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CEP

December 2014

Chemical
Engineering
Progress
An AIChE Publication

Vol. 110 No. 12

www.aiche.org/cep

Contents

DEPARTMENTS

14

4 Update

3 Editorial
Its All About the Culture

; Fossil Fuels Inspire Clean-Hydrogen Catalyst

13 AIChE Journal Highlight


Solving Wicked Sustainability Problems
Requires a New Approach

14 Catalyzing Commercialization
Bioabsorbable Magnesium Alloy Doubles
the Strength of Orthopedic Implants

15 Whats New

; Organic Solar Cells Heat Up


; Biomass Waste Gets Upgraded
; New Technique Puts Catalysts on the Right Track

15

; Silicon Gets Pressured into a New Structure


; Paper-Based Genetic Circuits Diagnose Disease
; A Masquerade: Disguising RNA Drugs
; Beetle Inspires Anti-Counterfeiting Technology

22 Safety

17 Product Digest
Fluids Handling

18 Profile
Perry Romanowski: Formulating
Cosmetics and Educating Millions

17

Consider the Role of Safety Layers in the Bhopal Disaster


As the situation unfolded, numerous layers of protection failed. 
Take a look at the safety layers that worked and those that did not,
and ask whether there are similarities at your facility.

29 Safety

19 Career Corner
Surviving an International Relocation

20 process Safety Beacon


Bhopal The Worst Industrial
Disaster in History

34 Software

19

Apply Cant Rather than Dont to Your Process


Many safety systems rely on human intervention to prevent incidents.
A different approach is to make it impossible for a catastrophic 
accident to occur. Learn how to implement the Cant Rather than
Dont principle.

35 Reactions and Separations

51 Books
52 Institute News
Corner:
Strengthening AIChE For Growth
; N ew Fellows
; D ivisions and Forums Present Awards
; A IChE Election Results
; AIChE Foundation Provides Travel Grants
for Overseas ChE Student Leaders

56 CEP Showcase
57 CEP Marketplace
59 Recruitment Classifieds

40 Back to Basics

34
SO FTW
& INFORM
AR E
ATION
TECHNO
LOGY

SOFTWARE
& INFORMATION TECHNOLOGY

; P residents

Choosing a Fine-Particle Filtration System


Filtration technology has advanced to meet the demand to remove
small particles at low concentrations. When designed correctly, 
a candle filter or a pressure plate filter may be a more-efficient
replacement for a traditional filtration scheme.

51

Avoid Fluidization Pitfalls


Fluidized beds are susceptible to such problems as bed slugging,
loss of fines, and gas bypassing. This article explains how to avoid
these pitfalls.

46 Instrumentation

52

Account for Uncertainty with Robust Control Design Part 2


Robust control can be applied to design controllers that can handle
process uncertainty. Learn how to use identification experiments to
obtain estimates of this uncertainty.

63 Ad Index
64 Calendars

22

Chemical
Process Safety

59
CEP (Publication Number 101-920) (Print ISSN 0360-7275, Online ISSN 1945-0710) is published monthly by the
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646-495-1346. n Each issue of CEP is indexed regularly by Engineering Village and Applied Science & Technology Index;
microfilm/fiche copies of each issue are available from University Microfilms, Inc.

64

Reprinted with permission from Chemical Engineering Progress (CEP), December 2014.
Copyright 2014 American Institute of Chemical Engineers (AIChE).

Reactions and Separations

Choosing a Fine-Particle
Filtration System
Barry A. Perlmutter
BHS-Sonthofen Inc.

Filtration technology has advanced


to meet the demand to remove small particles at
low concentrations. When designed correctly,
a candle filter or a pressure plate filter
may be a more-efficient replacement
for a traditional filtration scheme.

any chemical manufacturing processes, such


as those that make chemicals, petrochemicals,
pharmaceuticals, biofuels, etc., involve reactions
of solid- and liquid-phase reactants to produce a slurry. The
slurry typically needs to be separated into its component
parts the liquid (i.e., mother liquor) and the solid.
The valuable material may be the liquid, the solid, or
both phases. The location of the valuable component to be
recovered determines the type of separation method and
equipment used. For example, if the liquid is the desired
product, the solids are removed as waste to produce a clean
liquid; if the solid is the desired product, removal of small
particles increases the product yield.
Generally, the first step after the reaction is a bulk separation process that removes large, coarse solids (larger than
5 m). This is relatively straightforward, but as processes
have become more sophisticated and quality requirements
have tightened, it has become necessary to remove residual
particle fines from slurries. These particles are small
typically 15 m in diameter, or even smaller and at low
concentrations, on the order of parts per million (ppm).
This article describes clarification technologies used to
remove or recover residual particle fines. A brief overview
of coarse separation equipment illustrates how these systems fit into the realm of filtration technologies. Examples
of installations in chemical, refinery, biofuel, and pharmaceutical plants provide engineers with ideas for evaluating
process filtration problems, as well as potential solutions
based on laboratory testing.

