phone: 800.992.0209 Fax: 781.829.6515 sales@sturtevantinc.com
www.sturtevantinc.com
FIGURE 12. A sintered stainless-steel module is
fabricated as one solid, highly porous unit Circle 26 on p. 78 or go to adlinks.chemengonline.com/66427-26

10,000
rate that permeate is removed, so
9,000
8,000
that the rententate volume remains
7,000 constant. It is easy to show that the
Solute, ppm
6,000 displacement of permeable compo-

5,000 nents obeys the exponential rela-
4,000 tionship given in Equation (3):
3,000
2,000
1,000 C(t)/C0 = eWtV = eN (3)
0
0 1 2 3 4 5 6 Here, C(t) is the concentration of the
Volume turnovers
FIGURE 13. In this example, diafiltration is used for the removal of residual crosslinking agent from a slurry permeable component(s) at time t,
of polymer beads. The points are the actual data and the solid line is the prediction from Equation (3) C0 is the concentration at the start
of diafiltration, W is the flowrate of di-
high cost, although this is some- perature tolerance and resistance afiltration water (equal to the perme-
times economically justified by their to chemical attack, but at a lower ate flowrate), V is the volume of re-
longer life. Other disadvantages are cost. In addition, there are no seals tentate and N or Wt/V is the number
low area per unit volume, part of to fail, because all connections are of volume turnovers that is, the
the reason for the high cost; and welded. On the downside, avail- volumes of diafiltration water per vol-
high pumping cost, a downside of able pore sizes are limited with ume of retentate. For example, if the
operating at a higher linear velocity. stainless-steel modules, stain- retentate volume is 1,000 L, each
Sintered stainless steel. These less steel is subject to chloride 1,000 L of diafiltration water added
modules are made by placing pow- stress corrosion, and erosion of is one turnover. The data in Figure 13
dered stainless steel in a mold, the TiO2 active layer can occur in are for removal of a residual cross-
then heating to a temperature just some applications. linking agent from a slurry of polymer
below the melting point. Atoms beads. As predicted by Equation (3),
diffuse across particle boundar- Diafiltration 95% of the solute was removed after
ies, fusing the particles together As mentioned above, diafiltration three turnovers.
to create one solid, highly porous is used to recover additional per- When the permeate is the valuable
piece. As shown in Figure 12, meable components from the re- stream, in most cases, the water
again, a shell-and-tube geometry tentate, when the permeate is the added during diafiltration must be
is employed. The active layer is valuable stream. Alternatively, when removed downstream, usually by
titanium dioxide (TiO2), which is the retentate is valuable, diafiltration evaporation. The optimum amount
annealed onto the inside surface serves to improve purity by removing of diafiltration water represents a
of the channels. These modules permeable contaminants. In a batch trade-off between the value of the
offer most of the same advantages process (such as in Figure 2), diafil- recovered product and the cost
as ceramics, including high tem- tration water is added at the same of energy.
Continuous operation
Batch and semi-continuous pro-
Permeate cessing are discussed above, and
these operating modes are impor-
Feed
tant when volumes are relatively
Steam
small. However, as with other chemi-
Water
cal engineering unit operations, con-
tinuous processing is more efficient
Feed tank Stage 1 Stage 2 Stage 3
and cost-effective when volumes
are large. In most cases, continu-
Steam Steam ous membrane filtration processes
CIP
contain multiple stages. This is ad-
solution Water Water vantageous because, for many ap-
plications, flux declines with increas-
CIP
tank ing concentration of the retained
species. Since each stage operates
CIP: clean in place PIC: pressure indicator-controller
FI: flow indicator PSH: high pressure switch Retentate at the flux corresponding to the con-
FIC: flow indicator-controller RC: ratio controller
FIT: flow indicator-transmitter T: steam trap centration of the retentate leaving
PI: pressure indicator TIC: temperature indicator-controller
Diafiltration
that stage, the overall flux is higher
water with multiple stages, and less mem-
FIGURE 14. This example of a flowsheet for a three-stage, continuous crossflow membrane filtration pro- brane area is needed to reach the
cess includes diafiltration added to the third stage targeted productivity. A continuous
TABLE 5. COMMON CLEANING AGENTS nally, a high linear velocity is needed
Type of cleaner Example What it removes to impart sufficient shear at the
Caustic 12% NaOH, pH > 10 Proteins, microorganisms, biological debris membrane surface.
Detergent 0.1% Alconox Particulate matter, miscellaneous organics, Common cleaning agents are
Enzyme-based detergent 0.1% Tergazyme colloidal fouling listed in Table 5. Typically, the clean-
Sodium hypochlorite bleach 2001,000 ppm in water Cleans and sanitizes ing protocol calls for several such
Acid 12% sulfamic acid Inorganic scale
cleaners in sequence. For example,
the following steps may be used
membrane system with an infinite Membrane fouling and cleaning to clean a membrane handling a
number of stages requires the same Because cleaning time is non-pro- stream containing microorganisms
filtration area as a batch unit. How- ductive, productivity is maximized and proteins, such as a fermenta-
ever, addition of stages eventually re- when cleaning is infrequent, fast tion broth:
sults in a diminishing return, because and effective. To minimize the rate Water rinse
the cost of the additional circulation of fouling and specify an effective Detergent or caustic cleaning
pump, piping, controls and other cleaning protocol, fouling mecha- Water rinse
components exceeds the savings nisms must be well understood. Acid cleaning
obtained from the reduced filtration Fouling may be organic, inorganic Water rinse
area. In general, the area needed or microbiological in nature. Usually, A cleaning cycle such as this one
for five stages is within 20% of the the foulants are present as physical may require 3 to 4 hours. Except
batch area. buildup on the membrane surface, when using acids, cleaning is usually
The continuous membrane filtra- but they may also be adsorbed, or more effective at elevated tempera-
tion process shown in Figure 14 has small particulate matter may pene- ture. Acid cleaning is done at room
three stages, with diafiltration water trate the pores. Chemical reactions temperature because the inorganic
added to the third stage. With the on the surface may also contribute scale it is intended to remove (for ex-
control strategy employed, the fee- to fouling. ample, calcium salts) often exhibits
inverse temperature solubility.
Edited by Mary Page Bailey
There are a number of strategies for minimizing the
rate and extent of fouling. Prefiltration to remove large References
1. Gabelman, A., An Overview of Filtration, Chem. Eng.,
particulate matter, using a conventional filter or centrifuge, November 2015, pp. 5058.
is sometimes helpful. Similarly, fouling can sometimes be 2. inGabelman, A., Beyond Gravity: Centrifugal Separations
CPI Operations, Chem. Eng., July 2016, pp. 5259.
reduced by upstream removal of large molecules with a 3. Zydney, A.L., Colton, C.K., A Concentration Polarization
Model for the Filtrate Flux in Cross-flow Microfiltration
tendency to foul, using a UF membrane with a relatively of Particulate Suspensions, Chem. Eng. Comm. 47
(1986) 1-21.
high NMWC. 4. Singh, N., Cheryan, M., Process Design and Economic
Analysis of a Ceramic Membrane System for Microfil-
tration of Corn Starch Hydrolysate, J. Food Engr. 38
drate is set independently, while the There are a number of strategies (1998) 5767.
flowrate of final retentate is modu- for minimizing the rate and extent 5. Finn, A., Gabelman, A., Dewaxing, U.S. Patent
9,422,506, 2016.
lated by ratio control to maintain of fouling. Prefiltration to remove
the desired volume reduction. Ratio large particulate matter, using a
control is also used to regulate the conventional filter or centrifuge, is Author
flow of diafiltration water, based on sometimes helpful. Similarly, fouling Alan Gabelman is president of
the retentate flowrate. Each stage can sometimes be reduced by up- Gabelman Process Solutions, LLC
(6548 Meadowbrook Court, West
has provisions for temperature con- stream removal of large molecules Chester, OH 45069; Phone:
trol by heating or cooling, retentate with a tendency to foul, using a UF 513-919-6797; Email: alan.
back-pressure control and, to pro- membrane with a relatively high gabelman@gabelmanps.com;
Website: www.gabelmanps.com),
tect the module, a high-pressure NMWC. Upstream dilution of feed offering consulting services in pro-
switch that shuts off the circulation can reduce the rate of fouling, with cess engineering. Gabelmans 39
years of experience include nu-
pump when activated. The circula- the downside that a larger volume merous separation processes and other engineering
tion pumps are large, and the fee- needs to be filtered. Judicious se- unit operations, equipment selection, sizing and design,
drate to each stage is only a small lection of the membrane material is process simulation, P&ID development, and process
economics. He holds B.S., M.Ch.E. and Ph.D. degrees in
fraction of the circulation rate. Note crucial to minimize interactions with chemical engineering from Cornell University, the Uni-
that there are no controls regulating the process stream that may lead to versity of Delaware and the University of Cincinnati, re-
the flow of retentate from one stage fouling. In some cases, such inter- spectively. He is a licensed Professional Engineer, as
well as an adjunct instructor in chemical engineering at
to the next. These are not necessary actions can be reduced by chang- the University of Cincinnati. Gabelman has edited a book
because the system is self-adjusting ing processing conditions for on bioprocess flavor production, and he has authored
and stable. example, temperature or pH. Fi- several technical articles and a book chapter.

