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Maximize efficiency in distillation, absorption, stripping and extraction

Jose L. Bravo Shell Oil Co.; Edited by Irene Kim

Jose L. Bravo Shell Oil Co.

Over the last two decades, development in distillation and extraction

technology has focused on contacting devices and simulation tools for
analysis <1>. The driver has been a push for more capacity in existing
plants. Hence, new mass-transfer devices offer increased vapor- or liquid-
handling abilities within existing column shells. These devices reduce the
cost of new installations by providing more throughput per unit volume of

In the fields of distillation, absorption, stripping and extraction, theory and

technology go hand in hand. The thermodynamic principles of phase
equilibrium and the concepts of mass transfer and fluid flow are of primary
importance in all of these operations. The engineer must understand these
phenomena to select equipment effectively.

This article discusses the latest in commercial technology in column

internals for gas-liquid and liquid-liquid contacting. The principles of
operation are explained vis-a-vis the characteristics of the applications in
which they are used. The focus is on moderate-to-large columns for
refining and chemical applications. Guidelines for selecting the most
appropriate type of device are presented, and examples of typical
applications are described.

Principles of mass transfer

Mass-transfer devices, such as packings and trays, enable mass transfer to

occur in a given volume in distillation, absorption, stripping and extraction
columns. To achieve this, a device must allow two or more phases (vapor
and liquid, or two immiscible liquids) to intimately contact, but separate
once the transfer occurs. The device's ability to effect the contact
determines its efficiency; its ability to separate the phases determines its

Efficiency The rate of mass transfer depends on how well a device

performs and on the process fluids' physical properties, such as volatility
and viscosity. Mass-transfer efficiency per unit volume (i.e., high mass-
transfer rate) is achieved by providing large amounts of interfacial area for
the phases to exchange mass. In addition, mass transfer is enhanced via
interfacial and bulk turbulence. At the same time, plug-flow conditions and
uniform phase distribution must be maintained.
Of the three items, the first two are discussed in detail by mass-transfer
operations textbooks <2,3>. But the third, i.e., the effects of phase
distribution on mass-transfer efficiency, is usually inadequately discussed.
This item (addressed in a later section), has crucial implications in the
design and analysis of separations equipment <4>.

Capacity At the same time, a mass-transfer device's capacity is

dictated by its ability to allow the phases to separate effectively. The
hydraulic capacity of a mass-transfer device, roughly defined, is the point
where the phases cannot come apart after being put in contact (more-
subtle definitions of capacity relate to the point where mass-transfer
efficiency is lost in spite of available hydraulic capacity). In this sense, the
devices with the most capacity limit the entrainment or carryover of one
phase in another, and act as efficient phase separators. High-capacity
devices also preserve the plug-flow nature of the contacting.

In terms of both capacity and mass-transfer efficiency, a device's ability to

promote and preserve good phase distribution directly affects its
performance. It's no wonder that engineers are concerned with liquid- and
gas-distribution issues in these separations operations.

Two phases Another important concept is that of dispersed and

continuous phases. The dispersed phase in a column is broken up into
drops, bubbles and films (commonly called ``holdup''). The continuous
phase fills the void in the column left by mass-transfer devices. Examples
of dispersed and continuous phases in various devices are:

Packed column under vacuum-distillation conditions: The vapor is

continuous, and the liquid is dispersed

Tray column under pressure-distillation conditions: The liquid is the

continuous phase on the trays, and the vapor is dispersed in the form of
bubbles in a froth. The space above the froth is continuous vapor, with a
small fraction of dispersed liquid

Extraction column with its main interface at the top: The heavy phase is
continuous; the light phase is dispersed

Extraction column with the main interface at the bottom: The light phase
is continuous, and the heavy is dispersed

Countercurrent contacting

Most industrial distillation and extraction operations take place in

countercurrent fashion, i.e., the phases move in opposite directions. The
light phase in extraction (or vapor in distillation) moves upward in a
column, and the heavy phase or liquid moves downward.

Some special absorption applications involving fast reactions in the liquid

phase (i.e., acid-vent-gas control) use crossflow scrubbers, where the gas
moves horizontally and the liquid moves vertically downwards. Still other
reactive-absorption applications involve cocurrent flow, as in venturi
scrubbers. Crossflow or cocurrent devices are generally less efficient than
countercurrent ones (except where fast reactions of the absorbed
component take place in the liquid phase).

