D I S T I L L AT I O N R E VA M P S

Optimize Distillation
System Revamps

istillation remains the predom- potential improvements including:

Revamping can
improve most
D inant separation technique in
the chemical process industries
(CPI), accounting for more
than 90% of product recovery and purifi-
cation applications. Its use spans the en-
• eliminating operational bottlenecks
and increasing capacity;
• implementing a new process or
product within existing equipment;
• enhancing product purity, thereby
existing columns tire CPI, from massive continuous chemi- creating possible new markets for an ex-
cal and petroleum complexes to small isting product;
and, indeed, batch facilities manufacturing specialty • boosting product or raw-material
chemicals such as materials additives, recovery;
provides one of the pigments, paints, inks, pharmaceuticals, • purifying raw materials;
flavors, and fragrances. With more than • reducing waste-disposal quantities;
most economically 40,000 distillation columns in operation and
in the U.S., the capital investment in- • removing and capturing materials
attractive opportu- volved exceeds $8 billion (1). from water and air waste streams.
Though revamping of distillation sys- Even though these factors make re-
nities available in tems is not a new concept, it is assuming vamping a worthwhile endeavor, the dis-
greater importance today. Many compa- tillation process sometimes is not consid-
process engineering nies now are trying to maximize their re- ered a part of the primary production line
today. Use this turn from existing sites, rather than in- but instead a low-priority support opera-
vesting in new grassroots facilities. Plus, tion. Consequently, too often, it does not
proven strategy the opportunities for column revamping
abound: An increasing number of distil-
receive the emphasis and attention it
deserves.
to find the lation systems are required to process
variable-feed-composition streams and
Distillation for recovery of solvent or
unreacted raw materials also typically is
most-cost-effective to meet more-stringent product and considered a lesser operation than prod-
byproduct specifications. Many batch uct recovery. For such “secondary” oper-
option. systems are operated in campaigns, ations and within smaller facilities, finan-
which may make additional demands as cial constraints can be particularly sensi-
the feed components and composition tive, especially if it is assumed (mistaken-
John A. Williams,
are perpetually changing. Improving the ly) that revamping the distillation column
Environmental & Production
performance of such processes promises will be prohibitively expensive.
Solutions, LLC
a high economic return. In fact, for most
distillation systems currently in opera- Consider a real revamp
tion, a revamp may provide significant Many companies don’t actually assess
improvements in the competitive posi- the revamping of an existing unit — not
tion of the process. realizing that a high economic return usu-
Revamping opportunities are present ally is easily achievable with a well de-
in most existing distillation systems, with signed and executed revamp. Instead, the

CHEMICAL ENGINEERING PROGRESS • MARCH 1998 ©Copyright 1998 American Institute of Chemical Engineers. All rights reserved. Copying and downloading permitted with restrictions.
D I S T I L L AT I O N R E VA M P S

traditional “revamping” approach 4. How to analyze the economic identify whether existing equip-
often taken is to design and build a impact; ment, instrumentation, and controls
new column, rather than to work In addition, we will provide case actually may have the potential to
within the confines of the existing histories of distillation system re- achieve the necessary results with
unit. This may involve lower risk, but vamps to illustrate the value of the only minimal modifications. All
it almost always is more costly in approach. process and instrumentation dia-
terms of capital investment (including In short, this article will provide grams (P&IDs) and controls should
for equipment that a well-designed an overview of all the factors that be personally field-verified. In
revamp may obviate) and lost pro- must be considered when evaluating short, field assessment is not only
duction due to downtime. a possible distillation-system revamp. an excellent method for understand-
The reasons why improvement of Though the recommended approach ing current operations and problems,
existing equipment doesn’t get the em- involves more upfront effort by the but also is a cost-control measure
phasis it deserves are many and varied production engineer, it will identify that may save a company from pur-
— but they generally boil down to a the most economical way to achieve suing unnecessary expenditures.
lack of solid understanding of what operational objectives. Visual inspection — If the time
can be accomplished and a lack of re- frame of the project allows, visually
alistic analysis of capital requirements. HOW TO ACHIEVE inspect the column internals by ob-
Yet, to reiterate, revamping usually is A SUCCESSFUL REVAMP serving the operation through the ac-
the most cost-effective solution. One of the main issues involved in cessways or handholes. Look for in-
Revamps afford the opportunity to revamping a distillation system is de- ternals that may have been displaced
take advantage of the significant termining what must be done to effect or those that have become mis-
progress recently made in distillation an economic gain for the plant. We’ll aligned over time. Also, check for
systems. Such developments include outline several steps that can serve as plugging within the column, as well
the commercialization of higher-effi- a guide. as deformation or any signs of exces-
ciency trays and packings that sive wear of packing material or dis-
promise high economic returns. Define system objectives tributors. Surfaces that have become
Today’s high-performance mass- The first step is to define the de- fouled or show stress cracking or dis-
transfer internals offer dramatically sired objectives of a revamp. Infor- coloration may indicate such prob-
reduced column pressure drops and mation must be gathered relating to lems as poor wetting, pressure surges
increased turndown ratios — en- the processing requirements, includ- during operation, or excessive flash-
abling operation over a wider range ing determining the full range of po- ing near the reboiler discharge. Addi-
of high and low liquid-flow loadings tential feedstock compositions and tionally, if column performance has
— than was previously possible. stream conditions. It also is helpful to declined over time and signs of mate-
The purpose of this article is to note how many product lines are rials corrosion are apparent, consult a
show production and process engi- campaigned upstream of the distilla- metallurgist. A competent metallur-
neers how to determine, given their tion system. The desired minimum gist can assess the impacts of the cur-
particular objectives, whether or not and maximum processing capacity rent corrosion and specify either op-
revamping is a viable option. It intro- also must be defined, as well as the erational conditions less corrosive to
duces an approach that can be applied product composition wanted (both the the existing materials or materials
regardless of scale of operation or minimum acceptable and “ideal”). It that offer a higher degree of corro-
type of product. We will not get into also may be necessary to specify sion resistance.
specific design practices, which can other product attributes such as color Radioactive tools — Three estab-
be found in several excellent theoreti- and clarity. A report of the product lished column on-line diagnostic
cal and practical texts such as Refs. specifications and distillation system tools involving the use of radioiso-
2–8. Instead, we will outline the requirements should be confirmed topes — grid scanning, radioactive
following: with the organization’s Marketing tracing, and computer-assisted to-
1. How to achieve a successful Product Manager and the Production mography (CAT scans) — can be
revamp; Manager, respectively. useful in assessing the hydrodynam-
2. How to factor in environmental ics of the column under existing oper-
issues; Evaluate existing operations ational conditions. The internals defi-
3. How to develop the right strate- The next step is to assess how the ciencies identified then can be ad-
gy — including assessing the desired existing distillation system works. dressed in the revamping design.
operating conditions, finalizing de- On-site observations are crucial to Grid scanning basically is a mea-
sign parameters, and selecting the the understanding of the current sys- surement of the column cross-sec-
proper equipment; and tem’s operation — they often can tional density profile via a series of

