Separatio

n Process
Lab
Report
Liquid-Liquid
Extraction Unit
Submitted By:
M. Ahmad Ikram
(2010-CH-241)

LiquidLiquid
Extraction
Unit

THEORY:
INTRODUCTION:
Liquid/liquid extraction, also known as solvent extraction and partitioning, is a method to
separate compounds based on their relative solubility in two different immiscible liquids, usually water
and an organic solvent (propionic acid). It is an extraction of a substance from one
liquid phase into another liquid phase. Liquid-liquid extraction is a basic technique in chemical
laboratories, where it is performed using a separator funnel. This type of process is commonly performed
after a chemical reaction as part of the work-up.
In other words, this is the separation of a substance from a mixture by preferentially dissolving that
substance in a suitable solvent. By this process a soluble compound is usually separated from an insoluble
compound.

BASIC PRINCIPLE:
The basic principle behind extraction involves the contacting of a solution with
another solvent that is immiscible with the original. The solvent is also soluble with
a specific solute contained in the solution. Two phases are formed after the addition
of the solvent, due to the differences in densities. The solvent is chosen so that the
solute in the solution has more affinity toward the added solvent. Therefore, mass
transfer of the solute from the solution to the solvent occurs. Further separation of
the extracted solute and the solvent will be necessary. However, these separation
costs may be desirable in contrast to distillation and other separation processes for
situations where extraction is applicable.
Many processes in chemical engineering require the separation of one or more of
the components of a liquid mixture by treating the mixture with an immiscible
solvent in which these components are preferentially soluble. In some cases
purification of a liquid may be the function of the process, in others the extraction of
a dissolved component for subsequent processes may be the important aspect. An

example of the former is the preparation of the pure organic liquids from products of
the oil industry.

WHEN USE EXTRACTION/DISTILLATION?

Liquid-liquid extractions may also be used as energy saving processes by, for
example, eliminating distillation stages. It is possible, of course that the substance
of interest may be heat-sensitive anyway and that distillation is accordingly an
unacceptable process.
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
cannot withstand the temperature of the distillation, even under a vacuum, may
often be separated from impurities by extraction, which utilizes chemical differences
instead of vapor pressure differences. For example, penicillin is recovered from
fermentation broth by extraction with a solvent such as butyl acetate. Another
example for liquid extraction is recovering acetic acid from dilute aqueous solutions;
distillation would be possible in this case, but the extraction step considerably
reduces the amount of water to be distilled.

DISTILLATION OR EXTRACTION?

When either distillation or extraction may be used, the choice is usually

distillation, in spite of the fact that heating and cooling are needed. In extraction the
solvent must be recovered for reuse (usually by distillation), and the combined
operation is more complicated and often more expensive than ordinary distillation
without extraction. However, extraction does offer more flexibility in choice of
operating conditions, since the type and the amount of solvent can be varied as well
as the operating temperature. In many problems, the choice between the methods
should be based on a comparative study of both extraction and distillation.
In liquid-liquid extraction, as in gas absorption and distillation, two phases
must be brought into contact to permit transfer of material and then be separated.
Extraction equipment may be operated batch-wise or continuous. The extract is the
layer of solvent plus extracted solute and the raffinate is the layer from which solute
has been removed. The extract may be lighter or heavier than the raffinate, and so
the extract may be shown coming from top of the equipment in some cases and
from the bottom in others. The operation may of course be repeated if more than
one contact is required, but when the quantities involved are large and several
contacts are needed, continuous flow becomes economical.
The rate at which a soluble component is transferred from one solvent to
another will be dependent, among other things, on the area of the interface
between the two immiscible liquids.
Therefore it is very advantageous for this interface to be formed by droplets and
films, the situation being analogous to that existing in packed distillation columns.

GENERAL DESCRIPTION OF THE EQUIPMENT:

A general extraction column has two input stream and two output streams. The
input streams consist of a solution feed at the top containing the solute to be
extracted and a solvent feed at the bottom which extracts the solute from the
solution. The solvent containing the extracted solute leaves the top of the column
and is referred to as the extract stream. The solution exits the bottom of the column
containing only small amounts of solute and is known as the raffinate. Further

separation of the
separation processes.

output

streams

may

be

required

through

other

DESCRIPTION OF APPARATUS:

The apparatus consist of:

Floor-standing and welded steel framework fitted with adjustable feet.
The stainless steel glass liquid/liquid extraction columns.
Water for the column is stored in the supply tank from where it is pumped by
the centrifugal pump.
Polythene tank to collect the water leaves the top of the column.
The organic solvent supply tank provides the feed for the solvent metering
pump.
The level of the water/solvent interface in the column is determined by the
operation of the solenoid valve.

