48 www.cepmagazine.

org February 2002 CEP

Reactions and Separations
ingle-stage distillation systems are widely
used in petrochemical, chemical and phar-
maceutical plants. This unit operation goes
by several names, but is often referred to
as a flash drum or evaporator. We will use
evaporator here, with the understanding that we are
not referring to a heat-transfer device, but, instead, to
the entire single-stage distillation system (an adiabat-
ic evaporator system has no source of heat input).
A review of the design and operation of this most
basic unit operation is available in various sources (1,
2) and will not be covered here. However, we need to
ensure that the terminology of evaporators is under-
stood, since there are several design features that are
common to most such processes.
Basic terminology
Evaporators typically employ heat to concentrate
solutions or to recover dissolved solids by precipitat-
ing them from saturated solutions. The scope of our
practical solutions will be primarily evaporators of
the former classification. A typical industrial evapo-
rator has tubular heating surfaces, a vessel to hold in-
ventory and disengage vapor from liquid, and a heat
exchanger to condense the lighter overheads product.
These units can operate at atmospheric or elevated
pressures, but are often run under vacuum to reduce
the system temperature. This unit operation can be
run continuously, semi-batchwise or fully batchwise.
In the pharmaceutical industry, it is our empirical ob-
servation that most evaporations are either semi- or
fully batch. While the product from the evaporation
step can either be the overhead or pot contents, the
solution to be separated is usually either wide-boiling
or has a non-ideal vapor/liquid equilibrium (such as
an azeotrope), which results in a more discreet sepa-
ration between mixture components. Figure 1 shows
a typical evaporator system.
A recent capacity initiative at Eli Lilly uncovered
several varied and creative methods to reduce cycle
time, increase throughput, and/or increase product
quality in our semi-continuous train of evaporators.
These were based on observations of a series of vacu-
um evaporator units that remove and exchange various
solvents from a temperature-sensitive, high-boiling
product stream (dissolved solute or slurry). These im-
provement methods were simplied and generalized to
illustrate select ways to boost capacity or reduce cycle
time in similar batch distillation operations. In most
cases, the practical solutions are applicable to both vac-
uum and atmospheric evaporators, and can sometimes
be extended to continuous units, as well.
Increasing capacity
With a basis established as to what an evaporator
train may look like, as well as the terminology to be
used, discussion can now move into capacity creation
and/or recovery. The question typically posed by man-
agement is: How can we increase our capacity? To
answer this, other questions need to be resolved:
1. By how much do we need/want to increase the
output of our system?
Try these practical ways to boost
capacity, increase product quality
or reduce cycle time in batch
and continuous systems.
Get More Out of
Single-Stage
Distillation
S
Ernest A. Perkins
and Ryan C. Schad,
Eli Lilly and Co.
CEP February 2002 www.cepmagazine.org 49
2. Where are we with respect to system design capacity?
3. Are current process yields optimized?
4. What additional constraints will we need to impose
(i.e., capital, time or regulatory)?
The answers to these and similar questions can lead to
different recommendations and, as such, need to be an-
swered early in the improvement process.
The answers to the first three questions are process
dependent and, consequently, will be different for each
project, while the answer to the fourth may be more de-
pendent on the industry, product or facility. For instance,
we were tasked recently with minimizing process down-
time. Although capital, by itself, was not a limiting issue,
adding capital equipment and the space it needed were
not the best choices due to restrictions on downtime, as
well as the regulatory hurdles.
In the following discussion, it is assumed that the en-
gineers can develop the fundamental knowledge and in-
formation necessary to facilitate the changes discussed.
These include mass and energy balances for the process,
equipment-design specifications, and calculations such
as sizing and rating of heat-transfer and other miscella-
neous equipment. As an example, we had engineers de-
velop rigorous process simulation models using Aspen-
Techs AspenPlus product models for heat and energy
balances and HTRIs IST 2.0 to better understand de-
tailed heat-exchanger rating and design calculations.