Feature Report
Part 2
Gas-Phase Filtration
Media Properties:
What to Know
There are many physical properties that can impact the ultimate performance of
adsorbent media in gas-phase filtration applications
G
Chris Muller as-phase filtra- 1.0
Purafil, Inc. tion media speci-
Ce
fications may list 0.9 C0
= 0.9
numerous physi-
IN BRIEF cal parameters, such as 0.8
MEDIA SHAPE shape, moisture content, B = 0, n = 1, Bi =
MOISTURE CONTENT bulk density, impregnation
C/C 0
0.7
level, size and hardness
BULK DENSITY
(crush strength or abra-
0.6 Legend a Ce/C 0 Shape
ADSORPTION EFFICIENCY sion), as important deter- 1 0.9 planar
minants of final media per- 2 0.9 cylindrical
REMOVAL CAPACITY 3 0.9 spherical Ce
0.5 = 0.5
formance. The way these 1 0.5 planar C0
2 0.5 cylindrical
physical characteristics 3 0.5 spherical
can be controlled and opti- 0.4
105 104 103 102 101 100 101
mized during media manu-
facturing processes can FIGURE 1. The effects of shape factor (a) and concentration on adsorption are shown
ultimately determine media for both theoretical and numerical solutions [1]
performance when installed
into any number of end-use applications, Spherical-shaped media of uniform size pro-
including standalone pressurization or recir- vide the most uniform packing, because with
culation units to prevent corrosion in pulp both planar (flake) and cylinder shapes, the
and paper mills or petrochemical plants, or media could settle upon itself. With spheres,
in deep-bed scrubbers in petroleum refin- one could ideally pack them to take up al-
eries and wastewater treatment plants to most 75% of the available space. However,
contain a release of toxic chemicals. this would only occur with complete pack-
In order to optimize the packing density, ing of the particles in the media container.
whether the media is to be used in dis- It would not be achieved by simply pouring
posable modules or deep-bed scrubbers, them into the container rather, randomiza-
spherical media is generally preferred. It is tion effects will only yield a maximum pack-
also the most favorable shape with regard ing fraction of 6065%.
to the diffusion of contaminants into pellets. With flake and cylindrical shapes, the
This article discusses the physical param- packing density from random packing meth-
eters of media shape, moisture content and ods, such as pouring without tamping or
bulk density specifically as they relate to vibrating, would result in a packing fraction
overall media performance, with some gen- similar to that of spherical media. However,
eral discussion of related parameters. over time, both of these media shapes can
stack upon themselves along their planar
Media shape axes, resulting in a higher packing fraction
The ability of particles to fill space by packing and settling of the media. This leads to by-
together is obviously related to their shape. pass and a reduction in performance of the
air-cleaning system. 0.6 FIGURE 2. Different adsorbent
Spherical shapes allow more ac- geometries are compared for
the same adsorption process.
cess to the external surface of the Here, coverage indicates the
0.5
particle, which is important in ad- fraction of adsorption sites of
sorption and in taking advantage of the surface of the media un-
Sphere available versus the number of
the large internal surface area. When 0.4 Cylinder
1 vacant sites still available for
planar or cylindrical media line up adsorption [2]
Coverage
or stack upon themselves, this effec- 0.3
2
tively blocks access to the external
surfaces in contact with each other.
Proper packing of spherical media 0.2
limits the surface area affected by
particle-to-particle contact and as- 0.1 3
sures access to the maximum num- Plane
ber of adsorption sites.
0.0
Adsorption is usually described
0 1,000 2,000 3,000 4,000
through isotherms the amount Time, s
of adsorbate (contaminants) on the
adsorbent (media) as a function tion (Ce) and initial concentration (C0), to preferentially adsorb water from
of its pressure or concentration at all in kg/m3. Other pertinent terms the air, which occupies adsorptive
constant temperature. The quantity in Figure 1 are the Freundlich coef- sites and reduces the efficiency and
adsorbed is nearly always normal- ficient (n), the dimensionless time () capacity of the carbon. The water
ized by the mass of the adsorbent and the dimensionless Biot number adsorption isotherm for activated
to allow comparison of different ma- (Bi). Figure 1 shows that the rate of carbon (Figure 3) shows that as long
terials. There are basically two well- adsorption will increase as the ad- as the relative humidity (RH) of the
established types of adsorption iso- sorbents shape factor (a) increases airstream remains below 5055%,
therms: the Langmuir and Freundlich in all cases, indicating that there is the carbon performance should not
adsorption isotherms. a minimum of surface energy for be affected. The carbon will equili-
Among numerous studies on ad- the sphere among the three shapes brate with the moisture content of
sorption dynamics of adsorbent of adsorbents. the air. However, this can produce
media, little has been reported on the Figure 2 [2] shows another rep- periods of much lower performance
effect of shape. One study compared resentation of the effect of differ- for a great number of contaminants.
adsorption dynamic processes for ent media geometries (shapes) on This is especially so when the car-
three adsorbent shapes: spherical, adsorption rate. Additional graphs bon is used to clean outdoor air.
planar and cylindrical. The results of could be provided to show the re- Some engineered media can op-
a comparison of both Langmuir and lationships between the rates of erate in a specified RH range of
Freundlich adsorption isotherms and adsorption (or removal) and other 595%, although it is recommended
kinetics showed that the rate of ad- physical parameters, but each has to operate in the range of 2080%
sorption will increase as the shape the same basic shape. The spheri- for optimum performance. Operation
changes from planar to cylindrical cal media is always to the left of the at the extremes of the RH range (for
to spherical, indicating that there cylindrical media, indicating a faster instance, <20% or >80%) can cause
is a minimum of surface energy for adsorption rate. a drop-off in performance due to
the sphere among the three media The real power of the Langmuir the following:
shapes. In other words, the spherical and Freundlich adsorption models is 1. The media drying out, which
geometry is the most favorable for in providing a reference framework causes the chemical impregnant
adsorption, and the planar geometry within which one is able to compare to come out of solution and not be
is the most unfavorable. the adsorption rates of spherical, cy- available for reaction
There are no simple representa- lindrical and planar geometries in a 2. The media becoming soft with
tions of the Langmuir and Freundlich relative scale. Figures 1 and 2 show too much water. Although a soft
adsorption models that can easily ex- this very well. media still retains full functionality
plain the changes in adsorption rates (and even works better in some
between spherical and cylindrical Moisture content applications), this can cause set-
media shapes. The easiest thing to Plain activated carbon used for air fil- tling of the media due to abrasion
do is to provide a graphic that shows tration typically has a moisture speci- loss, leading to bypass through
these differences. fication of 25 wt.%, and as long as the system
Figure 1 [1] compares theoretical the moisture content remains below
and numerical solutions for the rate 810 wt.%, the performance is rela- Bulk density
of adsorption in terms of concentra- tively unaffected. Above a moisture Practically all granular adsorbent or
tion in air (C), equilibrium concentra- content of 10 wt.%, carbon begins chemisorbent media are almost al-