EXPERIMENTS DONE ON IT:

DETERMINATION OF DISTRIBUTION COEFFICIENT:
The objective of this experiment is to determine the distribution coefficient for the
system organic solvent-Propionic Acid-Water and to show its dependence on
concentration. The solvent (water) and solution (organic solvent/propionic acid) are
mixed together and then allowed to separate into the extract phase and the
raffinate phase. The extract phase will be water and propionic acid and the
raffinate, organic solvent with a trace of propionic acid. The distribution coefficient,
K, is defined as the ratio. It is assumed that equilibrium exists between the two
phases. At low concentrations, the distribution coefficient is dependent on the
concentration and thus Y = KX.

BASIC OPERATION OF THE LIQUID/LIQUID EXTRACTION COLUMN:

The objective of this experiment is to observe the hydraulics of counter current flow
in a packed column. The experiment will be carried out using the two immiscible
liquids organic solvent and water and the column will be operated in the two modes:

(a) The aqueous phase as the continuous medium.

(b) The organic phase as the continuous medium.
Overall Mass Balance and Mass Transfer Coefficients with the
Aqueous Phase as the Continuous Medium:
The objective of this experiment is to demonstrate how a mass balance is
performed on the extraction column, and to measure the mass transfer coefficient
with the aqueous phase as the continuous medium.

Overall Mass Balance and Mass Transfer with the Organic Phase as
the Continuous Medium:
The objective of this experiment is to demonstrate how a mass balance is
performed on the extraction column, and to measure the mass transfer coefficient
with the organic phase as the continuous medium.

Summary:
Liquid-liquid extraction experiment consists basically of two parts.

First is to determine the distribution coefficient for the system organic

solvent-Propionic acid-water and to show it dependence on concentration.

Second is to demonstrate how a mass balance is performed on the extraction

column, and to measure the mass transfer coefficient with the aqueous phase
as the continuous medium.

DISTRIBUTION CO-EFFICIENT:
A quantitative measure of the how an organic compound will distribute between
aqueous and organic phases is called the distribution or partition coefficient. It is
the ratio, K, of the solubility of solute dissolved in the organic layer to the solubility
of material dissolved in the aqueous layer. (Note that K is independent of the actual
amounts of the two solvents mixed).
K= distribution coefficient
K =solubility of organic (g/100 mL)/solubility of water (g/100 mL)

MASS BALANCE:
Let Vw: Water flow rate, lt/s
Vo: Trichloroethylene flow rate, lt/s
X: Propionic acid concentration in the organic phase, kg/lt
Y: Propionic acid concentration in the aqueous phase, kg/lt
Subscripts:
1: Top of column
2: Bottom of column
Propionic acid extracted from the organic phase (rafinate)

Propionic acid extracted by the aqueous phase (extract)

Therefore theoretically,

Mass transfer coefficient:

where Log mean driving force : (X1-X2) / ln (X1/X2)

X1: Driving force at the top of the column = (X1-X1*)
X2 : Driving force at the bottom of the column = (X2-X2*) = X2
Where, X1* and X2* are the concentrations in the organic phase which would be in
equilibrium with concentrations Y1 and Y2 ( = 0.0) in the aqueous phase,
respectively. The equilibrium values can be found using the distribution coefficient
for the chemicals used (Assumed that Y=KX relation holds at equilibrium for a
constant K).

EXPERIMENTAL PROCEDURE:

Add 100 ml of propionic acid to 10 liters of trichloroethylene. Mix well to

ensure an even concentration then fill the organic phase feed tank (bottom
tank) with the mixture.

Switch the level control to the bottom of the column by keeping the bottom
electrodes on (switch S2 valve on)

Fill the water feed tank with 15 liters of clean demineralised water, start the
water feed pump and fill the column with water at high flow rate.

As soon as the water is above the top of the packing, reduce the flow rate to
0.2 lt/min.

Start the metering pump and set at a flow rate of 0.2 lt/min.

Run for 15-20 minutes until steady conditions are achieved, monitor flow
rates during this period to ensure that they remain constant.

Take two or three batches of 15 ml samples from the feed, raffinate and
extract streams.

Titrate 10 ml of each sample against 0.1 M NaOH using phenolphthalein as

the indicator. (To titrate the feed and raffinate continuous stirring using a
magnetic stirrer may be needed).

Repeat the experiment with water flow rate being increased to 0.3 lt/min.