CHEMICAL ENGINEERING PROGRESS • MARCH 1998

systematic gamma scans taken files and their stability to determine not steady state, how does it change
through the column vessel. The tech- if there are any abnormalities in the and how smoothly does that happen?
nique exhibits limitations on pressure drop that would indicate Throughout your observations, ad-
columns diameters less than 18 in. or column leaks, steam losses, or feed dress the possibility of the current
more than 30 ft, and on very dense surges. Is the system constrained by hardware accomplishing the desired
systems. Grid scanning can be effec- the supply rates or condition of the objectives, either by using a different
tive for column integrity checks and utilities? Does a batch system operating algorithm (controls), by
the identification of column maldis- plateau or get stuck at some point? correcting an existing malfunction
tributions, flooding, foaming, and Check also for any thermodynamic within the system through modified
entrainment. or kinetic effects, such as the onset instrumentation, or by modifying or
Radioactive tracing introduces a of a reaction, or a phase change that replacing an equipment component.
traceable material into the process may cause the conversion of materi- Controls and ancillary equipment re-
and tracks its passage within the sys- al into waste. vamps/changes often present them-
tem with detectors. Commonly used Interview the operators to deter- selves and enable the company to
radioisotopes are bromine 82 and io- mine other critical information. Ask avoid expensive revamping designs.
dine 131 for organic and aqueous sys- them how often the unit must be For instance, it may be beneficial
tems, respectively. Tracing can be ef- shut down, and whether this is due to modify the control algorithm to
fective for flow-related problems to a lack of distillation feed or a increase the liquid or vapor rates by
such as holdup, mixing, and leakage. product changeover. Does there more aggressive condensation and
CAT scans develop detailed cross- seem to be a lack of operating staff? boilup rates, and to incorporate alter-
sectional density profiles via several Do distractions by other plant activ- native reboiler or reflux ratios. Po-
angular measurements at fixed eleva- ities interrupt the distillation system tential changes to noncontinuous op-
tions. CAT scans are more detailed operation? Do the operators notice erations include adding an interme-
and costly than grid scans and, there- problems with fouling or plugging diate hold temperature above the
fore, often are used as a detailed com- of any equipment or lines in this current procedure to reduce long
plement to a grid scan in identifying area of the plant? If so, how do they heatup or cooldown times, and using
specific patterns of maldistribution. remedy them? multiple receivers or quick pumpout
Bowman provides a comparison You also will need to determine procedures.
of radioisotope techniques and their actual startup and shutdown proce- Objectives often can be achieved
use for maintenance, troubleshooting, dures for the unit. These may identify through upgrading of control ele-
and optimization (9,10). limitations of the system and addi- ments — such as putting a manually-
Historical performance — Com- tional sources of waste generation. operated, or inadequately controlled,
pare the current system performance Note any unusual events in the distil- feed valve under continuous feedback
with data generated at the time of in- lation system’s history and what may and cascaded control. Instrumentation
stallation and startup. Can the exist- have caused them. Ask the operators upgrades include the installation of
ing column operate at the same pres- to detail when the product streams are an on-line sampler that quickly iden-
sure profile, or are there obvious indi- off-specification and when the system tifies targeted stream compositions
cations of changes to the column in- is performing at its best. They may and deviations from them. Equipment
ternals such as corrosion, misalign- have information that is key to deter- may be improved, for example, by al-
ment, or blockages? Note any mining the conditions that lead to col- tering the system pressure, supplying
changes and what caused them. umn instability. the existing reboiler with a higher-
To evaluate current column per- What is the current instrumenta- temperature utility source and the ex-
formance, you will need to review tion, and how closely do the system isting condenser with a lower-temper-
the operations log and any archived parameters follow the control system? ature coolant, or increasing heat-ex-
charts and data sheets. Look at the In your inspection of the existing in- change surface areas by the addition
maintenance records of the column strumentation and controls, determine of in-parallel or in-series heat ex-
and ancillary equipment. Verify the if any of the instruments need recali- changers, depending upon desired
mass balance, including the feed, bration. It is not uncommon for distil- flow rates, temperature profiles, and
distillate, and bottoms rates and lation systems to perform poorly due available utilities.
compositions, and reflux ratio, as to faulty thermocouples or dry ther- A hypothesis-based problem-solv-
well as the energy balance, including mowells. Also, find out how much of ing approach incorporating process
the condenser and reboiler condi- the operation is truly automatic vs. simulation and field data is most ef-
tions and utility usages. Is there con- manual, and how often the operators fective for accomplishing the re-
sistency with the mass balance? Ex- must interrupt the control scheme to vamping objectives with minimal
amine the column temperature pro- use manual settings. If the system is capital expenditures.