For evaporators, areas requiring further study are im-
provements in either the process or the equipment, with a
denite overlap between the two. Depending upon the re-
quired scope of capacity increase, we often found easy so-
lutions to achieve the desired output.
Improving yield
To clarify what is meant by pro-
cess yield calls for understanding
what is important, i.e., What is the
product? In our operations, we
needed to ensure that the ability to
recover the product was not affect-
ed. The product was a solute in a
mixed-solvent stream. The process
yield relates to how much of solute
is lost during evaporation. In other
applications, the product is typically
a solvent in a mixed-liquid feed-
stream, and the yield is the amount
and/or purity recovered.
For most of this article, we will
treat the process yields as defined in
the former case; however, we will
try to provide a few simple alter-
ations that may be useful to those
whose yields are defined more ap-
propriately by the second one. If
yields are low and improving them
by making simple process changes
leads to the desired capacity, then this is an attractive
route to consider.
Product transfer and cleaning
One area examined during our recent project, particu-
larly for batch or semi-batch processes, was eliminating
or minimizing physical product losses due to cleaning in
between batches, or inadequate flushing of precipitated
materials. It may be possible to correct this by simply
changing flushing/cleaning techniques or solvents.
(Flushing is removing the last remaining product from
the equipment.) Again, extending flush time may cut
some capacity by extending cycle time, but it may be
justified in increased yield.
There may be numerous other opportunities for im-
provement here that are process specific, but still worth
the time. Look closely at the product/solute properties. If
the product is sticky, look for a flushing agent (that is
compatible with downstream processes) that will aid in
removing such particles prior to their transfer to the next
process step.
Another area often overlooked when searching for
more capacity, perhaps more-related to specific process
materials than the unit operation itself, is the cleaning-
cycle time. Assess the impact the cleaning cycle has on
the overall cycle time and then investigate what changes
can be made to simply reduce this time. Assess the ap-
propriateness of the cleaning agents, analyze the clean-
ing sequence, the quantities used, etc. Optimize the
water flush/rinse times or volumes to achieve more pro-
duction time. Reducing the amount of idle time increases
I Figure 1. A typical evaporator system with common standard features.
Utility
In
Utility
Out
Utility
In
Utility
Out
Condensate
Pump
Condenser
Vacuum
Source
Condensate
Feed
Bottoms
Recirculation
Pump
Evaporator
Body
VLS
Heater
VLS = Vapor/Liquid
Separator
the number of lots processed. A third
opportunity is looking at the efficiency
of any vapor/liquid de-entrainment de-
vices. Investigate the equipments ap-
plicability for current process condi-
tions. In other words, Do we have the
most efficient mist eliminator pad, and
is there a product that will provide us
with more efficient de-entrainment?
If there is an external vapor/liquid
separation system (VLS), does its size
or configuration help to eliminate
product losses in the vapor stream?
Depending upon vapor velocities re-
quired by the system, a substantial loss
of product could take place during this
step product certainly worth recov-
ering. For example, could a cyclonic feed injection be
used rather than feeding straight into the vessel? Or,
could the vapor be forced to change directions in the ves-
sel and flow up an internal chimney? Be careful when
analyzing these systems, particularly with vacuum evap-
oration, because modifying the configuration of the VLS,
or otherwise attempting to increase de-entrainment effi-
ciencies may mean increased pressure drop and subse-
quent issues with system performance.
Temperature-sensitivity and other
temperature issues
When the product is a solute, one needs to know the
yield/product losses due to the heat-treatment of temper-
ature-sensitive materials. Even if the system temperature
is not deleterious to the product, ensure that local hot
spots in the base heater are not degrading some material.
One way to resolve this is to ask: Can we run the pro-
cess at a lower temperature (which usually means run-
ning at lower pressure), such that we can keep the prod-
uct cooler? Again, this may extend the cycle time, but if
yield improvements are large enough to counteract those
losses, this could be an elegantly simple change.
If the process is currently set up as atmospheric evap-
oration, the obvious change would be to modify the pro-
cess train such that it can become a vacuum operation.