However, phase contact within a vessel e.g., on particular trays may

not be truly countercurrent although the overall configuration is
counterflow. The most common example of this is a conventional tray
column, where contact in each tray takes place with the liquid flowing
across the tray, while the vapor flows vertically through the liquid
(crossflow tray). Some newer devices, such as the so-called ``Trutna Tray''
<5>, actually contact the gas and liquid in a cocurrent fashion within the
tray, but produce a net countercurrent effect in the column.

Packed extraction and distillation towers are true countercurrent devices.

Here, the contacting takes place countercurrently within the device itself.

Axial mixing and plug flow In all the cases described above, axial
mixing (mixing in the direction of overall flow) is detrimental to mass-
transfer efficiency. This is because mixing in the direction of flow actually
reduces the concentration gradients available for mass transfer,
consequently reducing the volumetric efficiency of the device.

Various forms of axial mixing or axial dispersion can occur. The most
common is phase maldistribution, where one or both phases in a column
show an uneven velocity profile in portions of the column. This is the type
of maldistribution often associated with trickling liquid in packed columns.
Also, the lack of true plug flow in liquid-extraction columns leads to lower
efficiencies through conventional axial dispersion, which mixes the
continuous phase in the direction of flow.

Modern contacting devices for distillation and extraction strive to maximize

plug-flow characteristics by promoting radial distribution and preventing
axial dispersion of both phases. These devices also preserve phase
distribution as flows progress up or down inside a column.

In general, an effective mass-transfer device for separation:

Provides large amounts of interfacial area for phases to exchange mass

Enhances mass transfer through interfacial and bulk turbulence

Limits the entrainment or carry-over of one phase in another

Acts as an efficient phase separator

Preserves the plug-flow nature of the contacting (i.e., limits axial mixing)

Promotes radial distribution of the dispersed and continuous phases

Preserves phase distribution as flows progress up or down the column

Operates at low pressure-drop/mass-transfer-efficiency ratios (pressure

drop per theoretical stage)

Can be installed easily and properly in a column and has the required
mechanical strength

Column internals

The internals used in industrial columns can be roughly classified into two
categories: trays and packings.

Trays promote contact between vapor and liquid through bubbling and
jetting. In this article, we will consider ``conventional trays'' to be those
with traditional downcomers. The bubbling devices of conventional trays
are bubble caps or valves, or the holes of a sieve tray.

High-performance trays feature improved downcomer designs that

enhance liquid handling ability or liquid distribution. These tray designs
can also incorporate improved bubbler designs, such as reduced-size
valves or directional devices (box, p. 82).

Packings for gas-liquid contacting can be divided into three main

categories: random, structured and grid. Each type has a defined set of
characteristics (box) that makes it more or less suitable for a particular
application. But all offer reduced pressure drops, compared to trays.

In industrial applications, internals for extraction include the trays and

packings described above, plus mechanically agitated devices. The use of
mechanical agitation in extraction applications is still fairly common,
particularly in applications using small columns (e.g., less than 2 ft dia.).
Generally speaking, refining and bulk-chemical plants tend to use packed
or tray extractors, whereas food and pharmaceutical plants tend to use
agitated extractors more often.

The selection of the most effective mass transfer internals for a distillation
application depends on the conditions of the distillation. A recent paper
<25> describes a procedure to select the most appropriate device based on
the value of the flow parameter, Fp.

F subscript p = L/G (rhog/rhol) 1/2

where L = liquid mass velocity, G = gas mass velocity, rhog = gas density
and rhol = liquid density

In distillation applications, the value of the flow parameter can be directly

correlated with operating pressure, with the lowest values corresponding
to vacuum distillation and the highest, to pressure distillation.

A situation particular to distillation is the simultaneous existence of

saturated (boiling) liquid and saturated vapor, enabling heat transfer and
mass transfer to take place at the same time. The continuous vapor
condensation and boiling of liquid produces large surface-renewal rates
that enhance the available interfacial area and mass transfer. Distillation
thus produces the largest volumetric efficiencies for mass transfer,
compared with absorption, stripping or extraction.

The Figure on p. 80 shows that packings are the device of choice at low
flow parameters in terms of maximum available capacity, whereas trays
yield more capacity at high flow parameters.