ways sold by weight, and the over- provide a true cost-of-ownership Adsorption efficiency
all removal capacity for any given air comparison. To do so requires a de- As mentioned in the discussion of
cleaning system is determined by the termination of the removal capacity of media shape, the rate of adsorp-
volume of media it holds. Although the media (in units of g/cc or wt. %). tion is greater for spherically shaped
the media volume remains constant Media B lists a removal capac- media. This in turn can lead to a
for a given system, the media weight ity for hydrogen sulfide (H2S) of higher adsorption efficiency for a
can vary significantly due to differ- 17 wt.%. With a media bulk den- given combination of contaminant
ences in the medias bulk density. sity of 34 lb/ft3, the volumetric ca- types and concentrations, and ul-
For the purposes of this article, the pacity can be calculated as 5.78 lb timately higher removal capacities
bulk density is defined as the mass of H2S removed per cubic foot of and efficiencies. However, any dis-
(weight) of the media divided by the media (34 0.17). Media As stated cussion of adsorption efficiency must
total volume it occupies. This total H2S removal capacity is 20 wt.%, include an investigation of how freely
volume includes particle volume, in- which converts to 9 lb of H2S re- contaminants can diffuse into the
ter-particle void volume and internal moved per cubic foot of media inner structures (surface area) of the
pore volume. (45 0.20). Comparing these media pellet.
Lets say we are comparing two media based on their bulk density When uniform-sized spheres are
media (A and B) being offered and using the removal capacities packed into a media container, the
for the same application. Media provided, Media A exhibits a 50% same cross-sectional area presents
A has a bulk density of around higher volumetric H2S-removal ca- itself for each media pellet, promot-
45 lb/ft3 (0.721 g/cc). Media B has pacity. Air cleaning systems using ing radial diffusion. In cylindrical-
a bulk density of around 34 lb/ft3 granular media are filled by volume, shaped media, both radial and
(0.545 g/cc). Based on this, and as- not by weight, therefore, compari- longitudinal diffusion are important.
suming an equal cost per pound of sons based on a volumetric capac- Radial diffusion considers how long
media, Media B would cost less than ity and not a weight capacity should it takes materials to diffuse across
Media A to fill or replace the media in be used when developing media the radius of the cylinder, whereas
the same air-cleaning system. How- changeout schedules and lifecycle longitudinal diffusion considers how
ever, this is misleading and does not cost estimates. long it takes materials to diffuse
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50 dicates how much the media can
adsorb in grams of gas (for ex-
ample, H2S) per cubic centimeter
of media regardless of the system.
40
The volumetric capacity uses the
media density (g/cc) and the re-
moval capacity to determine the
total amount of contaminant gas an
Water loading, wt.%
30
air-cleaning system can remove per
unit volume. This provides a truer
comparison of one media to an-
20 other, because differences in bulk
density are taken into account.
Another helpful practice is to list
10
a medias capacity for a single con-
taminant as a minimum value, be-
cause the specific conditions under
which the media would be used
0 cannot be assured. This provides
0 2 40
RH, %
60 80 100 assurance that the media will be
able to remove a certain amount
FIGURE 3. This water adsorption isotherm for activated carbon shows the effect of relative humidity (RH) of contaminants before it has to be
on the adsorption performance replaced. This also allows for the
provision of media life estimates
through the length of the cylinder. cylinder length-to-diameter ratio that do not exceed those experi-
If the cylinders length-to-diameter exceeds 1.2. Many extruded media enced under actual use conditions.
ratio approaches 1, the rate of diffu- have an average length-to-diame- By determining removal capacities
sion approximates that of a sphere, ter ratio of 1.75, based on numer- against individual contaminants
which favors the more efficient ous sample analyses. and by specifying minimum values,
radial diffusion. users can properly account for the
With cylinder-shaped particles, Removal capacity actions of other contaminants that
the random nature of a packed bed To reiterate the statement from might be present in the airsteam
causes both the radial and longitu- above, gas-phase air cleaning against the media.
dinal axes to present themselves. systems using granular adsorbent Edited by Mary Page Bailey
When airflow is hitting the end of media are filled by volume and not
the cylinder, slower longitudinal dif- by weight. Therefore, one needs References
fusion is the result. With increasing to look at the removal capacity of 1. Wang, Z., Effect of adsorbent shape on adsorption dy-
cylinder length, the particles tend a particular media in terms of how namics in a batch adsorber, Chemical Engineering Sci-
ence, 54(23), pp. 5,7875,790, 1999.
to line up along their length. This much contaminant material a given
2. Kankare, J. and Vinokurov, I.A., Kinetics of Langmuirian
can have two results. If the ends volume of media can remove be- Adsorption onto Planar, Spherical, and Cylindrical Sur-
of the cylinders are perpendicu- fore it becomes spent and needs faces, Langmuir, 15, pp. 5,5915,599, 1999.
lar to the air flow, longitudinal dif- to be replaced. 3. Knaebel, K.S., Adsorbent Selection, Adsorption Re-
fusion predominates. If the media Media manufacturers may report search, Inc. Dublin, Ohio, www.adsorption.com/
publications/adsorbentsel1b.pdf.
particles are lined up along their a volumetric removal capacity or 4. Crittenden, B. D. and Thomas, W.J., Adsorption Tech-
length, radial diffusion dominates. as a percent by weight. These val- nology & Design, Butterworth-Heinemann, Woburn,
However, this media configuration ues are determined according to Mass., 1998.
results in a high packing density, the test procedures described in
which reduces the void volume the ASTM International Standard D Author
around the media, increasing the 6646-01, Standard Test Method Chris Muller is the technical di-
pressure drop, and decreasing the for Determination of the Accelerated rector for Purafil, Inc. (2654
Weaver Way, Doraville, GA 30340;
rate of adsorption. Hydrogen Sulfide Breakthrough Email: cmuller@purafil.com), a
Spherical media provides for Capacity of Granular and Pellet- manufacturer of gas-phase air-fil-
more efficient adsorption due to the ized Activated Carbon. Although tration media, filters, equipment
and air monitoring instrumenta-
uniform radial diffusion of contami- the title may suggest that this test tion. He is an expert on environ-
nant gases. The cylindrical shape method has limited use, it is read- mental air quality and gas-phase
air filtration, and has helped de-
of extruded media involves both ra- ily applicable for many different velop many standards on the topic of air filtration. He is
dial and the less efficient longitudi- media types against a wide variety an ASHRAE (American Society of Heating, Refrigerating
nal diffusion. Adsorption efficiency of contaminants. and Air-Conditioning Engineers) Distinguished Lecturer
who has presented over 75 seminars. Muller has written
is significantly reduced when the Breakthrough capacity testing in- over 150 peer-reviewed papers and articles.

Engineering Practice
Cooling Towers: Estimate Evaporation

Loss and Makeup Water Requirements
Applying mass and energy balance calculations yields critical operating insight
U. Vengateson FIGURE 1. Shown here is the
tin
National Petrochemical Co. typical variation of the water
(Saudi Arabia) temperature and the wet-
bulb temperature of the air
C
ooling towers are an impor- stream as the hot water inlet
tant unit operation in chem- stream flows down from the
top of the cooling tower and
ical process industries (CPI) the air stream flows upward Water Tw, out
Height of cooling tower, m

