LIQUID LIQUID EXTRACTION IN A PACKED BED

A seminar report

Submitted to

MEWAR UNIVERSITY

by

RAHUL RAGHAV

in partial fulfillment for the award of degree

of

BACHELOR OF TECHNOLOGY
IN

CHEMICAL ENGINEERING

DEPARTMENT OF CHEMICAL ENGINEERING

MEWAR UNIVERSITY
NH79, Gangrar, Chittorgarh ,Rajasthan, 312901

May 2014

1
 ACKNOWLEDGEMENT
We wish to express sincerely in great esteem, our gratitude and thanks to the Almighty GOD
for providing us through all the channels to achieve this stage.

We owe our regards to our Project guide Mr.Mehboob Alam ( Assistant Professor and
HOD) for his generous support to do this project. It was only due to his painstaking efforts
and help at various stages that the presentation of the work has been possible.

I extend my sincere thanks to my friends who are there with me directly or in directly during
the Work.

We would like to express sincere thanks to our parents, for enlightening the spirit of
dedication in us.

RAHUL RAGHAV

Roll No.-11MUBCHE008
Enroll No.-MUR1100388
th
6 SEM. CHEMICAL ENGINEERING

DEPARTMENT OF CHEMICAL ENGINEERING

Mewar University
NH - 79 Gangrar , Chittorgarh (Rajasthan) – 312901, India

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 CERTIFICATE

This seminar report entitled “LIQUID LIQUID EXTRACTION IN

A PACKED BED” submitted by RAHUL RAGHAV is accepted in
its present form by Department of Chemical Engineering, Mewar
University ,Gangrar in partial fulfillment of the requirement of the
award of degree of B.Tech. in Chemical Engineering. This is a
record of candidates own work carried by them under our supervision
and guidance. The matter embodies in this project has not been
submitted for award of any other degree.

MR. M.ALAM
Head Of Department
Department of Chemical Engg.
Mewar University

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 ABSTRACT

KEYWORDS: Liquid Liquid Extraction , Vaccum , Distillation ,Packed Bed Column

Liquid-liquid extraction is the separation of one or more components of a liquid solution by

contact with an immiscible liquid called the solvent. If the components in the original liquid
solution distribute themselves differently between the two liquid phases, separation will
result.
When separation by distillation is ineffective or very difficult, liquid extraction is one of the
main alternatives to consider .Close boiling mixtures or substances that can not withstand the
temperature of distillation, even under a vaccum, may often be separated from impurities by
extraction ,which utilizes chemical differences instead of vapour pressure difference.
This is the principle upon which separation
by liquid-liquid extraction is based, and there are a number of important applications of this
concept in industrial processes. The solvent should be selected so that it does not dissolve to
the solution to be processed ,but on the other hand it should dissolve the desired components
as much as possible, but no other components.

This thesis gives an overview of liquid-liquid extraction process, types of equipment used in
liquid-liquid extraction and the extraction of benzoic acid from toluene (dispersed phase) by
water (continuous phase) in a packed bed column.