Distillation at low pressures (less than 1 atm) Vacuum distillation is

characterized by:

High vapor velocities

Low liquid loadings

Low flow parameters

Critical pressure drop

Temperature-sensitive products

Large variations in vapor density from column top to bottom

High liquid-entrainment tendencies

High inlet velocities due to flashing feeds

Low-pressure distillation is the unquestionable domain of structured
packings <25>. Random packings are second, in terms of applicability;
trays need only be considered when fouling cannot be mitigated, or when
ineffective packing wetting may be a problem.

Preferable over trays because they offer lower pressure drop and reduced
entrainment tendencies, packings provide better volumetric efficiency than
trays in vacuum distillation and produce smaller, less-expensive new
towers for the same capacity or offer much better capacity in existing tower
shells. The cost-performance ratio for structured packings is low, and
payout times for retrofits are generally short.

When structured packings are considered for vacuum distillation, these

design issues merit special attention:

Liquid-distributor design and installation for low-liquid-load applications

High-velocity vapor inlets and reboiler returns; vapor distribution

Entrainment and carryover from liquid distributors and collectors

Liquid-distributor and -collector open area and pressure drop

Flashing-feed inlet design

Packing support, hold-down open areas

Packing size selection per pressure drop criteria (as opposed to only
considering capacity criteria)

Some large vacuum-distillation operations taking advantage of structured

packing performance are:

Styrene-ethylbenzene separation

Separation of glycols from water, and from each other

Glycerin separation

Vacuum flashers in refineries

High olefins fractionation

Distillation at medium pressure (1-4 atm) A wide range of devices can

be used for distillation at near-atmospheric conditions. Here, liquid and
vapor loads are moderate, relative to other applications. The selection of
the most appropriate device tends to depend on issues such as fouling,
corrosion, foaming and cost.

Examples of this type of distillation can be found in the main fractionators

of refineries. These columns generally operate a few pounds above
atmospheric pressure and in a wide range of temperatures. These columns
are sensitive to entrainment and fouling (i.e., coking). Modern designs
include the use of structured packings in upper sections to minimize
entrainment, with trays in lower sections to mitigate fouling. In many cases,
grid-type packings are used in the most-fouling sections of the tower,
especially in sections with heavy coking tendencies.

In general, the lower the pressure, the more attractive packings will be in
terms of capacity, when fouling is not a consideration. Here, the volumetric
efficiency of packings and trays is equivalent. Packings do offer the
advantage of lower pressure drop, which can be important when
temperature is of concern (e.g., because of product degradation or heat-
medium limitations). Packings are better to address foaming systems, but
offer less corrosion resistance than trays when metal construction is used.

Distillation at high pressure (above 4 atm) These applications are

characterized by the following:

Low vapor velocities

High liquid loadings

High flow parameters

Noncritical pressure drop (except in highly energy-integrated cases)

Low liquid entrainment tendencies

Small density differences between vapor and liquid

Low surface tensions

In many cases, and with notable exceptions described below, high-

performance trays are the device of choice in these distillations <25>.
These trays have better abilities to handle high liquid loads and allow for
efficient phase separation of dense vapor from liquid. Furthermore, the
added pressure drop of trays tends to reduce the axial mixing that appears
to plague structured packings in particular <26>.

At the same time, however, there are some important exceptions to the
advantages of trays in these applications. In the case of cryogenic
separation of air (into oxygen and nitrogen), the pressure drop across the
distillation column is crucial in terms of its effect on the temperature

Lower pressure drops mean less temperature difference between column

top and bottom, translating into important savings in heat-pumping costs.
In this case, even though the distillation is performed at high pressure, the
lower pressure drop offered by structured packings makes them desirable.
For example, air-separation firms commonly use structured packing in their
``cold boxes.''

Trays may not be best in high-pressure distillation when low surface

tensions tend to cause foaming. When this is combined with moderate
liquid loads, such as cryogenic demethanizers, random packings are often

The advantages of high-performance trays over conventional trays come

from their increased ability to handle large liquid loads through specialized
downcomer designs. High-performance trays can also be used at reduced
tray spacings, offering better volumetric efficiency than conventional units.
These high-capacity trays allow new towers to be made smaller for the
same rating, or offer increased capacity in existing tower shells.