operations. Applying mass along the height of the cool-
and energy balance calculations en- ing tower
ables process engineers to evaluate tout
evaporation loss, blowdown and Air
makeup-water requirements, and
to evaluate the performance of the
cooling tower. In this article, an illus- Tw, in
trative study showcases an induced-
draft cooling tower and describes Range
Approach
several key parameters range, (tout Tw, in) (tin tout)
approach and efficiency and their
significance. Two methods are dis-
cussed to estimate evaporation loss.
Temperature, oC
Requirements for blowdown and
makeup water are also detailed. ization from the water, and thus the Case study
water is cooled. The CWR line from the process unit
Cooling tower operation As a rule of thumb, for every enters an industrial cooling tower at
The cooling of process streams 10F (5.5C) of water cooling, 1% 45C and leaves at 33C, as shown
and condensation of vapors are total mass of water is lost due to in Figure 2. The tower has three
important functions in CPI opera- evaporation. The humidity level cells, each operating at 2,500 m3/h
tions. The use of a cooling tower is of the up-flowing air stream in- of water flow. The total flow 7,500
the most common way of extract- creases, and once it leaves the m3/h is measured at the CWR line.
ing waste heat in CPI operations, tower the air stream is almost sat- The dry-bulb temperature and wet-
and water is the most commonly urated. The temperature profile of bulb temperature of the inlet air are
used coolant to remove waste heat the water and the wet-bulb tem- measured as 30.3C and 29C, re-
in the majority of such operations. perature of the air along the height spectively. The dry-bulb tempera-
A typical large petroleum refinery of a typical cooling tower is shown ture of the exit air is 41.5C, and it
that processes 40,000 metric tons in Figure 1. is assumed to be 100% saturated.
(m.t.) of crude oil per day requires The cooled water is collected in This case study is aimed at calculat-
80,000 m3/h of cooling water. This the sump (or basin) of the cooling ing the unknown variables that is,
is roughly equivalent to 25 barrels tower, and it is typically pumped to evaporation loss, air flow through the
of water for every barrel of crude oil the plant as the cooling-water-supply tower, blowdown flow, and the re-
processed [1]. (CWS) stream. After extracting heat quired makeup water flow. First, the
In a cooling tower, the hot water from the process units, this stream is important parameters approach,
stream (typically called the cooling returned to the cooling tower, as the range and efficiency are detailed.
water return) is introduced down- cooling-water-return (CWR) stream. Approach. The approach is defined
ward through spray nozzles into fills The heat load extracted from the as the difference between the water
inside the tower. There are different process unit is finally released to the temperature at the tower outlet (tout)
types of fills splash, trickle and environment in the cooling tower. A and the wet-bulb temperature of the
film that are aimed at creating cooling tower is designed to re- inlet air (Tw,in). The approach repre-
more surface area, to maximize con- move the total heat load that is ex- sents the cooling tower capability.
tact between the hot water stream tracted from the plant by reducing In general, the larger the tower, the
and air. As air rises inside the tower, the CWR temperature to the CWS smaller is the approach. In this case
it receives the latent heat of vapor- temperature. study, the approach is 4C.
Theoretically, the extent of maxi- Components of the system:
1. Sump
Outlet air
eL = 132,000 kg/h
mum possible cooling that could be 2. Pump DBT (Tout) = 41.5oC
achieved through a cooling tower 3. Fan WBT (Tw,out) = 41.5oC
4. Spray nozzles Yout = 0.053 kg of water/kg of dry air
would be to produce a stream that 5. Fills Hout = 178 KJ/kg of dry air
Gout = 4,948,942 kg of air/h
is at the wet-bulb temperature of out = 1.09 kg/m3
the ambient air. However, to achieve
this theoretical maximum, the
3
tower would need to have infinite Inlet air Lin = 7,500,000 kg/h
G' = 4,699,850 kg dry air/h 4 tin = 45oC
height. So the practical limit of the DBT (Tin) = 30.3oC
CWS temperature is generally con- WBT (Tw,in) = 29oC Cooling-water return
Yin = 0.02492 kg water/kg dry air
sidered to be 4C above the wet-bulb Hin = 93.95 KJ/kg of dry air 5
temperature of ambient air. For Gin = 4,816,970 kg air/h
Cooling-water supply
in = 1.148 kg/m3
design purposes, the worst sce-
nario that is, the summer season Lout = 7,368,000 kg/h
tout = 33oC
wet-bulb temperature needs to 1
be considered. Makeup water Cooling-water flow to
Range (T). The range is the differ- exchanger
Lm = 165,000 kg/h
tm = 33oC Heat load
ence between the water tempera- 2 Q = 105 MW
tures at the inlet and the outlet of the Pump flow Cold blowdown
cooling tower (tin tout). In this case, Hot blowdown
Lp = 7,533,000 kg/h Lp = 33,000 kg/h
the range is 12C. The range does tp = 33 oC tp = 33 oC Lb = 0 kg/h
tin = 45 oC
not represent the cooling tower ca-
pability; rather, the range is based on FIGURE 2. This schematic diagram depicts the parameters of the case study cooling tower system.
the cooling-water circulation flowrate Note: All three cells and three fans are lumped together and shown as a single unit
(Lin), and the sum of the heat loads
taken from the heat exchangers in Use Equation (3) to apply a mass
the process unit (Q), and it is not re- balance for the entire section of (5)
lated to the size or capability of the tower. As shown in Equation (3), the
cooling tower. On the other hand, an amount of water evaporated (eL) in
increase in range will cause an in- the down-pouring liquid is the dif- Solving both mass and heat bal-
crease in approach, if all other conference between the inlet liquid flow ance equations [Equations (3) and
ditions are not changed. The range (Lin) and the sum of the outlet liquid (5)] simultaneously, the evaporation
is shown in Equation (1): flow (Lout) and the drift loss (dL). It is
equal to the difference of moisture
content of air across the tower. NOMENCLATURE
(1)
cw = Specific heat of water, kJ/kgK
dL = Drift loss, kg/h
Cooling tower efficiency (). The (3)
eL = Evaporation loss, kg/h
cooling tower efficiency is the ratio of
G = Air flowrate (wet), kg of air/h
actual cooling (range) to the theoreti- Where:
G' = Air flowrate (dry), kg of dry air/h
cally possible maximum cooling (that G' = the quantity of dry air flow
h = Water enthalpy, kJ/kg
is, when the approach is zero), as (which remains the same at the inlet
H = Moist air enthalpy, kJ/kg
shown in Equation (2): and outlet air streams), kg of dry air
L = Liquid flowrate, kg/h
Y = absolute humidity, kg water/kg
OL = Other losses (seal leak, pipe leaking,
dry air/h
and so on) in the system, kg/h
(2) The subscripts in and out refer to the
Q = Heat load, kW
entry and exit locations.
t = Water temperature, C
Theoretically, an approach of The overall energy balance is given
T = Air temperature, C
zero means the tower is 100% ef- by Equation (4):
Y = Air humidity, kg water/kg of dry air
ficient. Industrial cooling towers = Moist air density, kg/m3
typically have an approach tem- o = Latent heat of vaporization of water,
perature between 4 and 8.5C, (4) kJ/kg
and an efficiency between 70 and = Cooling tower efficiency, %
75% [2]; in this case, the efficiency Where: T = Range, C
is 75%. h = the liquid enthalpy, kJ/kg water Subscripts
H = the moist air enthalpy, kJ/kg d = Drift water
Evaporation loss and air needs dry air b = Blowdown
Method 1. The evaporation loss Substituting Lout from Equation (3) in = Inlet location
and air flow requirement through the into Equation (4), and assuming the m = Makeup water
tower can be evaluated by solving enthalpy of the drift water hd is hout, out = Outlet location
the mass and energy balance equa- and simplifying Equation (4), one p = Pump
tions simultaneously. gets Equation (5): w = Wet-bulb temperature

we
ratio of latent heat transferred (eLo)
t-b to the total heat released from the
ulb Exit
tem air
per
atu Latent heat water side is shown by on the left in
re, oC and mass the Equation (6), and this expression
transfer
is numerically equal to the ratio of la-
Specific humidity, Kg water/Kg dry air

HB tent heat added to the dry air to the
B YB total heat gained by the air, which is
we
t-b Ente shown on the right side in the Equa-
ulb rin
tem g a
per ir
tion (6):
atu
re, oC
HA
(6)
C YA
A
From Equation (6), eL is calculated
E D YD as 132,000 kg/h. It is to be noted
that in this method, the dry air flow
Sensible heat (G') is not required. Once eL is evalu-
transfer ated, G' is estimated from the mass
balance equation [(Equation (3)]. The
Dry-bulb temperature, oC
split of latent heat transfer and sen-
FIGURE 3. In this psychrometric chart, the relevant process condition from the case history is marked as sible air heating in this case is about
vector AB 85% and 15%, respectively.
loss (eL) and the dry-air require- the inlet air. But in the case of DB, Makeup water and blowdown
ment (G') are estimated as 132,000 the dry-bulb temperature of air is Makeup water (Lm) is added to the
kg/h and G' = 4,699,850 kg dry decreased and thus the air is cooled sump to compensate for the water
air/h, respectively. at the exit. In both cases, the wet- losses in the circuit. The water losses
Method 2. Depending on the tem- bulb temperature of the exit air will include evaporation loss (eL), drift
perature of the inlet air (whether it always be increased compared with loss (dL), blowdown (Lb), and other
is hot or cold), the air can be either that of the inlet air. So, the water leakage losses (OL) in the system,
heated or cooled as it travels along flowing through the cooling tower such as losses from the pump seal,
the height of a cooling tower. In the can be cooled by unsaturated air, ir- piping leak, washdown water and fil-
psychrometric chart shown inFig- respective of whether the air is hot ter backwash.
ure 3, the entering condition of the or cold.
air is denoted by point A, and the In this case study, from the field (7)
exit air (which is completely satu- measurements of DBT and WBT,
rated with water) is denoted by the psychrometric properties, such Drift loss. Small droplets that are
point B. The enthalpy difference of as absolute humidity, saturation hu- entrained by the upward-flowing air
dry air is (HAHB). The vector AB midity and moist air enthalpy for the stream are collected in a mist elimi-
is the sum of the two components. inlet air and the outlet air, could be nator, where they accumulate to
The horizontal component AC rep- evaluated. The inlet air is marked as form larger drops that are eventually
resents the sensible heating of air, point A, and the outlet air is marked returned to the fill. In general, very
and the vertical component CB is as point B in the psychrometric little water in the form of droplets is
the latent heating of air. In a cool- chart. Another hypothetical point C carried along with the air, but those
ing tower, it is also possible to is marked in such a way that it has a droplets do results in water loss,
cool the air if the inlet air condition dry-bulb temperature similar to point called drift loss or windage loss.
is at D [3]. At point D, the air is hot B and absolute humidity similar to This drift water typically contains dis-
and dry, when compared to the air point A. It must be noted that the solved solids and may cause stain,
at point A. point C is a hypothetical and does corrosion or damage to nearby
The component DE is the sensible not correspond to any location in the buildings and structures. Drift loss is
air cooling, and the component EB is cooling tower; the point C is marked usually about 0.10.3% of the circu-
the latent heating of air. The net heat on the chart to see the horizontal lation water rate (Lin).
received by the air is the difference and vertical component of vector To compensate for the evapora-
between the latent air heating and AB. Moist air enthalpy for point C is tion loss and drift loss, additional
the sensible air cooling. calculated. makeup water is added. Since the
In the case of the AB process, the The total heat gained by the air makeup water typically contains dis-
dry-bulb temperature of the air is (HBHA) has two components: the solved solids, these solids are typi-
increased at the exit that is, the latent heat transfer (HBHC), and the cally left behind in the sump water
exit air becomes hot compared to sensible heat transfer (HCHA). The as the water evaporates in the cool-
350,000
ing tower. Meanwhile, since the
cooling water is a very effective air Makeup water requirements, kg/h
scrubber, dust and debris present in
300,000
the up-flowing air is washed out by
down-pouring water and collects in
the sump. As solids accumulate in
250,000
the sump, they increase the poten-
tial for scale corrosion and biological
fouling in the cooling-water circuit.
Makeup water, kg/h