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 CONTENTS

Title Page
ACKNOWLEDGEMENTS 2

CERTIFICATE 3

ABSTRACT 4

LIST OF FIGURES 6

NOMENCLATURE 7

CHAPTER 1 INTRODUCTION 8

1.1 History 8

1.2 Definitions 10

1.3 Properties of Ideal Solvents 12

1.4 Continuous Contact Equipment 16

1.5 Axial Dispersion 17

1.6 Liquid Liquid Extraction in A Packed Bed Column 18

1.7 Mass Transfer in A Packed Bed 20

CHAPTER 2 PROCEDURES & CALCULATIONS 22

CHAPTER 3 RESULTS AND DISCUSSIONS 23

CHAPTER 4 CASE STUDIES 25

REFERENCES 27

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 LIST OF FIGURES

 Fig1 -Part of extraction column on a truck

 Fig:-2 Diagram of mixture settler
 Fig.3 types of flow in extraction
 Fig.4-Knitmesh Coalescer
 Fig.5-Horizontal gravity settling vessel
 Fig.6-Spray Columns For Extraction
 Fig.7-Tray Columns For Extraction
 Fig.8-Tray Columns With Mechanical Agitation
 Fig.9-Podbielniak centrifugal extractor
 Fig.10-Effect of axial mixing on concentration profiles in towers subjected to axial
mixing
 Fig.11-Types Of Packing Used In Liquid Liquid Extraction
 Fig12-packed bed column
 Fig.13sulzer packing
 Fig.14 sulfolane process

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NOMENCLATURE

dFC =critical packing size

σ = interfacial tension
gc = gravitational conversion factor
VK= characteristic velocity
dp= drop diameter
ε=fractional void volume in packed bed
Vc=continuous phase superficial velocity
df= packing size
Ed=longitudinal dispersion coefficient
Vd=velocity in a downspout
KW a = overall mass transfer coefficient based on continuous phase
LT= molar flow rate of dispersed phase
LW = molar flow rate of continuous phase
KT a = overall mass transfer coefficient based on dispersed phase
QT= volumetric flow rate of toluene (dispersed phase)
QW= volumetric flow rate of water (continuous phase)
Z= packed height
V= volume of toluene in feed solution
HOW= height of transfer unit based on continuous phase
HOT = height of transfer unit based on dispersed phase
ΔCT1 = inlet concentration difference of benzoic acid in dispersed phase
ΔCT2 = outlet concentration difference of benzoic acid in dispersed phase
CT = concentration of benzoic acid in dispersed phase
CT*=equilibrium concentration of benzoic acid in dispersed phase
HW= individual height of transfer unit based on continuous phase
HT= individual height of transfer unit based on dispersed phase
m = slope of equilibrium curve

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CHAPTER 1
INTRODUCTION TO LIQUID LIQUID EXTRACTION

1.1 HISTORY
Extraction has been practiced since the time of the Romans, who used molten lead to
separate gold and silver from molten copper by extraction. This was followed by the
discovery that sulfur could selectively dissolve silver from an alloy with gold.
However, it was not until the early 1930s that L. Edeleanu invented the first large-scale
extraction process, the removal of aromatic and sulfur compounds from liquid kerosene
using liquid sulfur dioxide at 10 to 20_F.

This resulted in a cleaner-burning kerosene. Liquid–liquid extraction has grown in

importance since then because of the demand for temperature-sensitive products, higher-
purity requirements, better equipment, and availability of solvents with higher selectivity, and
is an important method in bio-separations.

Fig1 -Part of extraction column on a truck

Table 1) Major Commercial Applications of Liquid-Liquid Extraction Processes

1) Petroleum Refining

a) Separating high purity products

Toluene
Butadiene
Olefins

b) Separating one or more groups of compounds from cuts of wide

boiling range

i) Treatment of ,kerosene, Edeleanu (08)

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ii) Lubricating oils treated with selected solvents
Edeleanu (liquid SO2 )
Chlorex [bis(2-chloroethyl)ether]
Duo-Sol
Furfural
Nitrobenzene
Phenol

c) Dewaxing, deasphalting, and decarbonizing operations

2)Extraction of Acetic Acid

a) Wood distillation

b) Recovery of acetic acid from dilute solutions from cellulose

acetate etc.

