MIXERSETTLER TYPE EXTRACTOR

OBJECTIVE:
To study the extraction of benzoic acid from toluene (dispersed phase) by water(continuous phase) in a
packed bed.
AIM:
To determine overall mass transfer coefficient based on continuous phase (water),K wa.
To determine overall mass transfer coefficient based on dispersed phase (toluene),K ta.
To determine overall Height of Transfer Unit based on continuous phase (water),HTU ow & based on
dispersed phase (toluene), HTUot
To determine Individual Height of Transfer Unit based on continuous phase (water), HTU w and dispersed
phase (toluene), HTUt
INTRODUCTION:
Liquid extraction, sometimes called solvent extraction, is the separation of the constituents of a liquid solution by
contact with another insoluble liquid. If the substances constituting the original solution distribute themselves
differently between the two liquid phases, a certain degree of separation will results, and this can be enhanced by use
of multiple contacts or their equivalent in the manner of gas absorption and distillation.
THEORY:
Towers filled with some random packing (say rasching rings) are widely used for extraction of valuable chemicals
from dilute solutions by liquid-liquid extraction. The packing provides a larger extract area for mass transfer and also
reduces the axial mixing to some extent.
The extraction rate in such columns depends on:
Choice of either continuous or dispersed phase
Packing and column variables
Velocity of the liquid phases in the tower
The tower performance is generally based on extraction rate data and evaluated in terms of overall height of transfer
unit, based on continuous phase, HTUow and the extraction factor expressed in terms of flow rate ratios of the liquid
phases, mVw/Vt These two variables are plotted against each other on Cartesian co-ordinates. As suggested by
Colburn, the slope and intercept of such a plot would represent the resistance of the individual films as:
OVER ALL HEIGHT OF TRANSFER UNIT:

mVw
1
Vt

HTU ow HTU W HTU t

Vt
mVW

HTU ot HTU t HTU w

Where, m is the slope of equilibrium curve, m = dCw/dCt

* Under certain conditions (e.g. low concentrations) m is a constant
V is the superficial velocity of the liquid phase based on empty cross section of the column, subscript w for continuous
phase (water) and t for dispersed phase (toluene).

Rate of mass transfer from dispersed phase to the continuous phase is defined as:

C w* 1 C w1 C w* 2 C w 2
N
K w aV

*
*

ln C w1 C w1 / C w 2 C w 2

C1 C 2
N
K w aV

ln C1 / C 2
The capacity coefficient based on continuous phase (water), Kwa, is thus defined as:

KW a
3
V CW ln

C w ln

C w1 C w 2
C w1
C w2

ln

Where,
Similarly, the capacity coefficient based on dispersed phase (toluene), Kta, is defined as:

Kt a
4
V C t ln
As per Chilton and Colburn, the over all height of transfer unit based on continuous phase (water), HTU ow is defined
as:

HTU ow

Vw
5
K wa

And the over all height of transfer unit based on dispersed phase (toluene), HTUot is defined as:

HTU ot

Vt
6
Kt a

DESCRIPTION:
The set up consists of two feed tank. In this system two different liquids are used in which the one is heavier (water)
which is used as solvent and the other is lighter in which the solute is present (toluene). The heavier liquid is inserted
from the top and the lighter from the bottom. The interface maintained in the column between the lighter phase and the
heavier phase at the top of the column can be adjust up or down as necessary by regulating the arrangement provided
at the water stream leaving the column. Flow rate of both the liquids is measured by the rotameters provided. The
samples are taken from the top for lighter liquid and bottom for heavier liquid.
UTILITIES REQUIRED:
1. Compressed Air Supply @ 0.5 CFM at 2 Bar,.
2. Drain required.

3. Laboratory Glassware.
4. Weighing Balance (least count + 1 gm)
5. CHEMICALS REQUIRED:
Toluene

20 L

Benzoic acid

488 gm

Distilled water

20 L

N/5 NaOH in alcohol

500 ml

N/20 NaOH in water

500 ml

Phenolphthalein as indicator = 10 ml
EXPERIMENTAL PROCEDURE:
1. Prepare a mixture of Toluene and Benzoic Acid as a feed mixture, with the concentration of Benzoic Acid
488gm in 20Ltrs (i.e. N/5).
2. Fill the column with the continuous phase (water).
3. Allow the dispersed phase (toluene + benzoic acid) to enter from the bottom of the column at some minimum
flow rate.
4. Adjust the Rotameter readings for Continuous and dispersed phase to same values.
5. The interface between the lighter phase and the heavier phase at the top of the column must be worked up or
down as necessary by adjusting the sliding arrangement provided in the water stream leaving the column. The
position of the interface is to be maintained at about 1 inch above the point of introduction of the heavier
6.
7.
8.
9.
10.

liquid (water) into the column.