MARCH 1998 • CHEMICAL ENGINEERING PROGRESS

D I S T I L L AT I O N R E VA M P S

Use computer simulations developed, empiricism will continue The two predominant process-
— wisely to predominate in the calculation or stream materials that cause the most
Computer simulators are readily assignment of stage efficiencies. Once environmental concern are: (1) “still
available and are computationally ac- an internals type is selected, you are bottoms,” which often consist of
curate — making it easy to quickly well advised to work closely with the tarry residues that frequently con-
simulate the full range of potential internals vendor to determine the tain a multitude of molecular
operating conditions. The majority of achievable stage efficiencies for a species and exhibit high viscosity at
simulators employ an equilibrium- given design. In practice, stage effi- ambient temperatures; and (2) high-
stage approach, based on vapor/liquid ciencies frequently are assigned based vapor-pressure materials (material
equilibrium (VLE) data, and model on the operation of similar systems of losses), which may slip through
steady-state operations. Batch and components and internals. condensers into vacuum systems or
dynamic simulators also are avail- Whatever methods of modeling are become fugitive emissions through
able. Process simulation packages are used, perform simple checks on the leaks in flanges and other equipment
offered by, among others, Aspen, simulation output to see if the simula- connections.
Chemstations, Hyprotech, and Simu- tion reflects real-world operation:
lation Sciences. • Assess the simulator results (out- Reduce the amount
The key to an accurate simulation, put) against those obtained from a of still bottoms
especially with respect to the number McCabe-Theile diagram. Still-bottoms or tarry-material
of equilibrium stages, is accurate VLE • Compare the output against data formation frequently is caused by
data. Most commercially available from the original startup and the cur- byproduct formation in the reactor
simulators come with libraries of VLE rent operation. and, if conditions permit, in the still.
data. Look also for in-house VLE data More details on how to make sure Distillation systems used to process
that may have been generated with pre- that you have a realistic and reliable effluents from more than one pro-
vious distillation designs for the com- simulation are given by Kister (18). duction line often are particularly
ponents within the system. Literature Using the process simulator, you susceptible to tar-forming reactions.
sources for VLE data include AIChE’s should do a methodical sensitivity An additional problem with still bot-
Design Institute for Physical Property study covering the full range of feed toms involves disposal. The pres-
Data (11), DECHEMA’s Chemistry and operating conditions and product ence of such high-molecular-weight
Data Series: Vapor-Liquid Equilibrium specifications. This allows you: (1) to products in the waste often results in
Collection (12), and publications by determine what is achievable in the additional waste, as processors try to
Hala and coworkers (13,14). VLE data existing equipment, and how the con- manage their flow by: (1) controlling
also can be measured for the compo- trols and the control algorithms may the discharge composition to include
nents under investigation and obtained need to be modified to achieve the lighter components, such as process
from contract research laboratories for target conditions; and (2) to begin to solvent; or (2) keeping the flow high
a fee. As a last resort, if actual VLE determine what a revamped system or the outlet orifice larger than nec-
data are not available and measure- would be capable of achieving. essary to avoid any chance of plug-
ment is impractical, a predictive model ging. Losses also occur when opera-
such as the UNIFAC group contribu- HOW TO ASSESS tors handle the high-viscosity mate-
tion method and its extensions (Sher- ENVIRONMENTAL ISSUES rial by diluting it with valuable sol-
wood and coworkers (15)) can be used, Process wastes and emissions can vents or raw materials.
but only with extreme caution. Carlson have a major economic impact on For distillation yield maximization
(16) provides a decision-based ap- distillation systems. Therefore, any and waste minimization, it is neces-
proach for evaluating physical-proper- revamping strategy needs to assess sary to obtain as much knowledge as
ty parameters for successful process environmental gains and losses. First, possible about any potential (ongo-
simulations. identify what is causing the solid or ing) chemistry occurring in the still or
Despite the precision of simulators liquid waste components in the cur- upstream that leads to tarry materials
in calculating the number of equilibri- rent system. Determine if there are air and their composition in the distilla-
um stages, translating theoretical to or water emissions from the system, tion feed. Because there may be no
real stages remains an inexact predic- and whether they are fugitive or con- documented research or history of the
tive art based on empirical correlations tained within the process streams. still’s chemistry, the only alternative
such as the Murphree tray efficiency Also, ascertain where the emissions may be to pinpoint as closely as pos-
(17). Further, each internals type, size, are escaping — that is, into the vacu- sible the chemistry of the tar forma-
and configuration exhibits different um system, the cooling water tion and its location. Pay particular
hydrodynamics, and, until detailed un- streams, through the piping flanges, attention to additional chemistry that
derstanding of the hydrodynamics is or somewhere else. may be occurring in multicomponent