3)Phenol Recovery

a) Raschig process, primary phenol production

b) Gas Works liquids, recovery and by-product phenols

c) Recovery of phenol from a wide variety of solutions

4) Chemical Processes with Liquid-Liquid Contacting

(Here the value of countercurrent operations may be questioned
because of the danger of over-reaction)

a)Nitration
b)sulphonation

5) Vitamins and Antibiotics

6) Vegetable Oil Refining

7) Fischer-Tropsch Synthesis of Liquid Fuels

a)Separation of water-soluble by-products

b)Separation of oil-soluble oxygenated by-products

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 Fig:-2 Diagram of mixture settler

1.2 DEFINITIONS

The feed to a liquid-liquid extraction process is the solution that contains the components to
be separated. The major liquid component in the feed can be referred to as the feed solvent.
Minor components in solution are often referred to as solutes. The extraction solvent, or
solvent, is the immiscible liquid added to a process for the purpose of extracting a solute or
solutes from the feed.
The extraction solvent phase leaving a liquid-liquid contactor is called the extract.
The raffinate is the liquid phase left from the feed after being contacted by the second phase.
A wash solvent is a liquid added to a liquid-liquid fractionation process to wash or enrich the
purity of a solute in the extract phase.

A theoretical or equilibrium stage is a device or combination of devices that accomplishes

the effect of intimately mixing two immiscible liquids until equilibrium concentrations are
reached, then physically separating the two phases into clear layers.
Crosscurrent extraction (Fig. 15-4) is a cascade, or series of stages, in which the raffinate R
from one extraction stage is contacted with additional fresh solvent S in a subsequent stage.

Countercurrent extraction is an extraction scheme in which the extraction solvent enters

the stage or end of the extraction farthest from where the feed F enters and the two phases
pass countercurrently to each other. The objective is to transfer one or more components from
the feed solution F into the extract E.

When a staged contactor is used, the two phases are mixed with droplets of one phase
suspended in the other, but the phases are separated before leaving each stage.

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When a differential contactor is used, one of the phases can remain dispersed as droplets
throughout the contactor as the phases pass countercurrently to each other. The dispersed
phase is then allowed to coalesce at the end of the device before being discharged.

Liquid-liquid fractionation, or fractional extraction is a sophisticated scheme for nearly

complete separation of one solute from a second solute by liquid-liquid extraction. Two
immiscible liquids travel countercurrently through a contactor, with the solutes being fed near
the center of the contactor.
The ratio of immiscible liquid flow rates is operated so that one of the phases preferentially
moves the first solute to one end of the contactor and the other phase moves the second solute
to the opposite end of the contactor.
Another way to describe the operation is that a primary solvent S preferentially extracts, or
strips, the first solute from the feed F and a wash solvent W scrubs the extract free from the
unwanted second solute. The second solute leaves the contactor in the raffinate stream.

Dissociation extraction is the process of using chemical reaction to force a solute to transfer
from one liquid phase to another.One example is the use of a sodium hydroxide solution to
extract phenolics,acids, or mercaptans from a hydrocarbon stream. The opposite transfer can
be forced by adding an acid to a sodium phenate stream to spring the phenolic back to a free
phenol that can be extracted into an organic solvent. Similarly, primary, secondary, and
tertiary amines can be protonated with a strong acid to transfer the amine into a water
solution, for example, as an amine hydrochloride salt. Conversely, a strong base can be added
to convert the amine salt back to free base, which can be extracted into a solvent.

This procedure is quite common in pharmaceutical production.

Fractionation dissociation extraction involves both the chemical reaction and the
fractionation scheme for the separation of components by their difference in dissociation
constants.

Fig.3 types of flow in extraction

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In general, extraction is preferred over distillation for:

1. Dissolved or complexed inorganic substances in organic or aqueous solutions.

2. Removal of a contaminant present in small concentrations, such as a color former in
tallow or hormones in animal oil.
3. A high-boiling component present in relatively small quantities in an aqueous waste
stream, as in the recovery of acetic acid from cellulose acetate.
4. Recovery of heat-sensitive materials, where extraction may be less expensive than vacuum
distillation.
5. Separation of mixtures according to chemical type rather than relative volatility.
6. Separation of close-melting or close-boiling liquids, where solubility differences can be
exploited.
7. Separation of mixtures that form azeotropes.