The first and hopefully most obvious issue here is to en-
sure that all equipment in the evaporator train is rated for
vacuum service. If not, this option may require a sub-
stantial capital investment and other means of achieving
desired capacity may need to be investigated. However,
if the process is already configured for vacuum evapora-
tion, it can simply be run at lower pressures, thus allow-
ing the system to operate at lower temperatures, keeping
the product cooler.
Take into consideration that running at lower pressure
may mean a decrease in vapor density and, thus, an in-
crease in vapor loading to the condenser to achieve the
same cycle time. Ensure that the condenser and utility
streams are capable of handling such an increase.
Consider using a tempered loop
Another option that provides benefits both in tempera-
ture control and heat-transfer efficiency is to install what
we term a tempered loop on the liquid-service side of the
heat exchanger (Figure 2). In this configuration, a pump
recirculates the bulk of the heat-transfer fluid through the
heat exchanger at an increased rate, with a small bleed-in
of cold or hot utilities to achieve accurate temperature
control. The increased mass of recirculating fluid buffers
the temperature, improving temperature control, which,
in turn, permits running a little closer to any limiting
temperature values (examples might be the freeze point
of the condensate mixture or degradation of a heat-sensi-
tive material due to a minor control upset on the base-
heater service fluid). The increased flowrate also results
in higher fluid velocities and a higher corresponding
Reynolds number, which positively affect the fouling re-
sistance, as well as the overall heat-transfer coefficients
and, thus, the heat exchanger efficiency.
However, with the tempered loop, as with all changes,
there are checks that need to be made to ensure that the
system works properly. Be careful that the heat exchang-
er is sized to handle increased flowrates, velocities, pres-
sures and pressure drops. It can be problematic, and
maybe dangerous, that after changing to a tempered
loop, the heat exchangers pressure-relief setting and sys-
tem pressure are too close, causing the system to relieve
pressure with any pressure spike. Check your heat-trans-
fer calculations to ensure that the tradeoffs that occur
among the decrease in the temperature driving force in
the heat exchanger, decrease in service temperature, and
increase in mass flow through the heat exchanger, pro-
vide the desired heat duties.
Accurate temperature control is an area to look at
early on in evaluating capacity increases or when trou-
bleshooting temperature problems (such as freezing con-
Reactions and Separations
50 www.cepmagazine.org February 2002 CEP
Cold Utility Return
Hot Utility Return
Hot Utility In
Cold Utility In
To Process
Recirculation
Pump
Control
Valve
Heat Exchanger
(Base Heater
or Condenser)
From Process
I Figure 2. Schematic for a tempered-loop utility design.
densate or heat treatment in a heater) in heat-transfer
systems. For a relatively small investment, the reward
can be large in terms of condenser freeze-protection, ad-
ditional heat duties and overheat protection needed for
temperature-sensitive materials.
Reducing cycle time
Now, discussion will focus on the area where many
chemical engineers might rapidly begin their search for
additional capacity. A desire for bigger, faster or better
equipment seems to be a universal trend. Armed with
basic knowledge of how much is needed to improve
cycle time and the basic mass and energy balances, one
can begin a system-by-system check of the evaporator
train looking for bottlenecks to remove.
From a very simplistic viewpoint, the problem of ad-
ditional capacity can be boiled down to: We need to run
faster; therefore, we need to put more energy into the
system to make the concentration occur faster. Although
this is a simple thought, it has ramifications that need to
be assessed. Completing or updating mass and energy
balances is the first step in determining what can be done
to achieve this simple fix. From the energy balance, de-
termine whether or not the utility systems have the ca-
pacities to deliver the new heat duties required. The ener-
gy balance coupled with the heat-exchanger (base heater
and condenser) design-parameters will tell if there is ad-
ditional capacity in the exchangers, not only to transfer
required heat to the material, but also to remove that heat
from the system. From the mass balance, simple simula-
tions and detailed calculations, determine the flowrates
and velocities of various vapor and liquid streams. This
will help to determine if the pumps, VLSs, decanting
vessels, nozzles, piping, mist eliminators, etc., are ade-
quately sized to meet additional requirements associated
with higher heat duties. And, for vacuum evaporation,
sensitivity analyses on the vacuum system will tell what
pressure would help to optimize heat, temperature and
flow requirements.