For pressure-distillation applications of high-performance trays, the

following issues merit particular attention:

Liquid-feed-distributor design, as well as installation, for high-liquid-load


Pressure drop on the tray and its effects on downcomer backup

Efficient liquid distribution across the tray. Flow-path lengths must be

kept to prevent efficiency loss

Prevention of bridging of the downcomer inlet by high liquid-inlet


Downcomer-inlet geometry for low-surface-tension systems

Potential compromise between possibly reduced efficiency and

additional stages offered by increased capacity

Some high-pressure distillation operations that benefit from high-

performance trays are:

De-ethanizers in gas plants

De-propanizers in crude unit light ends systems

De-butanizers in cat-crackers

Propane-propylene splitters

Ethane-ethylene superfractionators

Reactive and catalytic distillation A special application of distillation

is one where a significant chemical reaction takes place within the
distillation column. Commercial applications of this technology include the
manufacture of MTBE and TAME, as well as methyl acetate. Some newer
applications of simultaneous hydrotreating and distillation are also finding
their way into refineries as operators strive for cleaner-burning fuels.

When reactive distillation requires a solid catalyst (e.g., etherification and

hydrotreating processes), the catalyst itself becomes a mass-transfer
device for distillation. This type of device has also seen development in the
last few years. Structured catalytic packings now provide mass-transfer
and hydraulic performance equivalent to other distillation devices, while
providing enough catalyst volume for the required reaction (box, above).
Two high-performance catalytic packings are listed for reactive distillation
(box, p. 82). The catalyst used in these packings can be selected for a
particular reaction, while the packing is selected to fit the distillation
requirements of separation and throughput.


In absorption, one or more components are moved from a gas mixture into
a liquid solvent. Unlike distillation, absorption applications involve gas and
liquid phases that are not undergoing bulk condensation or boiling. Herein
lies the most important difference between distillation and absorption:
Volumetric rates of mass transfer are low in the noncondensing systems.

Good absorption solvents exhibit high solubility and selectivity for the
desired component. In many cases, solubility and selectivity are enhanced
via a chemical reaction in the liquid that allows the solution uptake to be
larger and faster. This is the principle of chemically enhanced absorption.
Physical absorption is also commonly used. In some instances, as in the
case of ammonia absorption into water, the lines between reactive and
physical absorption are blurred.

Internals for absorption applications can be categorized by their efficiency.

On one side are absorbers selected to do large amounts of absorption, but
not to achieve high-purity effluents. These devices operate cocurrently and
include venturi scrubbers and other devices that rely on intensive liquid
and gas mixing. At best, they can achieve close to one theoretical stage of
contact. However, they have the advantage of operating even under high
temperatures and dust loads.

On the other hand, trayed and packed countercurrent absorbers can

achieve low concentrations with lower solvent rates by providing multiple
stages of contact. Nevertheless, this type of absorber has problems
handling solids and can be cumbersome at high temperatures. An
interesting feature of these packed or tray absorbers is that the liquid
holdup (i.e., dispersed phase) can be manipulated to affect selectivity in
reactive-absorption applications.

The most common mass-transfer devices used in absorption are packings.

Most absorptions operate at low flow parameters. Also, since most
absorption reactions are fast, low liquid holdups (which imply short
residence times) work well.

An interesting example is the joint absorption of CO2and H2S from natural

gas. These are commonly absorbed into alkanol-amine solutions in
refineries and gas plants. The selectivity between CO 2and H2S can be
manipulated by the selection of the amine, as well as by the liquid
residence time. One tends to see packed towers when the absorption of
H2S is to be favored; tray towers with larger holdups will also show
extensive CO2absorption.

Plastic internals In many chemical absorptions involving corrosive

process fluids, the use of plastic column internals is common. Random
plastic packings offer some advantages.

The use of plastic, which is nonwettable by water, poses few limitations to

efficiency. This is because absorptive systems provide interfacial area in
the form of drops and rivulets, and the amount of wetting of the packing
that takes place is insignificant to the overall process. What remains
crucial is liquid and gas distribution. The mass-transfer and hydraulic
characteristics of absorbers are the same as those of distillation columns.