1.3 PROPERTIES OF IDEAL SOLVENT

The ideal solvent has:

1. High selectivity for the solute relative to the carrier to minimize the need to recover carrier
from the solvent.
2. High capacity for dissolving the solute to minimize solvent-to-feed ratio.
3. Minimal solubility in the carrier.
4. A volatility sufficiently different from the solute that recovery of the solvent can be
achieved by distillation. but not so high that a high extractor pressure is needed, or so low
that a high temperature is needed if the solvent is recovered by distillation.
5. Stability to maximize the solvent life and minimize the solvent makeup requirement
6. Inertness to permit use of common materials of construction
7. Low viscosity to promote phase separation, minimize pressure drop, and provide a high-
solute mass-transfer rate.
8. Nontoxic and nonflammable characteristics to facilitate its safe use
9. Availability at a relatively low cost
10. Moderate interfacial tension to balance the ease of dispersion and the promotion of phase
separation
11. Large difference in density relative to the carrier to achieve a high capacity in the
extractor
12. Compatibility with the solute and carrier to avoid contamination
13. Lack of tendency to form a stable rag or scum layer at the phase interface
14. Desirable wetting characteristics with respect to extractor internals.

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Fig.4-Knitmesh Coalescer

Fig.5-Horizontal gravity settling vessel

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Fig.6-Spray Columns For Extraction

Fig.7-Tray Columns For Extraction

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Fig.8-Tray Columns With Mechanical Agitation

1.4 CONTINUOUS (DIFFERENTIAL) CONTACT EQUIPMENT

General Characteristics Countercurrent flow is maintained by virtue of the difference in

densities of the liquids and either the force of gravity (vertical towers) or centrifugal force
(centrifugal extractors).Only one of the liquids may be pumped through the equipment at any
desired velocity. The maximum velocity for the second is then fixed; if it is attempted to
exceed this limit, the second liquid will be rejected and the extractor will be flooded.

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Equipment Classification Equipment can be broadly classified into the following
categories, generally in order of increasing complexity of internal construction.
Those most generally used are:
I. Gravity-operated extractors

A. No mechanical agitation
1. Spray towers
2. Packed towers
3. Perforated-plate (sieve-plate) towers

B. Mechanically agitated extractors

1. Towers with rotating stirrers
2. Pulsed towers
a. Liquid contents pulsed
b. Reciprocating plates

II. Centrifugal extractors

Fig.9-Podbielniak centrifugal extractor. (Courtesy of Baker Perkins Inc.)

This report basically deals with the phenomenon of liquid liquid extraction in a packed bed
column.

1.5 AXIAL DISPERSION

Because axial concentration gradients in the direction of bulk flow are established in each
phase in column extractors, diffusion of a species is superimposed on its bulk flow in that
phase. Axial diffusion degrades efficiency of the separation equipment, and in the limit, a
multistage separator behaves like a single equilibrium stage.

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Fig.10-Effect of axial mixing on concentration profiles in towers subjected to axial mixing

Two effects of axial diffusion are seen:

(1) Concentration curves in the presence of axial diffusion are closer than they are for
plug flow and
(2) These close proximities are due partially to concentrations at the two ends, which are
different from those in the original feed and solvent. These differences are jumps due to axial
diffusion outside the region in the contactor where the liquid phases are in contact.

The effects referred to as axial dispersion, axial mixing, longitudinal dispersion,or

backmixing is due to factors such as:
(1) Molecular and turbulent diffusion of the continuous phase along concentration
gradients;
(2) Circulatory motion of the continuous phase due to the droplets of the dispersed phase;
(3) Transport and shedding of the continuous phase in the wakes attached to the rear of
dispersed droplets;
(4) Circulation of continuous and dispersed phases in mechanically agitated columns; and
(5) Channeling and nonuniform velocity profiles leading to distributions of residence times in
the two phases.