For example, increasing the pressure (and tempera-
ture) of an evaporator substantially reduces the vapor
volumetric flowrates and, thus, the velocities of the
vapor streams. This unloads a potential hydraulic bottle-
neck of the process equipment, allowing use of current
equipment over new units. However, this could introduce
other bottlenecks, such as increased velocities of liquid
streams. Here is why increasing the temperature/pressure
in the evaporator will require an increase in the liquid
flow through the heater: As pot-content temperature in-
creases, temperature driving force will be suppressed,
and flowrates through base heater will need to increase
to achieve the same heat transfer.
The increased liquid velocities may necessitate in-
creasing the size of the liquid nozzles to avoid tube chan-
neling, which is poor liquid distribution through base
heater tubes due to increased liquid velocities. Tube
channeling leads to loss of heat-transfer efficiency and
perhaps unintended heat treatment of the temperature-
sensitive product.
If the desired rate cannot be achieved with capital im-
provements or any combination of the previously men-
tioned improvement ideas, then consider adding an entire
unit in parallel to the existing one. In many cases, this
may be preferable to making extensive modifications to
existing units. This is particularly true where space is not
limited, or where the existing unit has already been opti-
mized to run as efficiently as possible.
Simple improvements
When the primary use of evaporation is to concentrate
a solvent(s) in a liquid feed of mixed solvents, either
continuously or semi-continuously, simple options to
consider for capacity improvements may be different
than for evaporating solvent away from a solute or slurry.
As previously stated, process improvements for both
types of evaporations are highly system-dependent, but
the general nature of the types of improvements and or-
ganized approach we are suggesting can be illustrated by
the following simple examples.
Optimal feed placement
This example is almost trivial in nature, yet we have
seen this exact configuration duplicated several times in
industry. Often, a single-phase evaporator is configured
for the feed to mix directly with the solution in the unit,
which is near its boiling point. If the evaporator has an
external heat source (either forced or natural convection),
this arrangement will allow a portion of the feed in the
well-mixed evaporator to discharge with the underflow,
having achieved no distillation whatsoever, thus resulting
in some efficiency loss. The most appropriate position to
add the feed would be directly upstream of the evapora-
tor heater, after the bottoms product split.
Think outside of the box
Here is a complex example that demonstrates outside-
CEP February 2002 www.cepmagazine.org 51
The energy balance coupled with heat-exchanger design parameters
will tell if there is additional capacity in the exchangers to transfer
required heat and remove it from the system, as well.
of-the-box thinking. Admittedly, such a change is highly
processspecific, would require much research, and in a
regulated industry such as pharmaceuticals, could only
be considered during process development.
Imagine that the process is to concentrate a low-boil-
ing Solvent A from a higher-boiling Solvent B in a ho-
mogeneous liquid feed, but no azeotropes exist between
A and B. Some inefficiencies are necessarily accepted in
the single-stage process as low-yield/high-purity or vice
versa, even if several evaporators are used in series. (It
may even be an impossible separation if there is a dis-
solved solute from which the higher-boiling solvent must
be removed.)
However, if a third, (process compatible) solvent,
Solvent C, with special non-ideal characteristics, could
be introduced to the system, it could allow a reduction
in separation inefficiencies. For instance, if highest boil-
ing Solvent C forms a low-boiling heterogeneous
azeotrope with Solvent B, then one could add Solvent C
to the mixture, and boil away the B-C azeotrope (which
could be cooled and decanted, if desired). In the next
step, Solvent A would be evaporated away from Solvent
C, likely leaving Products A and/or B much purer than
in the original design.