CHEMICAL ENGINEERING PROGRESS • MARCH 1998

mixtures. If your expertise in chem- retrofit of the column internals. purging a lower quantity of waste.
istry isn’t up to the task, consult a Check to see if inadequate instru- This frequently is achievable and ef-
competent chemist. Once you’ve de- mentation and process control could fective in batch and semicontinuous
termined the cause of tar formation, be causing the tar formation. distillations.
methods for avoiding it can be devel- 3. Can recycling a stream from the 8. Startup and shutdown opera-
oped. Here are several options for re- distillation system to the upstream tions also must be assessed for waste
ducing tar formation, ranging from process cut tar formation? This also generation, as practices may involve
economical to costly: may offer the benefit of returning un- purging of the still contents, resulting
1. If tar forms because of compo- converted raw materials or perhaps in additional waste.
nents that originate upstream, look at providing a solvent source.
the upstream process to determine 4. Can the distillation system pro- Run laboratory tests
how it can be changed. Address what duce other, marketable cuts that can The next step is to perform a labo-
is causing byproduct formation reduce still bottoms? For example, ratory distillation, preferably in a
(yield losses) in the reactor, and de- adipic, glutaric and succinic acids glass system to allow visual observa-
termine if higher-purity raw materi- from nylon-intermediate-manufactur- tions. Though this step is an uncom-
als can minimize or even eliminate ing stills and crystallizers are sold as mon one, it can provide valuable in-
it. Can the process be operated at an additive in flue-gas scrubbers. sights on the system at hand, helping
different temperature or pressure 5. After achieving possible source the engineer to understand the chem-
conditions to avoid byproducts? If reductions, you must reclaim or dis- istry that is occurring and to identify
so, can this be accomplished with pose of the remaining tar stream. phenomena and their possible causes.
minor equipment modifications? Reclamation typically involves rela- By performing the distillation process
Can the optimum residence time be tively expensive unit operations such under a similar temperature and pres-
controlled more tightly? Can the sol- as extraction or high-vacuum wiped- sure to plant conditions, it is possible
vent system be changed? If the pro- film evaporators and, so, often is to:
cess is operating away from its opti- cost prohibitive. Disposal options in- • observe any foaming effects;
mal conditions, is this due to inade- clude off-site incineration and dis- • create conditions that might lead
quate instrumentation and process posal in landfills — which are both to plugging by solids or fouling by
control? Do detrimental nonunifor- costly and politically incorrect. Be- tars;
mities, such as temperature or con- sides the expenses already incurred • detect sublimation of unknown
centration gradients in the reactor in raw-material procurement and up- components;
due to heat-transfer mechanisms or stream processing, landfilling or in- • spot a color change indicating
mixing, respectively, exist? cineration runs from $0.15–1.50/lb that reactions are occurring;
2. If the problem is occurring of waste. And, the approval and per- • notice a change in viscosity;
within the distillation system, deter- mitting processes and the effort as- • verify or discount any assumed
mine what is causing it. Can operat- sociated with the paperwork impose chemistry (presuming samples can be
ing at different pressure or tempera- additional costs. taken); and
ture conditions help avoid tar forma- 6. A more economic disposal op- • characterize product streams, to
tion or concentration? Lowering the tion is to cofire tar in an existing boil- confirm stream composition, espe-
pressure may improve distillation er. This, however, may also mean cially impurities and byproducts.
recovery or reduce equipment-in- consuming lighter components such
duced pressure drops such as vapor as process solvents to maintain the HOW TO DEVELOP
line restrictions. If the heat-transfer flowability of the tar. It also mandates THE RIGHT STRATEGY
mechanisms are prompting thermal implementing a reliable firing config- Armed with data from the previ-
degradation or undesirable reac- uration that won’t plug, and ensuring ous steps, you now can develop the
tions, the reboiler can be re- acceptance of the system by the boil- distillation-system-operation strate-
designed, or different heat-transfer er operators. Last but not least, in gy that will create favorable condi-
media can be utilized. If heat losses most states, cofiring requires revi- tions for yield maximization, oper-
on certain surfaces are causing un- sions to the facility’s Clean Air Act ability, and waste minimization re-
desirable effects, the insulation can Title V operating permit, which, de- quirements. To do so, the following
be improved. Evaluate whether pending upon the state’s regulations, operational parameters must be
these solutions could be accom- may take more than a year. specified: product stream composi-
plished with minor equipment modi- 7. An operational technique for tion, operability, onstream time, av-
fications, such as more-effective waste minimization with tars is to erage column residence time, col-
condensers, improved heating or concentrate the tars, removing valu- umn holdup, and startup and shut-
temperature control of the feed, or a able components and, thereby, down procedures.

MARCH 1998 • CHEMICAL ENGINEERING PROGRESS

D I S T I L L AT I O N R E VA M P S

Conduct field trials mass balance calculations and com- There are, as we’ll discuss, some
At this point, your knowledge putational modeling, and provide an general differences in performance be-
level and revamping strategy should assessment of the actual number of tween trays and packings, and these
be at least 90% complete. Running separation stages — that is, the stage can serve as a guide for preliminary
tests now with the existing equipment efficiency. selection. The final comparison, how-
should verify the strategy, while pro- The goal, throughout the field trial, ever, should be between optimum
viding the final assessment of the ex- is to clarify and confirm the three trayed-column and packed-column de-
isting equipment under the proposed fundamental questions for the column signs. The optimal tray design is one
conditions. Prior to the field trial, fin- revamp, specifically: that balances bubble and downcomer
ish any remaining mass- and heat bal- 1. What are the required hydrody- areas so that neither becomes a capaci-
ances and system productivity-rate namics to achieve efficient phase ty pinch. Such a design then will max-
calculations. Throughout the field contact? imize the fractionation efficiency and
trial, the data logging should include 2. What are the number of stages column capacity by specification of
a continuous assessment of how close necessary for the separation, based on weir height and geometry, downcomer
the system is running to the target the equilibrium thermodynamics of clearance, and the fractional hole area.
conditions; this is critical for deter- this distillation system? Similarly, an optimal packed-column
mining what modifications are re- 3. What precautions, such as the design is one that properly incorpo-
quired to achieve desired operation. avoidance of plugging, fouling, or the rates liquid and vapor distributors,
Hanson and coworkers provide a like, are needed for system reliability? packing type and size, and supports to
summary of preparation procedures At the conclusion of the field trial, avoid or minimize adverse liquid and
prior to a distillation test run (19). the revamping strategy should be vapor maldistribution.
The field trial should strive to sim- nearing completion. You should have
ulate the full range and combinations determined the operational mode and Choose the right internal
of parameters including feed, liquid, sequence, as well as conditions con- The goal in selecting internals is to
vapor, boilup and reflux rates; tem- ducive for acceptable hydrodynamics, come up with a configuration that
perature and pressure profiles; and startup and shutdown procedures, and maintains effective vapor/liquid con-
the startup and shutdown procedures. the instrumentation and the process tact over the desired operating condi-
If the revamping strategy involves a control algorithm. tions, while minimizing pressure
change of operational mode — for in- With this critical information, you drop, liquid entrainment, weeping,
stance, from batch to semicontinuous now can turn to selection of the spe- corrosion, and fouling or plugging. At
operation — the trials may require cific internals. this point, it should be clear that col-
extensive manual control to achieve umn capacity is largely determined
the operational sequence. Limitations Start with by column diameter, specifically its
of the system should be identified and the existing internals ability to handle the desired liquid
explicitly assessed. Retrofitting better internals into an and vapor flow rates without inducing
The hydrodynamics, both liquid existing column can readily provide adverse flooding. Groups, including
and vapor, of column internals should increases in capacity and fractiona- Fractionation Research, Inc. (Stillwa-
be evaluated at the projected typical, tion capability. Such a revamp isn’t ter, OK), and the Separations Re-
minimum, and maximum flow rates, always needed, however. At times, search Program at the University of
and at the minimum and maximum performance of existing internals can Texas at Austin, have performed fun-
achievable reflux rates. This requires be improved significantly by under- damental research on system parame-
that close attention is maintained to all standing their inherent limitations and ters that affect internals selection.
system indicators such as temperature modifying the operation to overcome In general, most columns less than
and pressure profiles, flows, and re- these limitations. 36 in. dia. tend to favor packing, ei-
boiler and condenser operation. Signs No one internals type, be it trays, ther structured or random. Beyond the
of liquid entrainment (jet flooding), structured packing, or random pack- general 36-in.-dia. division, the di-
liquid flooding, and liquid or vapor ing, is superior to the others in all mensionless flow parameter, FP, can
maldistribution — and corresponding applications; indeed, all can be aid in selecting column internals type.
losses in the separating efficiency — made to fractionate the same chemi- The flow parameter is the ratio of the
should be monitored constantly. cal systems. Therefore, it behooves square roots of the kinetic energy of
As the distillation progresses, get a the revamping engineer to under- the liquid to the kinetic energy of the
compositional analysis of the feed, stand what the existing internals vapor — that is, in mass units:
bottoms, overheads, and, if available, configuration can and can’t accom- FP = (L/V)(ρV/ρL)1 (1)
intermediate stage(s) within the col- plish before opting to retrofit a new For optimized, modern 24-in.-spaced
umn. This analysis will refine the set of internals. trays, 2–21-in.-nominal-dia. packing,