200,000
By taking small amounts of water
continuously from the cooling tower
circuit (blowdown), the concentra-
150,000
tion of dissolved solids in the cool-
ing water can be reduced below the Evaporation loss, kg/h
upper limit of the acceptable range,
100,000
in order to meet the cooling-water
quality specification of the plant.
Blowdown. There are two ways
50,000
to remove the blowdown as hot
blowdown and cold blowdown (Fig- Drift loss, kg/h
ure 2). Hot blowdown refers to the
0
continuous removal of water in the 0 2 4 6 8 10 12 14 16 18 20
Cycle of concentration (CC)
cooling-water-return line to the ef-
fluent. Since the water is hot at this FIGURE 4. Makeup water requirements versus the cycle of concentration are shown here
location, hot blowdown may not be
acceptable in some applications due Equation (11): are calculated using Equation (11)
to potential environmental impact; and Equation (12), as 33,000 kg/h,
in other cases, it is desired, since it (10) and 165,000 kg/h, respectively. Fur-
reduces throughput to the cooling ther, assuming 0.2% drift loss and no
tower and increases overall cooling system leak, makeup water needs to
performance. be considered as 180,000 kg/h. n
Cold blowdown refers to the con- (11) Edited by Suzanne Shelley
tinuous removal of water from the
cooling-water pump outlet to the ef- Further, the amount of makeup References
fluent [4]. Drift loss and any leakage water needed is estimated, including 1. American Petroleum Institute, Programme in Learning
loss from the system are also con- drift, using Equation (12): Operating Techniques Cooling Towers, 1995.
sidered as blowdown, since these 2. Huchler, L., Cooling Towers, Part 2: Operating, Moni-
toring and Maintaining, Chemical Engineering Progress,
streams contain dissolved solids (but Oct. 2009.
such losses are unintentional). 3. American Society of Heating, Refrigerating and Air Condi-
The amount of water blowdown (12) tioning Engineers, ASHRAE Handbook, Chapter 39
is established by calculating the HVAC System and Equipment, 2008.
cycle of concentration (CC), which The required makeup water mainly 4. Smith, R., Chemical Process Design and Integration,
is defined as the ratio between the depends on evaporation loss and John Wiley & Sons Ltd., 2005.
amount of solids dissolved (mostly the CC calculated above. It is to be
chlorides) in the blowdown and in noted from Equation (11) that the Author
the makeup water, using Equation minimum value of CC to be consid- Uthirapathi Vengateson is a se-
(8): ered is 2, which requires blowdown nior process design engineer at
National Petrochemical Co. in
to be at the same amount of water Yanbu, Saudi Arabia (Phone:
as the amount lost in evaporation. +966 534878029; Email:
(8) Any attempt to reduce the CC below uvengateson@natpetpp.com,
2 results in a significant amount of drvengateson@gmail.com). For
17 years, Vengateson has been
makeup water, as shown in Figure 4. involved in process engineering
Assuming drift loss and leakage Higher CC means that Cm tends design, research and develop-
losses are negligible, and solving to zero (indicating good quality of the ment, and commissioning of chemical and petrochemi-
cal plants. Prior to this, he worked in Lurgi India Com-
the water-balance shown below in makeup water). But, this is achieved pany Ltd. in New Delhi, India. Vengateson earned a
Equation (9): at the cost of water treatment of the bachelors degree (B.Tech.) in chemical engineering
source water. A typical cycle of con- from Madras University, a masters degree in petroleum
refining and petrochemicals from Anna University, and a
(9) centration (CC = 5) is considered in Ph.D. in chemical engineering from Indian Institute of
this case study for the optimum re- Technology, New Delhi, India.
The dissolved-solids balance quirement. Based on the evapora-
shown below in Equation (10), tion loss and cycle of concentration,
the blowdown is calculated using cold blowdown and makeup water

2nd Annual
BULK SOLIDS
HANDLING WORKSHOP
Best Practices for Challenges, Safety & Solutions
Thursday, September 14, 2017 | Sky Philadelphia | Philadelphia, PA
Solids handling problems can be difficult to solve without some understanding of
why they occur. This one-day workshop tackles the basics of several key areas,
including the flow of solids, characterization of solid particles, safety concerns
for combustible dust, and fundamentals of pneumatic conveying.
Come learn the fundamentals of solids handling

from industry experts at the 2nd annual
Bulk Solids Handling Workshop.
chemengonline.com/bulksolids
Register by July 8 for $795! A $100 savings!

Solids Processing
special advertising section
CHEMICAL
ENGINEERING
ESSENTIALS FOR CPI PROFESSIONALS
Size reduction, packaging, conveying, drying, sampling, pastillation, level measurement,

mixing, weighing, and troubleshooting feature in this months solids handling showcase
H andling and processing solid materi-

als in the form of granules, powders,
pellets and pastilles has always been a key Inside:
part of the chemical engineering toolkit.
BEUMER 71
This special advertising section highlights
just a few of the many ways particulates are Charles Ross & Son Co. 70
transferred, processed, and packaged. CR Clean Air Group 72
On the following pages you will find a Dynamic Air 73
twin-shaft mixer featuring a central fluidized
zone; fluidized-bed dryers; dispersers for EKATO 75
mixing powders efficiently into liquids, and Endress+Hauser 69
IMAGE: DAVID STANLEY / FLICKR
venturis for removing particulates from gas Flexicon 70

streams; powder sampling systems; a jet
mill for ultrafine powders; systems to turn GEA 71
viscous melts into free-flowing pastilles; Jenike & Johanson 74
and radar level measurement devices with Material Transfer & Storage 74
long range and high accuracy. Alongside
Sandvik Process Systems 75
Wood chips, shown here, are just these dedicated operations are also a num-
one of the thousands of granular ber of companies offering a broad range of Sentry Equipment 72
materials produced or consumed by expertise in conveying, weighing, packing, Sturtevant 73
the chemical process industries and palletizing solid materials.
Get on the right wavelength

Endress+Hausers level measurement range
offers the right answer for each application
E ndress+Hauser has completed its radar level measurement port-

folio with the new Micropilot FMR60, FMR62 and FMR67. The
Micropilots are the first 80 GHz instruments to follow the safety-by-
design concept and to be developed according to IEC 61508. They
are also the first level instruments to support Heartbeat Technology,
as already used in many of the companys flowmeters. A full range of operating frequencies makes
At the beginning of 2016 Endress+Hauser launched the it easy to choose the best one for each application
Micropilot NMR81, the first high-accuracy instrument based on
80 GHz technology for tank gauging in chemical, oil and gas applica- gauges allows documented verification of every measured value, as
tions. Now the company has introduced the Micropilot FMR6x mod- well as facilitating trend recognition by collecting data for predictive
els, which promote safety and simplicity alongside high accuracy. maintenance. Automatic test protocols and a guided SIL proof test
For the first time, an 80 GHz process radar is available that fol- ensure that each instrument meets standards for safety and accu-
lows the safety-by-design philosophy, thus making customers lives racy at all times.
easier in terms of safety. The new products also offer a wide selec- Endress+Hauser uses the slogan 113 GHz + Your Wavelength
tion of Ex approvals. for its radar technology to emphasize how individual custom-
Improved focusing of the radar signal as well as dynamic pro- ers needs are best met by a full range of frequencies (see image,
cessing algorithms provide reliable, stable measurements with above). 1 GHz, for example, is used for guided radar in applications
a range of up to 125 m and an increased measuring accuracy of involving foam and liquids of low dielectric constant. 6 GHz is best
1 mm. Measurements are unaffected by baffles or other obstacles for turbulent liquids and heavy condensation. 26 GHz provides tight
on the tank walls. Thanks to the innovative antenna design, the focusing and is suitable for 90% of applications, even those in-
system also ignores product buildup and condensation. Interactive volving turbulence. 80 GHz provides the best focus (a 3-deg. beam
software makes commissioning fast and easy. angle), a measuring range of up to 125 m, and the highest accuracy.
Instruments with their own pulse the so-called Heartbeat In the end, radar is not the best solution for every application.
Technology have so far appeared mainly in Endress+Hausers flow Endress+Hauser therefore offers a complete portfolio of level mea-
measurement range. The addition of Heartbeat to the new radar surement technologies. www.yourlevelexperts.com/en

Solids Processing 2017 Special Advertising Section
Ultra-high speed powder dispersion made simple

Ross SLIM Technology employs high shear for rapid and complete mixing of powders into
liquids, avoiding agglomerates and dust formation
T he Ross Solids/Liquid Injection Manifold (SLIM) is a technol-

ogy for dispersing challenging powders like fumed silica, gums,
thickeners and pigments using a specially modified high shear
rotor/stator generator.
In both batch and inline designs, the SLIM is easy to retrofit
into almost any process. In an inline set-up, the SLIM mixer pumps
liquid from the recirculation tank while simultaneously drawing
powders from a hopper. As the liquid stream enters the rotor/sta-
tor assembly, it immediately encounters the powder injection at the
high shear zone. The mixture is then expelled through the stator at
high velocity and recirculated back into the tank. In just a few short
turnovers, solids are completely dissolved or reduced to the desired
particle size. Ross Inline SLIM powder
This method for high-speed powder injection is ideal for dispers- induction mixer with built-in
ing small concentrations of hard-to-wet solids like CMC or xanthan control panel mounted on a
gum (>5%). It is equally effective for solid loadings as high as 70%, portable cart with work bench
as in the case of titanium dioxide or magnesium hydroxide slurries.
By introducing solids sub-surface where they are instantly sub- flowmeters, load cells, solenoid valves, level sensors and thermo-
jected to vigorous agitation, issues like floating powders, excessive couples all integrated into a PLC Recipe Control Panel. Each ingredi-
dusting and formation of stubborn agglomerates (fish eyes) are ent addition and process step can be pre-programmed so that mixer
eliminated. Because the SLIM generates its own vacuum for powder speed, mixing time, temperature, composition and batch weight are
induction and does not rely on external eductors or pumps, it is free accurately replicated in every run.
of clogging and simple to operate. Established in 1842, Ross is one of the worlds oldest and largest
Several models are available including automated skid packages manufacturers of process equipment, specializing in mixing, blend-
where the SLIM mixer is piped to a jacketed tank and supplied with ing, drying and dispersion. www.highshearmixers.com
Handle virtually any bulk solid material