1.6 LIQUID LIQUID EXTRACTION IN A PACKED BED COLUMN

Axial dispersion in a spray column can be reduced, but not eliminated, by packing the
column. This also improves mass transfer by breaking up large drops to increase interfacial
area, and promoting mixing in drops by distorting droplet shape. With the exception of
Raschig rings , the packings used in distillation and absorption are suitable for liquid–liquid
extraction, but choice of packing material is more critical.

Because of backmixing, the HETP is generally larger than for staged devices; hence packed
columns are suitable only when few stages are needed.For a packed-tower liquid-liquid
extractor the empty shell of a spray tower is filled with packing to reduce the vertical
circulation of the continuous phase.

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 The standard commercial packings used in vapor-liquid systems are also used in liquid-
liquid systems. This includes Raschig and pall rings, Berl and Intalox saddles, and other
random-dumped packings as well as the newer structured packings. The packing reduces the
available free space for flow but also significantly reduces the height required for mass
transfer.

However, Nemunaitis , Eckert, Foote, and Rollinson [Chem. Eng.Prog., 67(11), 60 (1971)]
reported little benefit from a packed height greater than 3.05 m (10 ft) and recommended
redistributing the dispersed phase about every 1.52 to 3.05 m (5 to 10 ft) to generate new
droplets and mass-transfer surfaces. From this perspective the packing allows a wider spacing
between sieve plates than described for a conventional sieve-plate tower.

The pieces of random-dumped packing should be no larger than one-eighth of the tower
diameter to minimize the wall effect which gives larger voids at the wall. The packing
support can be an open grid or multiarch support if the dispersed phase is distributed to the
top of the bed. But the packing support may also be a sieve plate with multiple light-liquid
risers if the heavy phase is to be redispersed onto a lower bed. Or the packing support may be
a sieve plate with multiple heavy-phase downcomers if the light phase is to be dispersed up
into the bed. The streams of dispersed phase should be far enough apart to avoid coalescence
at the dispersion plate, and the dispersed phase should not preferentially wet the packing. If
the droplets wet the packing, they will coalesce and stream along the packing as rivulets.

Holdup It is recognized that the dispersed-phase holdup may be placed in two categories: a
smaller portion which is permanent and a larger portion, free, which moves through the
packing and enters into mass-transfer operations when a solute is transferred between phases.
Vignes [Chem. Ind. Genie Chim., 95, 307 (1966)] further classifies the moving holdup into
“free” and “semifree.” The total is Ød, which here refers to the volume of dispersed phase
expressed as a fraction of the void space in the packed section.

The critical size of packing, usually 1.27 cm (1/2 in) or more, is given by
dFC = 2.42(ΔgC /Δρg)0.5

For packing larger than dFC, the characteristic drop diameter, for liquids that are in
concentration equilibrium, is given by
dp = 0.92(σgc /Δρg)0.5 (VkεØd /Vd)

The interfacial area is given by

a = 6εØd /dp
It is generally desirable to design for Ød in the range 0.15 to 0.25 (the lower value for Vd /Vc
< 0.5).

Flooding :- It is recommended that flow rates be set at no more than 50 percent of the
flooding values, less if the interfacial tension of the liquids is high.

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1.7 MASS TRANSFER IN PACKED BED

The number of variables that are known to influence the rate of extraction is exceedingly
large, and includes at least the following:

1. Size, shape, and material of packing

2. Tower diameter
3. Packing depth
4. Dispersed-phase distributor design
5. Which liquid is dispersed
6. Direction of extraction, whether from dispersed to continuous,
organic liquid to water, or the reverse
7. Dispersed-phase holdup
8. Flow rates and flow ratio of the liquids
9. Physical properties of the liquids
10. Presence or absence of surface-active agents

Although many attempts have been made to establish a method for estimating the extraction
rates, it is still most important to pilot-plant any new process. About the most that can be said
is that, for a given system, packing, and method of operation, Htd should be practically
constant for all flow rates up to transition and that Htc should vary roughly as C(Vc /Vd )n,
where C and n are constants, and to both Ht’s correction must be applied on scale-up for axial
dispersion [Treybal, Chem. Eng. Prog.,62(9), 67 (1966)].