CHEMICAL ENGINEERING PROGRESS • MARCH 1998

and 67-ft2/ft3 structured packing, ca- ties and efficiencies. When an exist-
pacities and transfer efficiencies were ing column diameter is sufficient for
evaluated. At a FP between 0.02 and the desired capacities but the trays
0.1, the structured packing exhibited are outdated, revamping via a
approximately 50% higher efficiency; straightforward tray replacement, op-
as the FP rises above 0.1, however, timized at the current vapor and liq-
the efficiency advantage of structured uid loadings, often is attractive. Ven-
packing rapidly declines with increas- dors offering high performance trays
ing FP. For details, see Ref. 20. In include Koch Engineering (which re-
general, at a lower FP, for instance, cently bought Glitsch), Norton, and
less than 0.1, packing usually is the Nutter Engineering/UOP. Examples ■ Figure 1. CoFlo high-performance
first choice for evaluation, while at of high-performance trays are shown tray. (Courtesy of Jaeger Products, Inc.)
higher FP, say, 0.2–0.3 and greater, in Figures 1–3.
trays generally are favored; between
0.1 and 0.2, there is no clear initial Random and structured
choice between trays and packing. packing
While a parameter like FP can In columns where packing is an
help guide you to an initial choice, option, the installation of higher effi-
the subsequent internals design needs ciency or higher loading packing
to be fully evaluated based on com- often realizes significant increases in
plete system information. If a signifi- fractionation ability and capacity, re-
cant concern exists, then assess an- spectively. Properly applied random
other option. and structured packing operate with
considerably lower pressure drop ■ Figure 2. Bi-FRAC high-performance
Distillation trays (one-third to one-fifth less per theo- tray. (Courtesy of Koch Engineering Co.)
In the past, three basic tray designs retical stage) than correspondingly
— bubble cap, sieve, and valve — sized tray systems. Therefore, pack-
were the dominant distillation inter- ing usually is selected over trays in
nals in the CPI. Bubble-cap trays as- applications ranging from atmospher-
sure total contacting in high- ic to low-pressure/high-vacuum. In
vapor/low-liquid contacting situa- general, operating at a lower system
tions; however, such trays tend to be pressure and pressure drop raises the
more expensive, heavier, and to pro- relative volatility, allows for lower re-
duce higher vapor pressure drop, boiler temperatures, and may enable a
which leads to greater energy con- reduced reflux ratio or a higher prod-
sumption. Sieve trays have less hard- uct purity. This also translates into
ware and, so, are much lower in cost; lower utility usages. Packing, as al- ■ Figure 3. VGMD high-performance
they, however, offer limited turndown ready noted, also is favored for small- tray. (Courtesy of Nutter Engineering/
relative to bubble-cap or valve trays. dia. columns, where fabrication costs UOP Inc.)
Valve trays, which are intermediate in for trays can be relatively high, and,
the price range, generally afford a to a lesser extent, in high-pressure modern random-packing geometries.
larger operating range than sieve trays distillations where tray columns are If corrosion of the existing inter-
and also minimize weeping at low downcomer limited. nals has been detected, consider a
vapor rates and deflect entrainment at Random packing — This originat- packing with different material of
higher vapor rates. Valve tray designs ed ages ago with crushed rock and construction. Packing is readily avail-
often are proprietary and, therefore, glass, and progressed with the intro- able in various metals including spe-
close contact with the internals vendor duction of Pall rings in the 1960s. cialty alloys, ceramics, plastics, and
may be required in evaluating possi- Today, a wide variety of random glass-reinforced plastics. Because of
ble configurations. Although all three packing types are commercially avail- increasing understanding of the im-
types are still widely in use, improved able, with sizes ranging from 1–31- portance of liquid adherence to the
tray designs recently have been devel- in. nominal dia. Random packing has packing surfaces, many vendors are
oped, and should be considered first complex surfaces and high open area modifying surfaces to increase
for an internals revamp. to minimize pressure drops while wetability. Maintaining the physical
The new high-performance trays maximizing vapor/liquid contacting. integrity of packing (durability) also
enable distillation at higher capaci- Figure 4 shows an assortment of is important, as too often breakage