Filtration system categories


A successful solid-liquid filtration system includes a filter medium that retains the solids while allowing the liquid
phase to pass through. Filtration systems are divided into
four categories, based on the driving mechanism or force
behind the separation: gravitational, vacuum, pressure,
and centrifugal.
Gravitational filtration systems use gravity to drive
the separation process, in effect draining the liquid from
the slurry. They are typically continuous, but can also be
operated in batch mode. Because their capital and operating costs are low, they are common throughout the chemical process industries (CPI), but they can be slow and/or
inefficient.
The performance of a gravitational filter can be
enhanced by the application of a vacuum. This is called a
vacuum filtration system because it utilizes the pressure gradient of a vacuum typically produced by a liquid-ring-,
oil-, or dry-vacuum pump to drive the separation. The
thickness of the solid filter cake can be controlled within
a narrow range for optimal solids washing that produces
a high-quality product. Vacuum filters can be operated as
batch systems, but are normally continuous.
In pressure filtration, pressures of 150 psig or higher
are produced by a centrifugal or similar style of pump. The
final cake is usually as dry as can be expected without the
application of heat. All pressure filters are batch-operated
units, with the exception of the rotary pressure filter (RPF),
which has a unique discharge system that enables atmoCEP December 2014 www.aiche.org/cep

35

Reactions and Separations

spheric discharge. Pressure filters allow for excellent solids


washing, and produce high-quality products.
Centrifugal filtration is an alternative to vacuum and
pressure methods. During operation, a basket containing the
slurry is rotated, and the centrifugal force generated separates the liquid and solid phases. Centrifuges can be operated
continuously or in an automated, continuous batch mode.
They are further categorized by the orientation of the basket
and the type of cake discharge. The nature and behavior of
the solids determine the success of centrifugal filtration.

Coarse particle filtration


The choice of a filtration technology (clarification or
coarse) is influenced by the process and the nature of the
product. For example, coarse filtration may not be necessary if the product is a liquid and the solid byproducts are
smaller than 5 m; instead, clarification technologies can be
employed exclusively. Alternatively, if the product is a solid
and the reactor produces particles with a wide size distribution, coarse filtration is necessary.
Coarse filtration systems may operate as either batch or
continuous processes, under the influence of gravity, pressure, a vacuum, or centrifugal force. The method of operation for the filtration system depends on the type of reactor
used, as well as the type of equipment downstream, such as
a batch or continuous dryer.
Some examples of batch process systems include bag
filters, basket strainers, basket centrifuges, cartridge filters,

filter presses, membrane presses, leaf filters, Nutsche filters,


and tube presses. These systems generally operate under
pressure and are designed to handle the entire reactor batch.
The disc filter, rotary pressure filter, pusher centrifuge, rotary vacuum drum filter, and vacuum belt filter are
examples of continuous filtration systems. They are fed
continuously from the reactor or from a slurry holding tank
under liquid level control.

Clarification systems
A clarification system is employed after coarse-particle
filtration, or as a stand-alone system to remove fine particles
at low concentrations. This is accomplished by candle filters
and pressure plate filters, which are both batch-operated,
pressure-filtration systems. The cake structure and the
nature of the process determine which type of clarification
system is appropriate for an application.
Candle filter. A candle filter is a pressure vessel filled
with tubular filters called filter candles (Figure 1). A typical
filter candle is comprised of a pipe to conduct the filtrate
and pressurized gas, a perforated core with supporting tie
rods, and a filter sock (Figure 2). The filtrate pipe runs the
length of the candle and ensures high liquid flow, as well as
maximum distribution of the gas during cake discharge. The
tie rods create an annular space between the filter sock and
the perforated core, which helps to maintain a low pressure
drop during operation and promotes efficient expansion
of the filter sock during cake discharge. The filter sock
Filtrate and Gas
Pipe

Pressure Vessel
Filter Cake

Gas
Inlet

Low-Pressure
Gas
Dry
Filter Cake

Tie Rods

Perforated
Core

Registers

Filtrate Outlets

Filter Sock

Candles

Slurry Feed
Inlet

p Figure 1. In a candle filter, the slurry enters through the


bottom of a pressure vessel and flows across the filter media.
The filter candles are attached to registers that collect the
filtrate. Gas is fed into the top of the pressure vessel for cake
drying and discharge.