Axial dispersion:-is given by the following formula,

1. Nonwetted carbon rings and wetted Berl saddles:

Ed 𝑉𝑐
log = 0.046 + .301
Vd df 𝑉𝑑
2. Wetted ceramic rings:

Ed 𝑉𝑐
log = 0.046 + .347
Vd df 𝑉𝑑

The measurements were made with kerosine or diisobutyl ketone dispersed in water.

Fig.11-Types Of Packing Used In Liquid Liquid Extraction

raschig rings

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 pall rings

saddles
Polypropylene (mainly aqueous systems up to 100 deg. C)
Carbon steel (non-corrosive hydrocarbon systems)
Ceramic (sulphuric acid & nitric acid absorbers)
Stainless steels (most hydrocarbon systems)
PVDF, PFA (corrosive aqueous systems up to 150 deg. C)
PVC / C-PVC (corrosive aqueous systems up to 90 deg. C)

Fig12-packed bed column

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CHAPTER 2 PROCEDURES AND CALCULATION

EXPERIMENTAL SET UP:-The set up consists of a glass column packed with raschig
rings. Rotameters are provided to measure the flowrate of solvent and solute.Two feed tanks
are given with pump for feed supply. Pressure gauge and pressure regulator are provided to
measure the pressure.two receiving tanks are given to collect extract and raffinate phase
products. All the solvents, and salts and other chemicals used in the study is of analytical
grade.

EXPERIMENTAL PROCEDURE:-
1) A mixture of toluene and benzoic acid is prepared by mixing 488 gms of benzoic acid
in 20 litre of toluene.
2) One tank was filled with this solution and other by 20 litre distilled water.
3) Wait for steady state to reach (approx 20-30 minutes).
4) Collect the known amount of sample in measuring cylinder from both the outlet and
note down the volume of sample.
5) Titrate the sample solution of dispersed phase, against N/5 sodium hydroxide in
alcohol by using phenolphthalein as an indicator.
6) Titrate the sample solution of continuous phase, against N/20 sodium hydroxide in
alcohol(burette) by using phenolphthalein as an indicator.
7) Repeat the experiment for different flow rates of feed mixture and water.

LTdCT =KT a(CT –C*T )dZ -----------1

LT(CT1-CT2)= KTa (ΔCT)LM Z -----------2
𝐿′𝑇
𝐾𝑇 𝑎 = -----------3
𝑉(∆𝐶𝑇 )𝐿𝑀

𝐿′𝑊
𝐾𝑊 𝑎 = -----------4
𝑉(∆𝐶𝑊 )𝐿𝑀
𝐿𝑊
𝐻𝑂𝑊 = -----------5
𝑎𝐾𝑊
𝐿𝑇
𝐻𝑂𝑇 = -----------6
𝑎𝐾𝑇

𝑚𝑄𝑊
𝐻𝑂𝑊 = 𝐻𝑊 + 𝐻𝑇 [ ] -----------7
𝑄𝑇

𝑄𝑇
𝐻𝑂𝑇 = 𝐻𝑇 + 𝐻𝑊 [ ] ------------8
𝑚𝑄𝑊

Plot the graph of HOW vs (m*QW/QT) on a simple graph and calculate the slope HT and
intercept Hw.

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CHAPTER 3 RESULTS AND DISCUSSIONS

PACKING
The special Sulzer extraction packing reduces the back-mixing of the continuous
phase, thus providing nearly plug flow conditions and a narrow droplet size distribution.
Both are necessary to achieve high throughput and high efficiency. To further
increase the separation performance, additional dual flow plates can be inserted
between the packing elements.

Fig13.-sulzer packing

LIQUID DISTRIBUTORS
In order to create an even flow profile at either end of the packed bed, both liquid
phases are distributed over the whole cross sectional area by suitable distributors.
The design of the dispersed phase distributor requires special attention, in
order to achieve a narrow droplet size distribution.