MARCH 1998 • CHEMICAL ENGINEERING PROGRESS

D I S T I L L AT I O N R E VA M P S

occurs — leading to fluid maldistri- ■ Figure 4. An

bution, unwanted pressure drops, and assortment of
random packings.
losses in separation efficiency. (Courtesy of Koch
Packing size (diameter) is a signif- Engineering Co.)
icant design parameter. The height
equivalent to a theoretical plate
(HETP) declines with decreasing
nominal packing diameter; this, how-
ever, is at the expense of increased
pressure drop across the same height
of column. While smaller sizes en-
able better mass transfer, they also
can create higher pressure drop and
lower capacity. This must be bal-
anced against wall effects that can
occur. A rule of thumb is to limit the
packing diameter so that at least eight
packing pieces would fit across the
column diameter.
Random packing is most applied
in revamping small diameter
columns, large columns with noncriti-
cal product-stream specifications, and dors include Jaeger Products, Koch results, which is, in effect, the con-
columns where synthetic materials Engineering, Norton, and Nutter version between theoretical and actu-
are preferred, for instance, because of Engineering. al stages.
highly corrosive or low-temperature Liquid distributors — Properly de- In working with the desired ranges
operating conditions. The volumetric signed and operated liquid distribu- of feed and all product streams, the
cost for random packing typically is tors are critical in packed columns, required fractionation stages must be
less than that for structured packing, because poor distribution will severe- determined. The first option is to bal-
and random packing revamps are ly reduce vapor/liquid mass transfer. ance the number of stages against re-
quick and easy to implement. Some Liquid redistribution within a packed flux ratio. By increasing reflux ratio,
of the vendors supplying high-effi- column also is crucial for effective you boost the fractionation. To ac-
ciency random packing include mass transfer throughout the column commodate this change, the thermal
Jaeger Products, Koch Engineering, height. In general, liquid redistribu- capacity of the column (specifically,
Norton, and Nutter Engineering. tion plates should be inserted for the reboiler and condenser) must be
Structured packing —This fre- every 8–10 ft of column height.
quently is the preferred internal in re- Strigle (6) provides guidelines on liq-
vamps where high efficiencies or low uid distributor designs.
pressure drop and high capacity are
advantageous. Structured packing, Determine stage efficiency
which typically is fabricated from and required fractionation
corrugated sheet metal or synthetic Now, you are ready to evaluate the
materials, offers an even-lower pres- sufficiency of the existing column
sure drop per HETP and more capaci- height and its corresponding number
ty than random packing. Structured of stages. By coupling the field trial
packing HETPs continue to decrease, with the simulations, you should be
thereby boosting its attractiveness for able to verify the critical column pa-
revamps where greater fractionation rameter — stage efficiency. Internals
is a key objective. Because of in- vendors frequently can provide stage
creasing competition in the market- efficiencies for common systems. Al-
place, the cost of structured packing though reliable stage-efficiency val-
has declined to the point where it ef- ues may not be readily available for
fectively competes with random many revamps, the stage efficiencies ■ Figure 5. An example of structured
packing. (Courtesy of Jaeger Products,
packing on price. Figure 5 shows an can be calculated explicitly by com- Inc.)
example of structured packing. Ven- paring the simulations with the field

CHEMICAL ENGINEERING PROGRESS • MARCH 1998

capable of handling the correspond- The third cost consideration in- waste material at times was difficult
ing loads. Conversely, increasing the volves the engineering requirements to handle, which affected the cost of
number of stages by adding height to or fees to determine the best revamp- disposal. From an environmental and
the column (or revamping with high- ing strategy and design. It is most safety standpoint, the process materi-
er efficiency internals) allows a lower economical to handle the project in- al was an EPA-listed air pollutant and
reflux ratio and boilup rate for the ternally at the plant level or to hire a considered a carcinogen. Ultimately,
same degree of fractionation and col- distillation operations specialist. If, the issues at hand had led to a prof-
umn productivity. instead, you choose an outside engi- itability limitation, which the compa-
An increase in column height neering firm, bear in mind that some ny naturally wanted to overcome.
sometimes can be accomplished with less technically proficient engineering The chemists and engineers asso-
an extension of a flanged vessel; a firms operate on the same basis as ciated with the product line had iden-
structural analysis of the column is re- equipment vendors — effectively tified at least 12 potential process
quired to determine if this is feasible. charging a commission based on the causes of inadequate product purity
size of the total project. and appearance. A field investigation
HOW TO ANALYZE To reiterate: though it may cost was performed to ascertain when the
THE ECONOMIC IMPACT more initially to take the step-by-step product-quality and yield concerns
Using the guidelines and the order approach outlined here, this approach became most prevalent. Both subse-
of preferences described above, you will truly identify what is needed to quently were correlated to the propor-
can develop a strategy based on the achieve the desired results. Ultimate- tion of recycled feed materials from
economic realities of achieving cus- ly, this process often yields much the distillation system to the reaction
tomer requirements, system operabili- higher returns, especially from de- and separation trains.
ty, and reliability. Now, you have to creased downtime and eliminating The existing distillation system
assess the strategy’s costs, which pri- unnecessary changes. The potential processed reaction and separation sol-
marily consist of: economic gains achievable through vents and other reactants, and much
• distillation system downtime; this approach include: solvent was being lost with the waste
• capital expenditures; and • increased system throughput; materials. Also, higher volatility
• engineering requirements or fees. • higher recovery of raw materials; byproducts were being formed both
In most revamp projects, down- • better product yield; in the reactor and the still itself,
time is the largest economic factor. • more efficient energy usage; which led to increased disposal costs
Significant downtime can lead to lost • reduced waste-disposal quanti- and potential liability from shipping
market share or the need to buy from ties and costs; and large quantities of hazardous waste
competitors to supply customer ac- • more efficient use of operating on a daily basis.
counts. Further, in an integrated facil- personnel. The system, which had been in op-
ity, downtime within the distillation eration for more than a decade, con-
system often can cause outages that PROVEN IN PRACTICE sisted of a single-stage column (with
negatively impact other units. I have applied this approach to a wide no column internals) fitted with a
Capital expenditures usually are range of distillation processes. Here are jacketed, steam-heated kettle reboiler.
secondary to downtime costs. To esti- some examples to provide a sense of what The vacuum system was piped to a
mate the cost for retrofitting column can be accomplished. single receiver with two condensers
internals, consult the recent article by in series. It was a batch system with
Bravo (21). Investment for revamping Solvent recovery minimal process controls, mainly
the instrumentation and controls, an- Company X decided to take a on/off valving and a few temperature
cillary equipment, such as the reboiler fresh look at one of its well-estab- and pressure gages.
and condenser, and the column vessel lished, profitable manufacturing pro- One of the previously proposed
can be estimated using standard tech- cesses. Although the initial goal was engineering designs was to achieve
niques. When considering capital ex- to produce a higher-purity product at greater fractionation of three compo-
penditures, always keep in mind that higher capacity, the project rapidly nents via a column internals revamp
incorporating the proper system com- developed additional objectives. The and extensive process instrumenta-
ponent to accomplish the strategy is plant manager was concerned about tion and control. The components, in
more important than saving a few dol- raw material costs and customer com- order of decreasing volatility, were
lars on a lesser piece of equipment. plaints about product purity and ap- the reaction solvent, the separation
Also, remember that one of the best pearance. The production engineer solvent, and the reaction byproducts.
ways to avoid unnecessary expenses was troubled that yields sometimes To reduce the solvent losses through
is to resist the temptation to buy new were low, the quantity of waste mate- the condenser and into the wastewa-
equipment to solve every problem. rial was inconsistent, and that the ter system, the design replaced the

