Liquid- Liquid Extraction

Introduction
The extraction is a separation operation of dissolutions by contact with a
solvent, partially miscible with some or several of the components of the dissolution.
In this operation, two liquid phases originate between which happens the material
transfer all the components, included the solvent, until the balance is reached. The
extraction process can imply the separation of any number of components, and the use
of different solvent in several stages.
The Unit Extraction Liquid-Liquid “UELL” allows studying the extraction of
one or several components in a continuous way with a solvent in a theoretical stage.
The contact takes place inside a packed column, in which the two phases circulate in
countercurrent. The circulation velocity of both phases can be controlled in an
independent way. The equipment allows the recovery of the solvent, by a rectification
process.
Principles of Liquid-Liquid Extraction
The task of separation is to transfer one or more components from one liquid phase to
the other to a desired extent. The components to be removed or separated are called
solute. The former liquid is called diluent and the latter is solvent. The two liquid
phases are immiscible or partially miscible most of the time. At a condition where the
solubility of a solute, A, in both phases, yA and xA, will be in equilibrium, the ratio of
yA to xA, represented by Kd, is called distribution ratio.
The extraction can be regarded as one or more contacting stages. To simplify
the extraction calculation, these stages are assumed as equilibrium ones, as shown in
Fig.
Objective
1- Demonstrate how a mass balance performed on the extraction column.
2- Measure the mass transfer coefficient and its variation with flow rate with the
aqueous phase as the continuous medium.
3- Determination of Efficiency of Extraction
4- Investigate the Effect of Feed and Solvent Flow Rates on Extraction
Description of apparatus
The Unit of Extraction Liquid-liquid “UELL” is an equipment at laboratory
scale, designed to study the separation of liquid mixtures by contact with a solvent.
The equipment consists of the following parts:
a. The extraction unit is composed of a jacketed glass, packed column of 1200 mm
of longitude and 50 mm of internal diameter, with two enlargement pieces with 2
liters of capacity in the ends. The packing is glass Raschig rings with 3 mm.
b. The rectification unit consists in a glass packed column of 500 mm of longitude
and 25 mm of internal diameter. The packing of the column is glass Raschig rings
with 3 mm. It has a 5 liters boiler and two thermocouples, one in the boiler and
another one in the distillation head.
c. Supply circuits and collection of products connect the different units with the
storage tanks. It has samples takings to control the process in all the lines of fluid.
d. The dosing pumps are alternative pumps of positive displacement and regulating
flow. With each run of the pusher the pressure will increase in a gradual way in
the discharge pipe, being able to end up reaching a maximum pressure of 30.0
bars. A regulation system (point B of the figure) allows varying the adjustment of
the pump, rotating the regulation cap when the pump run or stop. If the turn is
carried out in a clockwise direction, the flow will increase while in clockwise
direction it will diminish.
The control elements include a regulating valve of the height of the inter-phases, a
temperature controller for the boiler, a temperature indicator for the distillation head,
a heating blanket power regulator, two dosing pumps and two rotameters for
measuring the flow.
Specifications:
The UELL unit is provided complete, and it only requires the additional assembly of
the glass parts. It has the necessary elements to connect it to the required services.
The unit is manufactured in stainless steel, anodic aluminum and glass, to allow the
visual observation of the process.
a. Jacketed glass packed column of 1200 mm of longitude and 50 mm of internal
diameter, packed with 3 mm glass Raschig rings. In this column the extraction
process is carried out.
b. Jacketed glass packed column of 500 mm of longitude and 25 mm of internal
diameter, packed with 3 mm glass Raschig rings. This column is used to the
distillation process.
c. Boiler with 5 l of capacity for the distillation, heated by an adjustable electric
blanket, with automatic control of the temperature.]\
d. Five glass tank with 10 l of capacity.
e. A dosing pump with stainless steel head, provides a maximum flow of 50 l/h
and a maximum pressure of 10 bar.
f. A dosing pump with stainless steel head, provides a maximum flow of 17 l/h
and a maximum pressure of 12.5 bar. This pump has a high chemical resistance.
g. Two rotameters to measure of supply and refined flow.
h. Two thermocouples J type, to measure the temperature in the column head and
control the boiler temperature.
i. A digital regulator-indicator of the temperature that receives the sign of the
thermocouple located in the boiler, and controls the temperature of the heating
blanket.
j. Seven samples takings distributed between all the circuits of the equipment.
k. Security Devices in the pumps, to avoid shortcomings by overpressure, pressure
switch that switch off the pump when the pressure is high.
l. Practices manual in English, with a detailed guide of their performance.
Supply circuits and collection of products.
Supply's circuits can be seen in the outline that is attached. In both circuits they have
been placed samples taking to follow the process and a series of valves to regulate the
flow or to configure a certain circuit.
The legend of the valves indicates:
VC - = two ways valve
VT - = three-ways valve
VR - = regulation valve
V - = needle valve
The sample selection is carried out for a valve of three roads, as it indicates the
outline.
CAUTION: The three ways valves, of stainless steel have three positions, the
