ABSTRACT

In liquid-liquid extraction experiment, it consists of two parts. Firstly, to determine

the distribution coefficient for the system organic solvent-Propionic acid-water and to show it
dependence on concentration and the 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. In the first part, mixture of organic solvent with
de-mineralised water that mixture has been separated to the organic and aqueous layer. Then
10 mL of the organic and aqueous layer has been titrated with 0.1 M of NaOH. When 5 mL of
propionic acid added to the mixture of organic solvent with de-mineralised water and titrated
with 0.1 M of NaOH, the amount of NaOH used is 30.1 mL for organic layer and 44.1 mL for
aqueous layer. When 3mL of propionic acid is added to the mixture and titrated with 0.1 M
NaOH, 16.9 mL of NaOH is used for organic layer while 18.4 mL of NaOH is used for
aqueous layer. Lastly, when 1mL mL of propionic acid added to the mixture and the solution
has been titrated with 0.1 M of NaOH, the amount of NaOH used is 1.2 mL for organic layer
and 9.7 mL for aqueous layer. In experiment B, 50 mL sample from feed (V13), raffinate
(V11) and extract (V1) stream are taken. Then 10mL of feed, raffinate and extract has been
titrated with 0.1 M and 0.025 M NaOH, the amount of 0.1 M NaOH that used is 17 mL and
0.025 M NaOH is 54.1 mL for feed, 0.1 M NaOH used is 1.0 mL and 0.025 M NaOH used is
1.5 mL for raffinate. Meanwhile the amount of 0.1 M NaOH used is 6.0 mL and the amount
for 0.025 M NaOH used is 23.2 mL for extract. The experiment is conducted and completed
successfully.

INTRODUCTION
Liquid-liquid extraction (LLE) is widely used in chemical, petroleum refinery,
pharmaceutical, mining, and the nuclear industries to separate chemicals in liquid mixtures 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 is the preparation of the pure organic liquids from products of the oil
industry. 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.
There are a few characteristics that are required in choosing the solvent for LLE
process. First, solvent would preferably completely dissolve both compounds in the mixture.
Second, the solvent selected must be immiscible with the first solvent. Third, second solvent
should preferentially dissolve only one component of the original mixture.
In liquid-liquid extraction, mixture is dissolved or suspended in the first solvent and
then this solution is introduced to the second solvent. By shaking the solvent together in an
apparatus called a separator funnel, one component of the mixture will be transferred into the
second solvent. This would leave the other component in the first solvent. Final separation of
two solvents is accomplished using separator funnel, followed by evaporation of solvents,
produces the separated components.
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 batchwise 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.

If the components of the original solution distribute differently between the two
liquids, separation will result. The component balances will be essentially identical to those
for leaching, but there are two major differences which are the carrier phase is a liquid, not a
solid, so the physical separation technique will change and two distinct phases develop, so the
simplicity of uniform solution is lost.
Propionic acid is an important commercial product and extracting it out of aqueous
solution is a growing requirement in fermentation based industries and recovery from waste
streams.

OBJECTIVES
In experiment Part A, the objectives are to determine the distribution coefficient for
the system organic solvent propionic acid water as well as to its dependence on
concentration. Meanwhile, the objectives of experiment Part B are 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.

THEORY
In dilute solution at equilibrium, the concentrations of the solute in the two phases are called
the distribution coefficient or distribution constant K, as describe in the followings:
K = Y/X ..............(1)
where Y is the concentration of the solute in the extract phase whereas X is the concentration
of the solute in raffinate phase. The distribution coefficient can also be expressed as the
weight fraction of the solute in the two phases in equilibrium contact:

K = y/x ................(2)
where y is the weight fraction of the solute in the extract and x is the weight fraction of the
solute in the raffinate.
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.
The theory for the system Trichloroethylene-Propionic acid-Water is as follows:
Let
Vw

: Water flow rate, lt/s

Vo

: Trichloroethylene flow rate, lt/s

: Propionic acid concentration in the organic phase, kg/lt

: Propionic acid concentration in the aqueous phase, kg/lt

Subscripts

: 1 : Top of column
: 2 : Bottom of column

Mass Balance :
Propionic acid extracted from the organic phase (raffinate).
=Vo(X1X2) .................(3)
Propionic acid extracted by the aqueous phase (extract)
=Vw(Y10) ..................(4)
Therefore theoretically,
Vo(X1X2) = Vw(Y10) ...................(5)

Mass transfer coefficient:

( Rate of acid transfer ) /(Volume of packing Meandriving force )

......................(6)
MTC =

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

X1 : Driving force at the top of the column = (X2 - 0)
X2 : Driving force at the bottom of the column = (X1-X1*)
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
(Assume that Y=KX relation holds at equilibrium for a constant K). Rate of acid transfer may
be calculated using Equation (3) or (4) based on raffinate or extract phases, respectively.