Refluxing condensate
Another outside-of-the-box idea to increase efficiency
for semi-continuous solvent processing is to assess
whether it would be beneficial to install a small packed
column on the vapor outlet of the evaporator tank with a
portion of condensate refluxing back to the packed sec-
tion. The considerations are many (cost to purchase and
install column/internals, rating of, and possible addition
to heating and cooling capabilities, increased pressure-
drop/temperature considerations for the step, and so on)
but additional efficiency and throughput may justify
such an investment.
Using spare equipment
If the continuous evaporator already has an online
spare (as is sometimes so in fouling or other high-main-
tenance service), consider configuring the evaporators in
series to add an additional stage to the process. The in-
creased capacity (from increased efficiency) might more
than make up for additional downtime to clean and main-
tain the system. An alternative way to use the spare
equipment is to consider running the evaporators in par-
allel, again trading roughly doubled capacity for in-
creased downtime to clean or maintain equipment.
Conclusion
In summary, when looking for capacity improvement
opportunities for a single-stage evaporator, first thor-
oughly understand the design and operating conditions of
the system. A detailed understanding will lead to the
most effective improvement opportunities, such as an im-
proved process/product (e.g., higher yield), greater ser-
vice efficiencies (e.g., by installing tempered loops), or
changes in core equipment design and ratings. Numerous
angles exist to investigate when to look for capacity im-
provements.
One final thought: capacity improvements must not be
made in a vacuum. If the process is fed by, or feeds an-
other process, consider the impact of changes on other
systems. Often, this impact is not trivial. Additionally,
for those improvement ideas presented here that are not
directly applicable to your system, we hope you can
learn from our approach of assessing the system and at-
tacking various areas of improvement. Many of the pro-
posals outlined in this article can provide easily integrat-
ed solutions, and always look for the quickest, easiest,
high-impact solutions first. However, potential tradeoffs
are associated with each, and be prepared to analyze
them along with achievable benefits to make the appro-
priate recommendations.
CEP
Reactions and Separations
52 www.cepmagazine.org February 2002 CEP
ERNEST A. PERKINS is a senior process engineer supporting Biosynthetic
Human Insulin Production at Eli Lilly and Co. (Lilly Corporate Center,
Indianapolis, IN 46285; Phone: (317) 433-3639; Fax: (317) 277-0897;
E-mail: perkins_e_a@lilly.com). His main focus is on improvement efforts in
the human insulin manufacturing processes. He has spent the bulk of his
career with Lilly in various process engineering roles supporting both
direct-manufacturing operational areas, as well as related support areas. A
registered P.E. in Indiana, Perkins received his BS in chemical engineering
from the Univ. of Nevada-Reno, and is a member of AIChE.
RYAN C. SCHAD is the Process Engineering Dept. head for Biosynthetic Human
Insulin Production at Eli Lilly and Co. (Phone: (317) 433-5519; Fax: (317)
277-0897; E-mail: rcschad@lilly.com). His group of process engineers,
partnered with manufacturing and other technical service groups, supports
and improves the insulin-production unit operations. Previously, Schad was
a senior process engineer supporting new and existing bulk-
pharmaceutical processes. He also has prior experience at Eastman
Chemical Co. in both development and process design engineering. A
registered P.E. in Indiana, he received his BS in chemical engineering from
Purdue Univ.
Literature Cited
1. Perry, R. H., et al. (eds.), Perrys Chemical Engineers Handbook,
Sixth Edition, McGraw-Hill, New York, Sec. 11, Heat Transfer
Equipment, p. 11-31 (1984).
2. Walas, S. M., Chemical Process Equipment Selection and Design,
Butterworth-Heinemann, Boston, Sec 8.10, pp. 208211 (1990).
Acknowledgments
The authors would like to recognize the contributions of Scott
Kuester, David Dzirbik, Rick Dargatz, Linda Stockton (all with Eli
Lilly), and John Calvert (consultant) for their talents in analyzing our
evaporation systems and developing some of the recommendations
included here.