MARCH 1998 • CHEMICAL ENGINEERING PROGRESS

D I S T I L L AT I O N R E VA M P S

existing steam-jet vacuum with a vac- By using the single solvent, the the lightest components into the sal-
uum pump system having a refriger- distillation was converted from a able component also was occurring,
ant-based condenser system. This batch operation to a semicontinuous and the true distillation yields were
proposed revamp would have cost in one, which achieved several objec- unknown.
excess of $2,000,000. It, however, tives for the revamp. The first was in- To achieve the desired distillate
would not have solved the product creased solvent recovery, which en- purity, the design engineers analyzed
quality issue, improved the environ- abled the plant to process consider- the system and developed two re-
mental aspects of the process, or re- ably higher quantities. Final product vamping proposals. One involved re-
duced the disposal costs. purity also was greatly improved due placing the batch still with a thin
Through careful analysis using the to better purity of the solvent. Addi- film evaporator and a three-column
approach discussed in this article, the tionally, because the distillation bot- distillation train including con-
revamping engineers came up with a toms’ concentration and viscosity densers, reboilers, accumulators,
far better alternative. were controllable, the company was pumps, and controls. The second de-
By identifying what the problems able to pump the bottoms to the boil- sign retained the existing still, fol-
were upstream, the engineers more er house for reliable on-site destruc- lowed by a three-column distillation
realistically determined what would tion, which was significantly less ex- train and its associated equipment
make the most sense in the distilla- pensive (and more politically correct) and controls. Either design would
tion process. The challenges to the than shipping it off-site. have required a capital expenditure
distillation included wide variations In summary, a costly revamp was in excess of $1,000,000.
in the feed to the still due to inconsis- avoided by understanding the limita- Fortunately, the approach dis-
tencies among reaction endpoints. tions of the existing distillation sys- cussed in this article then was used.
This became the focus of a short-term tem, modifying the upstream process, On-site analysis identified several
process-development project. It led to converting the operational mode, ad- problems within the existing opera-
alteration in the reaction conditions dressing the environmental concerns, tion. One of the key trouble areas was
and conversion of the reaction and and then retrofitting only a minimal that liquid maldistribution frequently
separation process from a three com- amount of equipment. occurred throughout the batch distil-
ponent system to a two component lation process, impeding fractiona-
one employing the same lower- Pharmaceutical intermediate tion. The existing column was operat-
volatility solvent for both the reaction purification ed on a variable reflux algorithm; the
and separation. Company Y needed to revamp a equipment, however, had been over-
Laboratory distillation deter- batch distillation operation to meet sized to the point that adequate liquid
mined that the reaction byproducts customer requirements for purity of a distribution was maintained only at
were extremely viscous, reaching particular pharmaceutical intermedi- higher reflux rates. The control algo-
more than 1,000 cP at room tempera- ate. The existing column contained rithm and the structured packing in-
ture, and that a stagnant reboiler structured packing with four receivers ternals, coupled with the batch opera-
mixture exhibited detrimental foam- in parallel and had variable reflux tion mode, also restricted the produc-
ing characteristics. In the laboratory, control based on single-loop con- tivity in the larger fraction cuts (the
the solvent in the still bottoms could trollers. It was operated under various five distillation cuts ranged from a
be limited to a few percent. In the vacuum settings utilizing a two-stage few percent to 45% of the feed); op-
plant, the properties of the still bot- steam-jet system. The process was erators frequently overrode the sys-
toms, including viscosity and solvent very operator intensive, requiring up tem controls to improve boilup rates.
holdup, varied widely even though to 80% of the operators’ available at- The feed composition to the still var-
the same temperature and vacuum tention. Additionally, because product ied considerably — however, most of
endpoints were consistently used. specifications were not met, large the variance could be attributed to
The laboratory distillation proved quantities had to be reprocessed. two components, one of which was
that the single-blade propeller agita- The challenges included variable the highest volatility component.
tor in the still simply didn’t provide feed concentrations from one batch to After the field observations were
agitation and, therefore, the interfa- the next. Also, the operation pro- made, the system was modeled on a
cial transfer quickly declined as the duced six components, and the purity simulator — first, batchwise and,
surface became quiescent in the of the salable one — a component of then, in a semicontinuous mode, ad-
early stages of solvent removal. So, intermediate volatility — was very justing the reflux ratio to maintain
the kettle was retrofitted with a dual inconsistent, typically ranging from adequate internal liquid rates for the
axial impeller, which induced a 90–95%, while the customer demand- existing column internals. Through
high-velocity axial flow and more ed purity levels in the >95% range. the simulations, the revamping engi-
interfacial transfer area. Unacceptable cross-contamination of neers determined that the current