Flexicon stand-alone equipment and automated plant-wide systems convey, discharge,
condition, fill, dump and weigh batch bulk materials dust-free
F lexicon engineers and manufactures a broad range of equip-

ment that handles virtually any bulk material, from large pellets
to sub-micron powders, including free-flowing and non-free-flowing
products that pack, cake, plug, smear, fluidize, or separate.
Individual bulk handling equipment includes: flexible screw con-
veyors, tubular cable conveyors, pneumatic conveying systems,
bulk bag dischargers, bulk bag conditioners, bulk bag fillers, bag
dump stations, drum/box/container dumpers, and weigh batching/
blending systems. Each of these product groups encompasses a
broad range of models that can be custom engineered for special-
ized applications, and integrated with new or existing upstream and
downstream processes and storage vessels.
All equipment is available to food, dairy, pharmaceutical and in-
dustrial standards.
For large-scale bulk handling projects, Flexicons separate
Project Engineering Division provides dedicated Project Managers
and engineering teams on four continents to handle projects from
concept to completion. Working with each customers preferred en- Flexicon offers stand-alone bulk handling equipment as well as
gineering firm or directly with their in-house team, Flexicon adheres plant-wide systems integrated with new or existing processes
strictly to the customers unique standards, documentation require-
ments and timelines through a single point of contact, eliminating and study the performance of new designs.
the risk of coordinating multiple suppliers. In 2015 the company doubled the size of its manufacturing fa-
Flexicons worldwide testing facilities simulate full-size customer cility and world headquarters in Bethlehem, PA, and also operates
equipment and systems, verify performance prior to fabrication, manufacturing facilities in Kent, United Kingdom; QLD, Australia;
demonstrate newly constructed equipment for visiting customers, and Port Elizabeth, South Africa. www.flexicon.com

Fluidized-bed drying, cooling and granulation

GEA is an expert in the design and manufacture of fluidized-bed dryers, coolers and
granulators, including versions for high temperatures and large throughputs
F luidized-bed dryers, coolers and granula-

tors are used for the controlled removal
of residual moisture from powder, crystal-
expansion for each dryer module, enabling
GEA to offer high-temperature fluidizers
with bed areas exceeding 100 m2.
line and granular products. Fluidized-bed A unique mechanical flex design ensures
processing is characterized by gentle dry- minimum thermal and mechanical stress in
ing, cooling or granulation over extended the construction. The use of multiple drying
product residence times. The gentle but in- zones guarantees optimum drying condi-
timate contact between the drying/cooling tions, while a tailored feed inlet spreader
gas and the product ensures minimal attri- design ensures trouble-free back-mixing of
tion and dust creation. moist product in the inlet section. The fluid-
GEA continuously develops its fluidized- izing plate itself, which is of a special pat-
bed drying technologies to meet the re- ented design that GEA refers to as the Gill
quirements for optimum design across an Plate, is tailor-made for each application to
expanding range of applications. This devel- ensure efficient movement of solid mate-
opment, which has been going on for many rial. Combined with the underflow discharge
years, has reached its current high standard design of the dryer, this ensures that the
based on feedback from more than 1,000 fluidized bed is continuously self-emptying
industrial fluidized-bed installations around during operation.
the globe and more than 30,000 pilot tests Attention to airflow and thermal expansion GEA specializes in supplying tailor-made
carried out in GEAs drying test center. lets GEA create fluidized beds up to 100 m2 industrial drying systems. The GEA compre-
The choice of the optimum GEA fluidized- hensive product range for industrial dryers
bed technology depends on the flowrate minerals industries, GEA has developed a includes fluidized-bed dryers, spray dry-
and properties of the raw material and high-temperature fluidizer design giving ers, flash dryers, ring dryers, rotary dryers,
the utilities available. For large-scale optimum energy efficiency. The special spray congealing plants, and spray drying
drying, such as in the agrochemicals and mechanical design allows free thermal absorption plants. www.gea.com
Securely bagged and wrapped

BEUMER supplies complete packaging lines for the chemical industry: from bag filling,
through palletizing, to shrink wrapping of finished pallets
section to the BEUMER fillpac FFS (form
fill seal) system (photo, left). This bagging
machine is fitted with an integral, high-
precision weigher that ensures the accu-
racy of the bag weights. High-performance
palletizers from the BEUMER paletpac
range then stack the bags on pallets quickly
and accurately. Depending on the product
requirements, the palletizers are fitted with
rotary-clamp or double-belt turning devices
to move the filled bags into the required po-
The BEUMER fillpac FFS: High sition. Even bags filled with granulate can
throughput, availability and a compact be palletized gently, remaining dimension- Many companies in the chemical industry
design are key features of the system ally stable when stacked. are using the stretch hood process to
Finally, customers use high-performance reduce transport damage and meet
T he BEUMER Group supplies complete

packaging lines which fulfill the complex
requirements of manufacturers in the chem-
packaging systems in the BEUMER stretch
hood series (photo, right) to secure the
load. For businesses in the chemical indus-
more exacting logistical demands
packaged goods, including barcode scan-

ical industry. These include highly efficient try, efficient packaging of palletized goods ning. If a cover film is additionally placed
filling, palletizing and packaging systems. is a crucial competitive factor. The film fits over the top of the pallet, the goods are pro-
Customers also get comprehensive support. snugly over each product on the pallet, en- tected from all six sides.
When the BEUMER Group implements suring safe transport and good load stabili- Customers get a complete solution from
a packaging line in the chemical industry, ty. The film is highly stretchable and secures a single source and have a reliable point of
here is how it typically works: The bulk ma- the material as it contracts. It is also very contact for the whole job, BEUMER notes.
terial passes from the silo along a conveyor transparent and permits a clear view of the www.beumergroup.com

Repeatable sampling for bulk solids

Sentry Equipments PR sampler automatically takes samples
of free-flowing products from pneumatic conveying lines
D esigned to eliminate the degradation

of product, the Sentry Model PR takes
point samples of free-flowing material from
The ability to get a sample when-
ever desired, in the volume
desired, in the same man-
dilute- and dense-phase pneumatic con- ner every time is a benefit
veying lines. The PR takes a sample when a for control efforts to ac-
solenoid-controlled air cylinder operates a curately diagnose process performance. The PR sampler is a flexible quality
reciprocating probe into the product flow. Automated sampling removes the unknown control solution that is ideal for
This sampler is suitable for pellets, pow- of whether a sample was taken properly products such as polymer pellets
ders, flakes and granules. and at the time required.
The PR sampler features a retractable For example, when polyethylene pellets allows the sampler to collect samples auto-
probe design that isolates process pressure are manufactured, each batch is sampled matically at a preset rate.
from the sample container. The sample tube a number of times for quality control, with Using the batch option on the sampler
and auger capture a fixed sample volume. the first sample needed to continue running controller, a facility can continuously collect
The sample probe retracts from the line to the process. In this application, a Sentry PR composite samples representative of the
avoid any restriction in the product flow sampler is mounted in the conveying lines process over the course of time. This reduc-
between sample cycles. It enables rapid before they exit the building to loadout. es waste as well as the possibility of over-
cycling to acquire a large volume of sam- The samplers automation is controlled filling the sample container, which could
ple over a short period of time. A standard by a Sentry P2B-4/7 sampler controller. result in wasted product or a spill.
purge port assures full sample discharge. Using the sampler controller, an opera- By implementing a Sentry PR automatic
The PR features rugged stainless steel tor can gather the first required sample by sampling solution within their processes,
construction with optional sample tube pressing the hand option as many times plastics manufacturers can improve efficien-
materials for abrasive or non-free-flowing as required to collect the needed sample cy and gain confidence that their sample
products. Its controllers and remote oper- volume. The operator then changes the analysis results are based on truly repre-
ating modules are available in a variety of container, places the sampler controller in sentative product samples.
configurations. auto, and utilizes the batch option. This www.sentry-equip.com
Venturi scrubbers remove particulates reliably