36

www.aiche.org/cep December 2014 CEP

p Figure 2. During operation,


filtrate exits from the top of the
candle, while the solids collect on
the synthetic filter sock.

p Figure 3. During discharge, gas is fed into the


top of the candle, which expands the flexible filter
sock. This causes the dry cake to crack and break
away from the filter. The solids are collected at
the bottom of the pressure vessel.

is installed over the candle, and can be made of various


synthetic materials capable of removing particles smaller
than 1 m. As the cake builds during operation, the candle
filters removal efficiency increases, enabling removal of
particles as small as approximately 0.5 m.
The candles are installed in a pressure vessel constructed of stainless steel or another alloy. Within the vessel
are horizontal manifolds called candle registers. Each
candle is connected to a register with a positive seal to prevent bypass. Depending on the filter size, each register may
contain 120 candles. The liquid filtrate and pressurized gas
flow through the register; automated valves ensure optimum
flow in both directions.
During operation, a feed pump or pressure from the reactor or feed tank forces the slurry into the bottom of the pressure vessel. The solids build up on the outside of the filter
sock, while the liquid filtrate flows into the candle, through
the registers, and out of the vessel. This process continues
until the maximum pressure drop, design cake thickness,
minimum flow, or maximum filtration time is reached.
The cake is washed to remove impurities and leftover
mother liquor, and then dried. Next, low-pressure gas enters
the individual candles and expands the filter socks. This
process breaks apart the dry cake, which detaches from the
filter sock (Figure 3) and falls into the vessel cone. The cake
can also be discharged as a concentrated slurry.
Candle filters are used for thin-cake (520 mm) pressure
filtration applications. They are best suited for filter cakes that

are stable vertically because of the orientation of the candles.


Pressure plate filter. Like the candle filter, pressure plate
filters (Figure 4) are comprised of filter elements contained
within a pressure vessel. However, instead of vertical filter
candles, the vessel contains horizontal filter plates.
These elements are slightly sloped, conical-shaped
metal plates that support a coarse-mesh backing screen covered with filter cloth (Figure 5). An opening in the center
of the plate allows the filtrate to travel between plates and
throughout the vessel.
Operation is similar to that of a candle filter. The slurry
enters the bottom of the vessel and is pumped upward. The
solids build up between the plates, while the liquid flows
through the core of the filter plates and exits from the top of
the vessel. The cake is then washed and dried. Two unbalanced motors vibrate or rotate the filter plates to dislodge the
cake from the filter cloth so it can be discharged (Figure 6).
Pressure plate filters are used for filtration of cakes up
to 75 mm thick. They are selected for cakes that are stable
horizontally because of the orientation of the plates.

Clarification technology selection


The structure of the cake determines which system is
better suited for the application. Cakes comprised of crystal
line or hard, irregularly shaped particles are stable when
oriented vertically and are compatible with the vertical filter
elements of a candle filter, whereas very fluffy or dense
cakes are stable when horizontal and need to be handled by
Filtrate

Filtrate Outlet
Motors

So

lid

Filter Cake

Pressure Vessel

Filter Medium

Filter Plates

Backing Screen

Filter Plate

p Figure 5. Each filter plate is covered by a backing screen and filter


medium, which may be metal or a synthetic material. The solids accumulate on the surface of the plate, while the filtrate flows through the core.
Gas
Dry
Filter Cake

Slurry Feed
Inlet

p Figure 4. In a pressure plate filter, the slurry is pumped into the bottom
of a pressure vessel. The solids collect on the filter medium, while the filtrate
flows through the core of the plates and exits through the top of the vessel.
Two unbalanced motors attached to the top of the unit effect cake discharge.

p Figure 6. After drying, the cake is discharged from the plates by


vibration created by two unbalanced motors affixed to the top of the vessel.
Gas is fed into the top of the unit to help push the dry cake off the plates
and to the bottom of the pressure vessel.

CEP December 2014 www.aiche.org/cep

37

Reactions and Separations

the horizontal elements of a pressure plate filter.