flow goes in the direction of the arrows, being the intermediate position to close.
It should been careful with the position of the three ways valves so that they are in the
correct position once it takes the sample or the process is changed. (See the circuit
diagram with the position of the valves).
Warning: before connecting anyone of the pumps, verify the position of the
valves.
All the valves have been prepared in the orifices of the front panel, so they can be
manipulated easily. The valves and their function in the system are detailed on:
VT-1: (three-ways valve) associated to the pump1 calibration and taking of
sample (position M.C.). It allows opening or closing the supply circuit, (see enclosed
figure).
VT-2: (three-ways valve). It allows opening or closing the extract circuit, as well as
to make sample takings.
VR-1: Regulated Valve. This valve allows controlling the interface level in the
column.
VT-6: (three-ways valve). This valve supplements to the previous one. In open
position, the control of the extract circuit passes to the valve VR-1 and VT-2
explained previously. This also allows the extraction column derange.
V-1: (two-ways valve). As opening, allows passing the extract to the boiler of the
rectificated unit.
VC -: These valves are used to drain the tanks of the unit.
VT-3: (three-ways valve). It allows discharging the boiler to the solute tank. Their
third position allows us the sample taking and the quick derange of the boiler.
VT-5: (three-ways valve). This valve is used to extract sample of the distilled
product (solvent), as well as to open or close the distillated circuit that it goes toward
the solvent tank.
VT-4: Three-way valve. It opens up or closes the refined circuit.
VT-7: (three-ways valve). This valve allows opening or closing the solvent circuit.
The third position allows extracting a solvent sample.
There are too, other 4 three way valves place in the back side of the unit (VT-8, VT-
9, VT-10 and VT-11).This valves let us to change the configuration of the unit
depending of the reactive used. It let us use different solvents types with different
densities. The valves VT-8 and VT-9 let us to introduce the feed into the column from
the bottom of column or from the top. The valves VT-10 and VT-11 let us interchange
the raffinated and extract tank.
Procedure
a) Add 100 ml of Acetic acid to 10 liters of water. Mix well to ensure an even
concentration then fill the organic phase feed tank (bottom tank) with the mixture.
b) Switch the level control to the bottom of the column by keeping the bottom
electrodes on.
c) (switch S2 valve on)
d) Fill the trichloromethane solvent tank with 15 liters of clean trichloromethane,
start the solvent feed pump and fill the column with trichloromethane at high flow
rate.
e) As soon as the trichloromethane is above the top of the packing, reduce the flow
rate to 0.2 lt/min.
f) Start the metering pump and set at a flow rate of 0.2 lt/min.
g) Run for 15-20 minutes until steady conditions are achieved, monitor flow rates
during this period to ensure that they remain constant.
h) Take two or three batches of 15 ml samples from the feed, raffinate and extract
streams.
i) Titrate 5 ml of each sample of the extract and raffinate and feed tanks against 0.1 M
NaOH using phenolphthalein as the indicator.
i. Take the initial NaOH volume.
ii. Drop a few droplet of phenolphthalein into the sample in Erlenmeyer flask.
iii. Titrate the solution with NaOH until the sample turn to pink colour.
iv. Record the NaOH volume after titration.
j) To titrate the feed and raffinate continuous stirring using a magnetic stirrer may be
needed).
k) Repeat the experiment with water flow rate being increased to 0.3 lit/min.
Note: Calibration of pump is needed whenever a change in flow rates is necessary.
The procedure for calibration is as follows:
The solvent metering pump is calibrated in percentage of maximum flow which varies
slightly from pump to pump.
The pump should be calibrated initially by setting F2 to 100%, setting valve V8 to the
calibrated position and measuring the flow from the pump, using a measuring cylinder
and stopwatch. Calculate the flow rate produced settings of 10% intervals (ml/min),
then plot a graph of ml/min against percentage of metering pump stroke.
Thereafter any selected flow may be obtained by using the graph.
Calculations
1- The theory for the system Trichloroethylene-Propionic acid-Water is as follows:
Let
Vw : Water flow rate, lit/s
Vo : Trichloroethylene flow rate, lit/s
X : Propionic acid concentration in the organic phase, kg/lit
 Y : Propionic acid concentration in the aqueous phase, kg/lit
Subscripts :
1: Top of column
2: Bottom of column
Mass Balance:
Acetic acid extracted from the aqueous phase (rafinate (

Vo X X2  

Acetic acid extracted by the organic phase (extract)

= Vw Y1-0

Therefore theoretically,

 Vo X1 – X2 Vw Y1 - 0 

Mass transfer coefficient:

MTC

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 aqueous phase which would be in
equilibrium with concentrations Y1 and Y2 ( = 0.0) in the organic 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
Eqs.(1) or (2) based on raffinate or extract phases, respectively.
2- Separation efficiency:
 Tables and results:
Flow rate of aqueous phases
Flow rate of organic phase
Titration of M/10 Concentration of propionic
NaOH acid kg/l
Feed
Raffinate
Extract
Propionic acid extracted
from the organic phase
Propionic acid extracted
from the aqueous phase
Mass Transfer Coefficient
Report
i. Find Acetic acid concentrations in each stream.
ii. Calculate the mass transfer coefficients based on both phases.
iii. Calculate the column efficiency using experimental and what should be done to
achieve the maximum acid transfer rate?
iv. Discuss the effects of feed and solvent flow rates on the efficiency of extraction
based on your experiment.