Venturi scrubbers from CR Clean Air offer a robust way to remove particulates and acid
gases from gas streams, with high-energy versions able to tackle particles below 1 m
C R Clean Air offers a wide range of jet

venturis and high-energy venturis to
remove particulate materials from gas
bing liquid. Both fixed- and variable-throat
designs are available, and removal rates as
high as 99.9% can be realized. High-energy
streams. The companys jet venturis remove venturis are the technology of choice for
any particles larger than 1 m, plus acid wet removal of submicron particulates, and
gases such as HCl and SO2. The venturis compare favorably to the cost of a compara-
themselves are often sold complete with ble wet electrostatic precipitator (WESP).
vapor/liquid separator tanks. Since large CR Clean Air offers its high-energy units
liquid-to-gas ratios are needed to maximize complete with cyclonic separators. The
performance, the scrubbing liquid is gener- company can also provide full systems, in-
ally recirculated from the tank back to the cluding an exhaust fan and liquid recircu-
venturi. The jet induces a small increase in lation pumps, skid-mounted with valves,
gas differential pressure, eliminating the instruments and controls. Both metallic and
need for an exhaust fan to pull it through FRP constructions are available, and each
the scrubbing system. system is customized around the require-
For smaller particulates, the companys ments of the process.
high-energy venturis can be used (photo, The company has over 50 years of ex-
right). These units impart a large pressure perience spanning a wide range of indus-
drop (as much as 60 in. w.c.) on the gas in tries, from chemicals to pharmaceuticals,
order to force the particulate into the scrub- and semiconductors to refineries, with
thousands of installations worldwide. So
High-energy venturi scrubbers like this whether you need a jet venturi, high-energy
one, shown complete with separator tank, venturi or even a packed tower, CR Clean Air
compare favorably with wet electrostatic has the solution to your emission control
precipitators on sub-micron particulates challenge. www.crcleanair.com

Creating free-flowing powder to boost energy storage

The Micronizer jet mill from Sturtevant relies on particle-on-particle attrition to cause
particle size reduction that boosts power capabilities within batteries
T o create powerful batteries, energy stor-

age manufacturers need to increase the
surface area of the lithium- or carbon-based
the lithium or carbon being milled.
The Micronizer utilizes a unique fluid
energy grinding system to generate parti-
materials that act as electrolytes between cle-on-particle impact without raising tem-
the positive and negative electrodes. During peratures that could damage the material
size reduction, it is critical that the lithium being milled. Its high-performance design
or carbon not become contaminated and surpasses the economical fineness limit of
maintain its purity for the final product. The mechanical grinders.
Sturtevant Micronizer brand jet mill reduces Sturtevant can solve the most chal-
the particle size of lithium and carbon pow- lenging wear and contamination problems
ders without contamination or heat buildup. using interchangeable wear-resistant liners
The Micronizer employs high-pressure such as PureLine, ShieldOx, and ArmorLine,
compressed air, steam, or other gas to dis- and specifically engineered coatings like
perse and deagglomerate the particles. It Lubriguard to provide contamination-free
consistently produces low-micron-sized par- wear protection and enhance product qual-
ticles whose chemical reactivity is increased ity and throughput.
compared to larger particles thanks to their Sturtevant offers a fully equipped test
far greater surface area. facility for conducting customer trials with
The Micronizers open manifold design the objective of determining the optimum The Sturtevant
allows complete access to the internal ma- equipment and system layout for each ap- Micronizer jet mill
terial grinding chamber and compressed air plication. Sturtevant invites customers to yields particle sizes
chamber for easy cleaning, product change- witness testing while determining the best down to 0.25 m. Its
over, or inspection. There are no dead zones way to achieve fine particle sizes and un- use of fluid energy
to trap material, no moving parts, and no derstand grinding characteristics. allows it to out-perform mechanical grind-
grinding media or lubricants to contaminate www.sturtevantinc.com ing systems without risk of contamination.
Fast, homogenous mixing

The Bella XN fluidized zone mixer from Dynamic Air is a twin-shaft design that uses a
weightless central fluidized area to provide thorough yet gentle mixing of dry products
ing times of 1530 s. A weight- ZONE A
ZONE B
wise direction at the perimeter
less zone created by low-speed while simultaneously moving
counter-rotating paddles gener- both left and right in the cen-
ates low friction without shear. ter (Figure 2). The material in
This makes it ideal for abrasive Zone B (Figure 1) is in its nor-
products and fragile products mal gravimetric state as it is
that cannot tolerate rough han- being moved and dispersed.
dling. Even flakes or spray-dried In Zone A, a weightless zone is
bodies remain intact. created which effectively lifts
The Bella mixer consists the ingredients to an almost
of twin drums which have two weightless state, allowing them
counter-rotating agitators with to move freely and randomly,
specifically angled paddles. The regardless of particle size and
The twin-shaft Bella mixer paddles sweep the entire bot- density. Thus the two zones
tom of both mixer drums and interaction becomes highly ef-
T he Bella fluidized-zone
twin-shaft paddle mixer
by Dynamic Air achieves fast,
yet allow the mixer to be started
under full load (Figure 1). The
material in the mixer moves
ficient as every particle moves
rapidly to create a highly ho-
mogeneous mix, the key to the
high-capacity, low-shear, preci- in a horizontal counter-clock- Bella mixer mixing technology
sion mixing of either dry bulk for fast, precise mixing.
solids or liquids with solids. Figure 1 (right, top): In The Bella mixer is available
Regardless of particle size, Zone A, fluidization promotes in stainless steel and mild steel
shape or density, materials are thorough mixing. Figure 2 construction.
mixed with a fast, efficient, and (right): Material interchange www.dynamicair.com/
gentle action, with typical mix- between the two drums products/mixers.html

A wide range of custom material handling equipment

Material Transfer is a premier manufacturer of custom material handling equipment, with
products including bag conditioners, dischargers, and filling systems
unique combination of application-focused quirements. Material Transfer has a team of
engineering, award-winning designs and talented engineers with the latest 3-D soft-
exclusive features results in equipment that ware for equipment design, professional
offers class-leading quality, value, durabil- metal fabricators and machinists with the
ity, ease of use, and performance. latest fabrication and CNC machining tech-
Equipment is fully assembled, inspect- nologies, and an experienced team of ma-
ed, and factory tested prior to shipment to chine assemblers to build its products.
ensure reliable performance and customer Material Transfers product line includes:
satisfaction, the company says. Material Master Bulk Bag Conditioners to
Material Transfers application experi- quickly and safely return hardened mate-
ence includes pharmaceuticals, food, chem- rials to a free-flowing state (photo);
icals, electronics, aggregate, agriculture, Material Master Bulk Bag Dischargers
foundry, manufacturing, mining, packag- with patented technology to provide
ing, pet food, petroleum, plastics, plating, clean, dust-tight discharge;
stamping, governmental, explosives and au- Material Master Bulk Bag Fillers from
tomotive. Experience in dust-tight handling economical 4-post units to fully automat-
of hazardous materials in hazardous envi- ed, high-output PowerFill filling systems.
ronments, with explosion-proof or intrinsi- Container and drum dischargers to empty
Material Transfers Bulk Bag Conditioners cally safe equipment, has placed Material containers of any size at heights to 40 ft.,
ensure that products are free-flowing Transfer in the forefront of designing and with dust-tight Lift & Seal system or open
building custom material handling equip- discharge, and patented system that al-
M aterial Transfer is an industry leader

in the custom design and manufac-
ture of material handling equipment and
ment for these applications.
Over 95% of the equipment Material
Transfer manufactures is custom-designed
lows 180 rotation.
Integrated systems to meet customers
requirements.
systems for dry powders and bulk solids. A for a customers particular application re- www.materialtransfer.com
Engineered solutions for reliable bulk solids flow

With more than half a century of experience, Jenike and Johanson relies on a strong
technical team to cure or preferably forestall clients problems with powder flow
delivered bulk material engineering solu- material flow can result in limited through-
tions for more than 55 years. put, non-uniform product, dust emissions,
Bulk materials and their flow properties or spillage. Reliable solids handling at
are at the core of all Jenike & Johansons chemicals plants will improve operations
work. Every project (7,500+ to date) is truly involving blending, extrusion, pneumatic or
unique, and clients are offered maximum mechanical conveying, and heating or cool-
flexibility in selecting services to meet their ing. Reliable powder flow and a first-in, first-
bulk material handling needs. Decisions out vessel discharge pattern (mass flow)
made during the feasibility and engineering minimizes cross-contamination between
stages of a project are critically important batches and maximizes process efficiency.
for success. If bulk solids systems are not Jenike & Johanson offers a wide range
engineered from the outset to handle the of services to effectively support any engi-
unique characteristics of the materials, pro- neering project in the chemical industry:
Skilled technical staff have always been cess start-up can be significantly delayed on-site audit to review problems;
key to Jenike & Johansons success and design capacity may never be reached. raw, intermediate, final grade flow testing;
The engineers at Jenike & Johanson are storage vessel, chute, and feeder design;
J enike & Johanson, Inc. is the worlds lead-

ing technology company for bulk material
handling, processing, and storage. The firm
renowned experts in bulk material engineer-
ing. They are frequent keynote speakers at
industry events, routinely deliver webinars
pneumatic conveying testing;
silo structural engineering (new, retrofit);
pilot-scale process modeling.
delivers engineered solutions to achieve re- and customized courses, and publish tech- Whether conveying raw materials from stor-
liable powder and bulk solids flow, based nical articles in top industry journals. age silos to a process, feeding powders to
on proven theories and decades of project 75% of all chemicals are handled in bulk a reactor, or packaging products in bulk,
experience. With a skilled, highly technical solid form during manufacturing. When Jenike & Johanson can help achieve reliable
team of experts and industry-leading inno- feeding powders to reactors or conveying material flow and high throughput.
vations, Jenike & Johanson has successfully wet cake from a centrifuge to a dryer, poor www.jenike.com