The candle filter is limited to cake structures with thicknesses between 5 mm and 20 mm, while a pressure plate
filter can handle thicker cakes up to 75 mm. Both units
can conduct filtration up to 150 psig.
Candle filtration and pressure filtration can remove
13-m particles. In some applications, candle filters can
remove even finer particles, as small as 0.5 m. Both
systems use synthetic filter media, but pressure plate filters
can also use metal media for high-temperature applications
(greater than 200C) or if steaming is required.
If the process requires washing of the solids, a pressure
plate filter is preferred, because the horizontal orientation
eliminates the possibility of the cake falling off the element
during operation. When washing is not critical, a candle
filter may be the best choice for clarification and removal,
since the cake is normally disposed of as waste.
For applications that require cake drying, pressure plate
filters are appropriate because they create cakes that are
as dry as possible without the application of heat. Candle
filters produce cakes with approximately 10% moisture, but
this value depends on the specific cake material.
Clean-in-place (CIP) and sterilize-in-place (SIP) operations can be conducted similarly in both systems. The vessel
is filled with cleaning fluid that is circulated while gas is
blown in the reverse direction, which creates a turbulent
mixture that has a quasi-ultrasonic cleaning effect. Cleaning
of pressure plate filters is enhanced by the ability to rotate
or vibrate the plates.

Clarification system design


Laboratory testing at a constant slurry flow or constant
pressure is used to determine the size and design of a clarification system for processes with extremely low concentrations of solids. The test evaluates the filter media, operating
pressure, and cake thickness to determine the optimum
clarification system design and size.
A lab-scale leaf filter (Figure 7) is used as the test filter.
Various filter media can be installed, depending on the
desired filtrate clarity, filtration flux rate (time), cake thickness, and cake discharge rate, as well as compatibility with
the process. A peristaltic pump supplies a constant flow of
slurry to the filter, and a pressure gage measures the change
in pressure across the filter bed.
A washing analysis consists of running a liquid at the
same flowrate as the test flowrate through the peristaltic
pump, or adding wash liquid to the leaf filter and applying
air pressure until the target quality level is reached.
The cake is then dried with compressed air or nitrogen.
The amount of compressed gas is regulated to prevent the
use of excess air, which could lead to overly optimistic moisture targets that require uneconomical volumes of air when
38

www.aiche.org/cep December 2014 CEP

scaled up. Airflow should be maintained below 10 ft3/hr, but


46 ft3/hr is a good starting range for initial testing.
Once the filtration, washing, and drying times are collected, the data are fit to the following equation and the
constants m and b are determined by least-squares analysis:
2

V
t = m + b
A

(1)

where t is the filtration time (min), m is a derived constant


(m4-min/m6), V is the feed volume (m3), A is the area of the
filter (m2), and b is a derived constant (min).
After rearranging Eq. 1, the area of the filter, A, can be
determined from the feed volume, V, and the filtration time, t.
This test method and subsequent calculations are used
in various applications to determine the appropriate size,
type, and operating time of candle filter and pressure-plate
clarification systems.
Application 1: Replace a manual plate and bag filter
system. A specialty chemicals manufacturer produces
various resins that require filtration. Current production
methods include a neutralization step that yields metal salts,
which are filtered by a manual plate filter followed by a bag
filter for polishing. Two solvent washes after the filtration
step are performed in an attempt to recover as much resin as
possible. After washing, the filters are steamed and opened,
at which point the solids are disposed of manually and the
filter paper is replaced for the next batch.
This two-filter process is inefficient and risks exposing
operators to the heptane used for cake washing.
Lab testing was conducted to determine a processing
scheme that eliminates exposure to heptane, reduces the
maintenance and operation requirements of the two-filter
system, and recovers resin that is as dry as possible. Current
production throughput is 3,000 gal in 45 hr.
The tests determined that one candle filter with 10 m2
of filter area could complete the cycle in 4.3 hr, and would
eliminate the need for the plate and bag filters.
Pressure
Gage
Slurry Feed

Peristaltic Pump
Lab-scale
Leaf
Filter

Beaker
or
Graduated
Cylinder

p Figure 7. Tests to determine the type and size of clarification system


needed are done in this simple laboratory setup. A peristaltic pump controls
the flow of slurry to a leaf filter, while a pressure gage measures the
pressure drop across the filter bed. The filtrate is collected in a beaker or a
graduated cylinder.

