Exp-9 - Liquid Liquid Extraction in A Packed Column

Experiment No.
‐9(b)

LIQUID –LIQUID EXTRACTION IN A PACKED EXTRACTION COLUMN

Introduction:

The packed columns fall in the class of gravity operated, unagitated extractors. They are
advantageous over spray columns since they provide extra contact surface and prevent
backmixing. Possible channeling effects are reduced by using redistributors.

Aim:

To determine the total height of a transfer unit, HOR (based on raffinate), HOE (based on
extract), the volumetric mass transfer coefficient KOR.a and KOE.a in the packed tower.

Theory:

Liquid–liquid extraction, also known as solvent extraction and partitioning, is a method
to separate compounds based on their relative solubilities in two
different immiscible liquids, usually water and an organic solvent. It is an extraction of a
substance from one liquid phase into another liquid phase. In liquid‐liquid extraction, a
distribution ratio is often used as a measure of how well‐extracted a species is. The
distribution ratio (D) is equal to the concentration of a solute in the aqueous phase
divided by its concentration in the organic phase, where water act as solvent. Depending
on the system, the distribution ratio can be a function of temperature and the
concentration of chemical species in the system.

In the present experiments, water acts as solvent. It extracts the solute (acetic
acid/acetone) from the organic solution. Consider an elemental height dz of the column of
cross sectional area S. Let Fr be the mass velocity of toluene (solute free basis) and Fe the
mass velocity of water (solute free basis).

Contd‐‐‐‐P/2
Mass Transfer Lab IIT Kgp
‘2’
.
The amount of solute (acetic acid/acetone) transferred can be written as
Fr.S.dx = Kor,a .(X-X*) . S .dz ……….. (1)

Fe.S.dy = Koe,a .(Y-Y*) . S . dz………...(2)
Where Kor,a and Koe,a are the respective volumetric mass transfer coefficients of the
raffinate and the extract phase.
X is composition of raffinate i.e. Mass of solute/ Mass of toluene
Y is composition of extract i.e. Mass of solute/Mass of water.
X* and Y* are the equilibrium compositions of raffinate and extract respectively. The
number of transfer units for raffinate and extract Nor & Noe may be calculated from the
following equations
Nor = …………..(3)
Noe = …………..(4)
‘3’
Where Xr and Xf are compositions of raffinate and feed i.e. mass of solute / mass of
toluene And Ye and Yo are compositions of extract and feed i.e mass of solute/ mass of
water.
Experimental setup:
Figure 1. Extraction Column
The equipment consists of a metal column of 50 mm ID provided with Raschig rings

packing of 6 mm size. The packing is adjusted in two sections with a liquid redistributor
in the middle. The column is also provided with liquid redistributors at the top and
bottom. Overhead and collection tanks are provided for aqueous and organic phase with
arrangements to measure their flow rates using rotameters. The composition of various
streams is measured by titration or refractometry depending on the system selected. In
this case the dispersed phase flow is downwards and the continuous phase flow is upwards.
The dispersed phase is water and the continuous phase is a mixture of toluene and acetic
acid/acetone. So the extract is collected through the bottom and the raffinate from the top.
‘4’
Experimental Procedure:
The column is filled with a given organic mixture of specified composition. The
recommended concentration of solute in feed is 1 to 2 kmol/m3.
The rotameter readings are adjusted for both the phases. The recommended range of
velocities for dispersed and continuous phase are 0.01 to 0.04 m/s and 0.005 to
0.02m/s. respectively.
The lower interface is adjusted to a suitable height with the help of a stopcock at the
raffinate collection point.
The first observation is taken after two times the mean residence time of the dispersed
or continuous phase (depending on which is larger). The flow rate of extract, raffinate and
density of extract, raffinate and feed are determined.
The extract and raffinate samples are collected and analyzed for solute concentration.
The above procedure is repeated for different flow rates.
Data Analysis:
Calculate the total number of transfer units based on raffinate and extract from eqns (3) and
(4 ) respectively. Calculate height of transfer unit and the overall height. Tabulate all
calculated data of HOR (based on raffinate), HOE (based on extract), KOR.a and KOE.a
for different run of experiment.

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Experiment No.

Fr.S.dx = Kor,a .(X-X*) . S .dz ……….. (1)

Y is composition of extract i.e. Mass of solute/Mass of water.

Figure 1. Extraction Column

The equipment consists of a metal column of 50 mm ID provided with Raschig rings

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