Continuous cleanroom pastillation A small footprint

Sandviks Rotoform pastillation system is available in GMP takes a big step
versions for pharma, cosmetic and food applications EKATOs new lab dryers are
A chieving a successful pharmaceutical
audit for cleanroom pastillation requires
trically around the stator. Product droplets
are deposited onto a stainless steel belt.
flexible and versatile
a GMP-compliant production unit with pro-
fessional documentation. The Sandvik
Rotoform granulation system meets this
Indirect cooling via the endless steel
belt eliminates any risk of cross-contami-
nation between product and cooling water,
E KATO SYSTEMS Germany is promoting a
range of desktop-type laboratory-scale
dryers. With working volumes of 36 l, the
while a hot-water-based belt cleaning sys- VPT3 dryers cater to a growing demand for
tem eliminates the risk of cross-contamina- drying tests in vertical apparatus, and also
tion between batches. allow small batches of product to be manu-
All working parts that can come into con- factured. Scale-up is easy because the de-
tact with the product are stainless steel for sign matches EKATOs
easy cleaning and maximum hygiene. The full-scale dryers.
structural materials have a very low surface The base model
roughness. All components (i.e. gaskets) in- in this plug-and-play
Uniform pastillation thanks to Rotoform side the Rotoform are made from materials system is a drying
compatible with the respective product. vessel with a water
requirement and converts liquid melts into The whole machine is covered with jacket for heating
solid pastilles. hoods, with an extractor fan to avoid pol- or cooling. The vari-
Every aspect of the Rotoform system has lution of ambient air. The control system is able-speed motor ac-
been designed to ensure GMP compliance. supported by cameras that transmit images cepts both the EKATO
All piping connections are quick-release to an outside terminal. PARAVISC impeller
types for easy cleaning, and the Rotoform is The Sandvik Rotoform system is widely for free-flowing solids
powered by a maintenance-free drive belt. used across the food, cosmetic and phar- and the EKATO ISOPAS
Rotoform uses a heated cylindrical sta- maceutical industries for products such as impeller for pasty
tor supplied with liquid product, and a chocolate, lipstick and suppository mass. products.
perforated rotating shell that turns concen- www.processsystems.sandvik.com Working pres-
sures range from
1 to +2 bar g.
Vacuum is pro-
Industry events for solids handling vided by a mem-
brane vacuum
and packaging to the chemical process in- pump with con-
dustries. Below is a short calendar of the denser and con-
most important of these events in the U.S. densate vessel.
and Europe this year: Working tempera-
ture is up to 131C.
May 410, 2017 Contact parts
interpack 2017 are made from EKATO VPT3 laboratory
Messe Dusseldorf, Dsseldorf, Germany stainless steel, dryers handle both
May 1011, 2017
SOLIDS Dortmund
with other ma- free-flowing and pasty
Messe Westfalenhallen Dortmund, Germany terials available materials, and are ideal
May 1618, 2017 on request. for process development
Toronto Powder & Bulk Solids Control is
PHOTO: MESSE DSSELDORF/CONSTANZE TILLMANN
Toronto Congress Centre, Ont., Canada

June 1921, 2017
via a touch screen, with an electric motor
Eurodrying 2017 European Drying used to lift the vessel lid. A data logger and
Conference an interface for remote data transfer are
University of Lige, Lige, Belgium available on request.
September 14, 2017
Bulk Solids Handling Workshop
Just like EKATOs production-scale dry-
organized by Chemical Engineering ers, the VPT3 dryers can handle thick paste-
Sky Philadelphia, Pa., U.S. like products just as easily as low-viscosity
September 2628, 2017 suspensions. For shear-sensitive active
POWTECH 2017
Exhibition Centre Nuremberg, Germany
ingredients that require gentle drying, the
September 2729, 2017 EKATO PARAVISC impeller combines uni-
Packaging in action at interpack The 2017 Powder Show & Conference form product circulation with good heat
Greater Columbus Convention Center, transfer. Varying the shaft speed allows ex-
Columbus, Ohio, U.S.
A large number of dedicated exhibitions,
conferences and training sessions
shows the importance of solids handling
October 45, 2017
SOLIDS Rotterdam 2017
Ahoy Rotterdam, Rotterdam, Netherlands.
perimenters to find the operating point that
reliably achieves the shortest drying times
or the best product properties. A rental unit
is available. www.ekato.com

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Economic Indicators
2015 2016 2017
Download the CEPCI two weeks sooner at www.chemengonline.com/pci
CHEMICAL ENGINEERING PLANT COST INDEX (CEPCI)

625
(1957-59 = 100) Jan. '17 Dec. '16 Jan. '16 Annual Index:
Prelim. Final Final
2009 = 521.9 600
CE Index ______________________________________________ 553.0 550.9 536.4
Equipment ____________________________________________ 664.1 661.0 640.5 2010 = 550.8
Heat exchangers & tanks _________________________________ 578.3 573.7 551.7
2011 = 585.7 575
Process machinery _____________________________________ 668.6 667.9 649.3
Pipe, valves & fittings ____________________________________ 835.2 833.9 795.0 2012 = 584.6
Process instruments ____________________________________ 398.5 396.9 378.9 2013 = 567.3 550
Pumps & compressors ___________________________________ 971.3 973.5 979.1
Electrical equipment ____________________________________ 512.6 512.1 509.0 2014 = 576.1
Structural supports & misc ________________________________ 722.4 713.9 701.9 2015 = 556.8 525
Construction labor _______________________________________ 324.0 324.4 319.6
Buildings _____________________________________________ 550.0 547.0 537.7 2016 = 541.7
Engineering & supervision _________________________________ 313.9 313.6 316.6 500
J F M A M J J A S O N D
Starting with the April 2007 Final numbers, several of the data series for labor and compressors have been converted to
accommodate series IDs that were discontinued by the U.S. Bureau of Labor Statistics
CURRENT BUSINESS INDICATORS LATEST PREVIOUS YEAR AGO

CPI output index (2012 = 100) ____________________________________________________ Feb. '17 = 102.5 Jan. '17 = 101.9 Dec. '16 = 101.3 Feb. '16 = 101.9
CPI value of output, $ billions _____________________________________________________ Jan. '17 = 1,872.2 Dec. '16 = 1,861.8 Nov. '16 = 1,785.0 Jan. '16 = 1,672.5
CPI operating rate, % __________________________________________________________ Feb. '17 = 75.1 Jan. '17 = 74.8 Dec. '16 = 74.4 Feb. '16 = 74.9
Producer prices, industrial chemicals (1982 = 100) ____________________________________ Feb. '17 = 244.3 Jan. '17 = 241.9 Dec. '16 = 239.2 Feb. '16 = 219.2
Industrial Production in Manufacturing (2012=100)* ____________________________________ Feb. '17 = 104.5 Jan. '17 = 104.0 Dec. '16 = 103.5 Feb. '16 = 103.3
Hourly earnings index, chemical & allied products (1992 = 100) ____________________________ Feb. '17 = 170.1 Jan. '17 = 169.0 Dec. '16 = 170.3 Feb. '16 = 158.6
Productivity index, chemicals & allied products (1992 = 100) ______________________________ Feb. '17 = 103.0 Jan. '17 = 103.4 Dec. '16 = 103.1 Feb. '16 = 103.1
CPI OUTPUT INDEX (2000 = 100) CPI OUTPUT VALUE ($ BILLIONS) CPI OPERATING RATE (%)
110 2300 80
105
2200 78
100
2100
95 76
2000
90
74
1900
85
72
80 1800
75 1700 70
J F M A M J J A S O N D J F M A M J J A S O N D J F M A M J J A S O N D
*Due to discontinuance, the Index of Industrial Activity has been replaced by the Industrial Production in Manufacturing index from the U.S. Federal Reserve Board.
For the current months CPI output index values, the base year was changed from 2000 to 2012
Current business indicators provided by Global Insight, Inc., Lexington, Mass.
CURRENT TRENDS
FREE On Demand Webinars

T he preliminary value for the January
CE Plant Cost Index (CEPCI; top; the
most recent available) represents a gain
CHEMICAL from the last reading of 2016. With that,
ENGINEERING
ESSENTIALS FOR THE CPI PROFESSIONAL
the annual CEPCI number for 2016 was
calculated to be 541.7, using the aver-
age of the monthly values from the year.
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February 2017 saw an increase in the CPI
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Circle 01 on p. 78 or go to adlinks.chemengonline.com/66427-01 Circle 02 on p. 78 or go to adlinks.chemengonline.com/66427-02

Circle 03 on p. 78 or go to adlinks.chemengonline.com/66427-03 Circle 04 on p. 78 or go to adlinks.chemengonline.com/66427-04

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM APRIL 2017 35

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