Scrubbers Cross-flow scrubbers are popular in certain fields. Though

these cannot surpass the efficiency of countercurrent scrubbers, they find
application in reactive absorption with fast reactions. In these cases, since
there is no liquid-concentration gradient (i.e., the process fluid is not mixed
with any other substance) they can be effective, offering lower pressure
drops though requiring larger liquid flows. Their most important
characteristic is their low profile; when installed, they are less bulky than
vertical towers.

In stripping, a volatile component is removed from a liquid. The lower
portions of distillation columns are generally called ``stripping sections''
for this reason. Unlike absorption, many stripping applications involve
boiling liquids and condensing vapors in contact with each other. In this
fashion, stripping is really a subset of distillation. Exceptions to this are
common inert-gas strippers used to remove volatile organics from water.
(i.e., air strippers). In these, as in absorption, both phases are removed
from saturation.

Some strippers must also deal with reactive systems, e.g., in the case of
ammonia and H2S removal from ``sour'' waters in olefin plants. The removal
efficiency of these strippers is affected significantly by the pH of the water.

Most strippers operate at high liquid-to-gas-flow ratios, which put them into
the high-flow-parameter region. The hydraulics are dominated by the liquid
flow, and internal traffic in the column is dictated by the heat balance.

The use of trays or packings in strippers should follow the previously

described guidelines for distillation towers. Packed towers are not
recommended for fouling strippers, unless fouling-control measures are
taken. Some new tray designs address high liquid flow (e.g., Koch Max-
Frac trays) and fouling (Nutter MVG trays), and are well suited for many
stripping applications. New and improved downcomer and bubbler designs
can be used to great advantage.

Foaming An interesting aspect of mass transfer technology is the

treatment of foams a nemesis of tray towers. Engineers normally deal
with foaming by adding anti-foaming agents to the systems or by making
the towers large. Better technical solutions have found their way into use
these days:

Use a packed tower to prevent bubbling and jetting. Packed towers are
markedly superior when dealing with foaming systems

Use proper feed inlet devices. Many foaming problems start with
flashing or degassing feeds. New technology in inlet devices, such as
Portatest inlet cyclones, deal very effectively with this problem by
suppressing foam formation at the feed location

Design liquid distributors properly to avoid foaming, splashing and



Applications for solvent extraction, and in particular liquid-liquid

extraction, are common in the CPI. The issues of mass-transfer internals in
extraction columns are in many ways similar to those discussed above.
The mass-transfer principles of effective contacting and phase separation

The most important difference is that the two phases have relatively small
density differences; so extraction is performed at much lower relative
phase velocities than in distillation. In addition, the definition of
``continuous'' and ``dispersed'' phases depends only on the position of the
main interface: In distillation, the main interface is always in the column
sump; whereas, in extraction, it can be found above the internals (light
phase dispersed) or below the internals (heavy phase dispersed). This
subject is discussed extensively in the literature <27, 28>.

Two major types of extraction devices are used in the CPI:

Mechanically agitated devices, such as, Karr columns, mixer-settler

combinations, rotating-disk contactors (RDC) and York-Scheibel columns

Stationary devices, such as sieve-tray columns and packed columns

The box (above) summarizes the features of packings and trays for
extraction applications. Methods for estimating capacity and efficiency are
listed on p. 78.

High- and low-pressure extraction The behavior of extractors at high

pressures can be described with the same models as those at low
pressures, as long as the correct properties are available <29>. The effects
of interfacial tension, phase viscosity, and coalescence in the presence of
mass transfer play an important role in the design of a liquid extractor,
unlike a distillation column. These issues are usually the limiting factor in
the design. More importantly, reliable designs for new applications in
extraction generally require a pilot test to confirm capacity and efficiency
of the devices.

New developments and trends

Distillation, absorption, stripping and extraction represent so much of the

capital and operating costs of process plants that great incentive exists to
improve on the efficiency and capacity of the devices used in these
operations. Even small improvements can be attractive economically.
Accordingly, development of new, improved devices continues. These
developments are largely proprietary to the vendors and some operating
companies, and not available for public consumption. The few commercial
developments include the Trutna (cocurrent) tray <5> and the flow-control
tray <30>.
Nevertheless, developments are moving in the direction of trays that
essentially allow themselves to operate above the jet-flood point, but have
a secondary stage that separates the phases before they reach the tray
above. These flood-de-entrain devices can then handle larger loads than
devices that are limited by gravity alone. This concept has also produced
proprietary developments that use intense contact, followed by a positive
separation step. Some examples of these trays have seen limited
commercial application in the plants of their developers.