22
The technology of extraction process design and development has advanced materially during
the past few decades. A great deal of work has been done on
liquid-liquid equilibria, but reliable and general predictive methods are still not available;
direct experimentation is still needed for all but the relatively simple systems. Methods are
available for computing theoretical stages or transfer units, once the equilibria are in hand.
The design of the extraction devices, however, remains mostly in the proprietary art, and
practice is often dependent on the proprietors for scaleup and design information. This is a
situation that needs correcting.
It is likely that for many applications, a simple and nonproprietary extraction device such as a
crossflow sieve tray column or a packed column would suffice. To aid in the development of
reliable models for such devices, larger-scale perfbrmance data are needed. Such data for
distillation columns have been provided by Fractionation Re-' search, Inc.; a similar
undertaking for extraction would be welcome.

Finally, there appear to be many situations where extraction would be less energy intensive
than distillation. Improvement in the state of extraction technology would enable exploitation
of such situations

23
CHAPTER-4 CASE STUDIES

(1)EXTRACTION OF BIOPRODUCTS
Small biomolecules such as inhibitory metabolites like ethanol and butanol , and antibiotics
such as penicillin, erythromycin, tylosin, bacitracin, and cephalosporin, can be extracted
directly from fermentation broth into an immiscible organic fluid phase. Liquid extraction
can significantly reduce process volume, separate bioproducts from cells/debris, and facilitate
further product recovery via evaporation and/or crystallization. Loss of activity (e.g.,
denaturation) associated with solid membrane barriers or adsorptive phase and bioproduct
dilution during elution can be avoided using liquid extraction.

Penicillin is recovered from the fermentation broth by extraction with a solvent such as butyl
acetate after lowering the pH to get a favourable partition coefficient.the solvent is then
treated with a buffered phosphate solution to extract the penicillin from the solvent
and give a purified aqueous solution, from which penicillin is eventually produced by drying.

(2)SULFOLANE PROCESS
The hydrocarbon feed is introduced near middle of extractor and the heavy solvent is fed at
the top.
In the top section, nearly all the aromatics are extracted from the raffinate, but the solvent at
this point also contains a few percent paraffins and naphthenes.the boiling point
ranges overlap,so preparation of pure aromatics by distillation is not possible.
In the lower section of extractor,medium and high boiling paraffins are displaced from extract
phase by contact with a low boiling hydrocarbon.water is present in this system and forms a
low boiling azeotrope so the distillation is azeotropic distillation.
Solvent is recovered in second distillation column, which is a vaccum steam distillation
column,with reflux of organic phase to get high purity aromatics.
The final column is a multistage extraction column , where water is used to wash the solvent
from the raffinate.

24
Fig.14sulfolane process

25
REFERENCES

1) Foust, Wenzel, Clump, Maus, and Anderson, Principles of Unit Operations ,2d
ed.,Wiley, New York, 1980.
2) Schweitzer (ed.), Handbook of Separation Techniques for Chemical Engineers, 2d
ed., McGraw-Hill,New York, 1988.
3) Perry, Green, Maloney,Perry’s Chemical Engineers Handbook,7th edition,Macgraw
Hill Publishers,New York1997.Pg No.1425-1471
4) Treybal, RE ,Mass Transfer Operations,3rd edition,Macgraw Hill, New York,
1980.Pg No.491-553
5) Seader ,Henley,Roper, Separation Process Principles, 3rd edition, John Wiley And
Sons, 2011. Pg No.299-350
6) Derry, T.K., and T.I. Williams, A Short History of Technology, Oxford University
Press, New York (1961).
7) Maccabe, Smith,Hariott ,Unit Operations Of Chemical Engineering , 5th
edition,TMH,1993.Pg No.644-664
www.sulzer.com
www.hatltd.com
www.nptel.com

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