CHEMICAL ENGINEERING PROGRESS • MARCH 1998

equipment could provide the desired Achieve the optimum it is developed only through practi-
fractionation with the desired purity, The approach presented here will cal experience and a thorough under-
improved yield, and at higher pro- enable you to effectively develop a standing of the engineering process.
ductivity rates, if the system was practical and profitable revamping The factors to consider in any distil-
converted from batch to semicontinu- strategy for distillation systems lation column revamp include:
ous operation. throughout the CPI. It is not intend- • the upstream process(es);
Next, the revamping strategy was ed to be a “cookbook” solution; in- • waste minimization;
to be confirmed in the field. The in- stead, it is more of an algorithm that • instrumentation and process
stalled instrumentation and the con- should be tailored to the specific sit- control;
trol, however, were not adequate for uation. Always remember that com- • plant and laboratory data;
semicontinuous operation; so, the ing up with the most economic over- • process simulation; and
field trial was conducted almost ex- all solution must involve taking into • the chemistry required for yield
clusively using manual control. Dur- account reliability, operability, maximization.
ing the plant trial, successful frac- downtime, and capital investment. As I have highlighted, using this
tionation was achieved for all six Although intuition does play a role, approach can pay big rewards. CEP
fractions, both with respect to distil-
late purity and cross-contamination.
Consistent increases in product puri-
ty and a gain in product yield also Literature Cited
were attained. 1. Humphrey, J. L., “Separation Processes: 12.Gmehling, J., U. Onken, and W. Arlt,
Ultimately, the revamp did not re- Playing a Critical Role,” Chem. Eng. “Chemistry Data Series: Vapor-Liquid
quire additional columns, but only a Progress, 91 (10), p. 31 (Oct. 1995). Equilibrium Collection” (continuing se-
change from batch to semicontinuous 2. Henley, E. J., and J. D. Seader, “Equi- ries), DECHEMA, Frankfurt, Germany
librium-Stage Separation Operations in (1979).
operation, as well as modified pro- Chemical Engineering,” Wiley, New 13.Hala, E., J. Pick, V. Fried, and O.
gramming of the controllers. As a re- York (1981). Vilim, “Vapor-Liquid Equilibrium,” 2nd
sult, more than $1,000,000 of unnec- 3. Treybal, R. E., “Mass-Transfer Opera- ed., Pergamon, Oxford, U.K. (1967).
essary capital expenditures were tion,” 3rd ed., McGraw-Hill, New York 14.Hala, E., I. Wichterle, J. Polak, and T.
avoided, along with the costly down- (1980). Boublik, “Vapor-Liquid Equilibrium at
time to implement them. Further, the 4. Kister, H. Z., “Distillation Operation,” Normal Pressures,” Pergamon, Oxford,
required operator involvement was McGraw-Hill, New York (1990). U.K. (1968).
reduced, and product rework was vir- 5. Diweker, U. M., “Batch Distillation,” 15.Reid, R. C., J. M. Prausnitz, and T. K.
Taylor & Francis, Washington, DC Sherwood, “The Properties of Gases and
tually eliminated. There also was an (1995). Liquids,” 3rd ed., McGraw-Hill, New
environmental benefit to the revamp, 6. Strigle, R. F., Jr., “Packed Tower Design York (1977).
in that waste disposal was dramatical- and Applications: Random and Struc- 16.Carlson, E. C., “Don’t Gamble with
ly decreased due to greater productiv- tured Packings,” 2nd ed., Gulf, Houston Physical Properties for Simulations,”
ity per heel discharge. (1994). Chem. Eng. Progress, 92 (10), p. 35 (Oct.
7. Kister, H. Z., “Distillation Design,” Mc- 1996).
Graw-Hill, New York (1992). 17.Ja::imovi::, B. M., and S. B. Geni::,
8. Perry, R. H., D. W. Green, and J. O. “Use a New Approach to Find Murphree
J. A. WILLIAMS is General Manager of EPS: Maloney, “Perry’s Chemical Engineers’ Tray Efficiency,” Chem. Eng. Progress,
Environmental & Production Solutions, LLC, Handbook,” 6th ed., Chap. 13, McGraw- 92 (8), p. 46 (Aug. 1996).
South Bend, IN (219/277–2577; Fax:
Hill, New York (1984). 18.Kister, H. Z., “Troubleshoot Distillation
219/277–3775; e-mail: eps@asme.org). He
has more than 12 years of experience with
9. Bowman, J. D., “Use Column Scanning Simulations,” Chem. Eng. Progress, 91
chemical, pharmaceutical, and energy- for Predictive Maintenance,” Chem. Eng. (6), p. 63 (June 1995).
generation companies in industrial research Progress, 87 (2), p. 25 (Feb. 1991). 19.Hanson, D. W., S. W. Golden, and G.
and development, process development, 10.Bowman, J. D., “Troubleshoot Packed R. Martin, “Make the Most of Distilla-
and plant operations. He received a PhD Towers with Radioisotopes,” Chem. Eng. tion Test Runs,” Chem. Eng. Progress,
and an MS from the Univ. of Utah in Progress, 90 (9) p. 34 (Sept. 1994). 92 (2), p. 72 (Feb. 1996).
chemical and fuels engineering, and a BS 11.Gess, M. A., R. P. Danner, and M. 20.Kunesh, J. G., H. Z. Kister, M. J. Lock-
from the Univ. of Delaware in chemistry, as Nagvekar, “Thermodynamic Analysis of ett, and J. R. Fair, “Distillation: Still
well as an MBA from the Univ. of Chicago.
Vapor-Liquid Equilibria: Recommended Towering Over Other Options,” Chem.
A registered professional engineer in six
states, he is an AIChE lecturer on the
Models and a Standard Data Base,” De- Eng. Progress, 91 (10), p. 43 (Oct. 1995).
economic evaluation and development of sign Inst. for Phys. Prop. Data, AIChE, 21.Bravo, J. L., “Select Structured Packings
engineering projects. He is a member of New York (1991). or Trays?,” Chem. Eng. Progress, 93 (7),
AIChE, ACS, ASME, and ISA. p. 36 (July 1997).

MARCH 1998 • CHEMICAL ENGINEERING PROGRESS