Application 2: Replace a filter press for hot slurry


filtration. A chemical manufacturing process that produces
various grades of polyols from ethylene glycols requires
filtration to remove small, 12-m particles. The current
production scheme includes a manual filter press that operates at 200250F. This unit requires frequent filter media
changes and manual cake discharge.
Lab testing was conducted to devise a process that
avoids operator exposure to the glycol mother liquor,
reduces the high maintenance and operating costs of the
filter press, and increases the polyols yield. The current
production scheme handles 45,000-lb batches of slurry.
The tests and calculations determined that one candle
filter with 27 m2 of filter area could complete the required
batch in three 6-hr cycles.
Application 3: Replace a centrifuge and a cartridge
filter for a hydroxide slurry. Amorphous, fine-crystal metal
hydroxide salts are present in a chemical manufacturing
process. The centrifuge and cartridge filters used for filtration do not remove the crystal fines, which cause operating
problems in the downstream plant.
Lab testing was conducted to determine a scheme
capable of removing the fine solids, washing the solids for
recovery, and drying the cake for reuse.
Tests showed that the process could be improved by
replacing the filtration scheme with one 10-m2 candle filter
and a filter aid (an inert material used for pretreatment) to
remove the amorphous crystals and to prevent the filter
socks from blinding.
Application 4: Replace a filter press that uses paper
media. In a specialty oil manufacturing process, a filter press
fitted with paper filter media is used for final clarification of
30,000-lb batches of slurry. The filter aid, diatomaceous earth,
is injected into the slurry to agglomerate the fine solids. The
plant produces several grades of oil, which necessitates cleaning between campaigns. The cake, comprised of the process
solids and filter aid, is dried using nitrogen, and the solids are

nk

Ta
Wash

Clean

ank
mine T

ters
ntrated
ndle Fil
Conce ank Ca
T
y
rr
Slu
Plate

sure
Filter

Pres

p Figure 8. Amines from a refinery or gas plant are effectively filtered in


this two-stage system that combines candle filters to concentrate the slurry
and a pressure plate filter to finish the clarification.

removed and burned in the onsite power plant as fuel.


The process suffers from limitations associated with manual filter presses (e.g., frequent blinding, the need to change
the paper filter media, manual cake discharge), as well as
the safety concerns of processing hot oil. The particles to be
removed are small, with an average size of 0.7 m.
The lab testing demonstrated that the oil slurries could
be filtered using a 10-m2, jacketed candle filter, and that
the oils would meet customer specifications for clarity
and dryness.
Application 5: Install two-stage candle and pressure
plate filters. The fines generated by catalytic crackers and
cokers at refineries and gas plants are generally smaller
than 1 m and are present at very low concentrations. For
large flows of up to about 800 gal/min, bag filters, cartridge
filters, and filter presses are not practical because of the
large filter area and frequent manual changes of bags and
cartridges that would be required.
For this type of application, a two-stage process with
candle filters for concentrating and pressure plate filters for
polishing, cake washing, and drying are used (Figure 8).
This operational scheme increases reliability, reduces
compressed air/gas consumption for drying by 25%, and
reduces the amount of water needed for cake washing.
At a typical refinery, gas, or energy plant, amines (which
scrub sulfur dioxide and carbon dioxide) are filtered to
remove solids from the recirculation stream. The solids are
smaller than 1 m, and the total solids concentration is estimated to be less than 1,000 ppm.
Testing determined that the optimum process solution
was a two-stage filtration system. For an average recirculation process with a flow of 176 gal/min, two candle filters,
each with 19 m2 of filter area, are used to concentrate the
solids. These are followed by two pressure plate filters with
areas of 1 m2 for the final filtration, washing, and drying.

Final thoughts
There are many choices of technologies appropriate for
initial filtration, but these options may not achieve the necessary level of quality. With lab testing and data analysis, a clarification system for fines removal can be designed. Although
these systems incur additional capital expense, they result in
CEP
more reliable, efficient, and optimized processes.
Barry A. Perlmutter is President and Managing Director of
BHS-Sonthofen, Inc. (Email: barry.perlmutter@bhs-filtration.com).
He has over 30 years of technical and marketing experience in the
fields of solid-liquid separation, filtration, centrifugation, and drying.
He has published and lectured worldwide, and is responsible for the
introduction and growth of many European companies in the filtration
market. Perlmutter has a BS in chemistry from the Univ. at Albany, an
MS in environmental science and technology from Washington Univ. in
St. Louis, and an MBA from the Univ. of Illinois at Chicago.

CEP December 2014 www.aiche.org/cep

39