Packings have seen less development in the last ten years. Of significance
is the appearance of the Sulzer Optiflow packing, a new structured packing
for low liquid rates. It appears to offer the high efficiencies associated with
wire gauze structured packings, but at lower cost. Most developments in
the packing field are taking place in distributor (gas and liquid) technology
that allows the user to fully realize the inherent advantages of structured

Edited by Irene Kim


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2. Treybal, R., Mass Transfer Operations, McGraw-Hill, 1968

3. Sherwood, T. K. , Pigford, R. L. , Wilke, C. R., Mass Transfer, McGraw-Hill,


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1993, pp. 47-61

5. Trutna, W. R., Seibert, A. F. and Garcia, J. A., ``Trutna Tray performance

studies,'' AIChE Spring Meeting, Houston, March 1993

6. Muller, D., Marquardt, W. ``Distillation and Absorption `97,'' Inst. of Chem.

Eng., Symposium Series No. 142, 1997

7. Ilme, J. K., Keskinen, K. I., Markkanen, V. I., Aittamaa, J. R., ibid.

8. Wesselingh, H., ibid.

9. Fitz, Jr., C. W., Shariat, A., Kunesh, J. G., ibid.

10. Fair, J. R. and Bravo, J. L. , Chem. Eng. Prog., Vol. 86, No. 1;1990

11. Kister, H. Z., Distillation Design, McGraw-Hill, 1992

12. Robbins, L. A., Chem. Eng. Prog., May 1991, p. 87

13. Kister, H. Z. and Gill, D. R. , Chapter 10 in Distillation Design, McGraw-

Hill, 1992

14. Bravo, J. L., Rocha, J. A., and Fair, J. R., Hydrocarbon Processing,
March 1996

15. Bravo, J. L., Rocha, J. A., and Fair, J. R., ``Distillation and Absorption
`92,'' Inst. of Chem. Eng., Symposium Series, No. 128, 1992

16. Seibert, A. F. and Fair, J. R., ``Mass-transfer efficiency,'' Ind. & Eng.
Chem., Oct. 1993, p. 2213

17. Seibert, A. F., et al., ``Performance of a large-scale,'' Ind. & Eng. Chem.,
Sept. 1990, p. 1901

18. Chan, H and Fair, J. R. Ind. & Eng. Chem., Proc. Des. Dev. 23, 1983, p.

19. Bravo, J. L. and Fair, J. R., Ind. & Eng. Chem., Proc. Des. Dev. 21, 1982,
p. 162

20. Bolles, W. L. and Fair, J. R., ``Improved mass-transfer model,'' CE, July
1982, p. 109

21. Lockett, M.J., ``Structured packing HETP,'' presented at the AIChE

Spring Meeting, Houston, March 1997

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January 1995

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Eng. Chem. Res., 1996, pp. 1660-1667

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26. Zuiderweg, F., Olujic, Z., Kunesh, J. G., ``Distillation and Absorption `97''
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extraction,'' CE, September 17, 1984, p. 76

29. Seibert, A. F., Moosberg, D. F., Bravo, J. L. and Johnston, K. P., ``Spray,
Sieve-tray,'' Proceedings of the International Symposum on Supercritical
Fluids, Soc. Franaise de Chimie (1988)

30. Biddulph M. W., Lavin, J. T., and Thomas, C. P. ``Distillation and

Absorption `97,'' Inst. of Chem. Eng., Symposium Series No. 142, 1997


Jose L. Bravo is a specialist in separations and physical chemistry at Shell

Oil Co. (P.O. Box 1380, Houston TX 77251; Phone: 281-544-6721; Fax: 281-
544-8123). Previously, he worked for Jaeger Products, and was program
manager of the Separations Research Program at the University of Texas at
Austin, where he received an M.S. in chemical engineering. He has
extensive experience in the design and troubleshooting of mass-transfer
equipment and has published more than 30 articles in the areas of
distillation, absorption, extraction and stripping. He is also the senior
author of a book on separations technology. A member of AIChE, he is a
registered professional engineer in Texas.