Take the first observation after the steady state has been established i.e. after 10to 20 minutes.
Collect known amount of sample of Extract (water) and raffinate (Tolune).
Titrate the sample of tolune against N/5 NaOH in alcohol using phenolphthalein as indicator.
Titrate the sample of water against N/20 NaOH in water using phenolphthalein as indicator.
Repeat the experiment for different flow rate of liquids.

OBSERVATION & CALCULATION:

DATA:
Dc

0.045 m

0.75 m

NTT,NTB = ----------------(for Tolune)

NWB

= ----------------(for Water)

Equilibrium data for Benzoic Acid - Toluene Water

Cw, g mole/L
0.0000
0.0016
0.0064
0.0080
0.00961
0.011211
0.012816
0.01442
The equilibrium data can be represented by:

Ct, g mole/L
0.0000
0.0080
0.0336
0.0673
0.08811
0.12015
0.14097
0.17301

Cw
H 0.2015 1.4273C t 4.3672C t2
CT
And

C w 0.0745C t 0.0019
Or slope of the equilibrium line can be assumed to be constant at

dC w
0.0745
dC t

OBSERVATION TABLE:
S.No.

Qt, LPH

Qw, LPH

V1, ml

VTT, ml

VTB, ml

CALCULATION:
A) CONCENTRATION OF BENZOIC ACID IN TOLUENE:
1) At bottom: (feed concentration)

N1

N TB VTB
______________ gmol / L
V1

Ct1= CF = N1 g mole/L
2) Similarly At Top:

N1

N TT VTT
______________ gmol / L
V1

Ct2= N1 g mole/L

A1 C t1 C t 2 Qt ______________ gmol / h
B) CONCENTRATION OF BENZOIC ACID IN WATER:
1) At Top:
Cw2= 0

N1

N W BVW B
______________ gmol / L
V1

Cw1 = N1 g mole/L

A2 C w1 C w 2 Q w ______________ gmol / h

N A1 A2

______________ gmol / h

OVERALL MASS TRANSFER COEFFICIENT BASED ON DISPERSED PHASE:

Kt a

VWB, ml

At bottom:

Cw

Ct

H1

atCt Ct 1

using equilibrium data

C t1 C t1 C w1 / H 1 ______________ gmol / L
At Top:

Cw

Ct

H2

atCt C t 2

using equilibrium data

C t 2 C t 2 C w 2 / H 2 ______________ gmol / L

C t ln
V

C t 2 C t1
______________ gmol / L
ln C t 2 / C t1

2
DC Z ______________ ml
4

Kt a

N /
______________
V C t ln

C w1 H 1C t1 C w1 ______________ gmol / L
C w 2 H 2 C t 2 C w 2 ______________ gmol / L

C w ln
K wa

AC

C w 2 C wt 1
______________ gmol / L
ln C w2 / C w1

N /
______________
V C w ln

2
DC ______________ m 2
4

OVER ALL HEIGHT OF TRANSFER UNIT BASED ON CONTINUOUS PHASE:

Vw

Qw
______________ m / h
AC

HTU ow

Vw
______________ m
KW a

OVER ALL HEIGHT OF TRANSFER UNIT BASED ON DISPERSED PHASE:

Vt

Qt
______________ m / h
AC
Vt
______________ m
Kt a

HTU ot

Vw
Vt
Plot the graph (HTU)ow vs.

on a simple graph. Determine the slope & intercept.

HTUt = Slope of graph = --------- m

HTUw = Intercept of graph = --------- m
NOMENCLATURE:
A1 = Amount of benzoic acid extracted by water, g mol/h
A2 = Amount of benzoic acid recovered by water, g mol/h
Ac = Column cross sectional area, m2
Cw1 = Concentration of benzoic acid in water at bottom,g mol/L
Cw2 = Concentration of benzoic acid in water at top, g mol/L
Ct1 = Concentration of benzoic acid in toluene at bottom, g mol/L
Ct2 = Concentration of benzoic acid in toluene at top, g mol/L
Cw = Equilibrium solute (benzoic acid) concentration in water
phase, gmol/L
CF = Concentration of benzoic acid in feed. g mol/L
Ct =

Equilibrium solute (benzoic acid) concentration in toluene phase, gmol/L

Dc=

Column diameter, m

H=

Equilibrium distribution coefficient,H1,H2 (CW / CT)

HTUw =

Individual height of transfer unit based on continuous phase (water), m

HTUt = Individual height of transfer unit based on dispersed phase (toluene), m

HTUow=

Overall height of transfer unit based on continuous phase (water), m

HTUot= Overall height of transfer unit based on dispersed phase (toluene), m

Kw a

Overall mass transfer coefficient based on continuous phase

Kt a

Overall mass transfer coefficient based on dispersed phase

N/

Average amount of Benzoic acid recovered, g mol/h

N1

Normality of sample

NTT,NTB =

Normality of NaOH used(for Tolune).

NWB

Normality of NaOH used(for Water).

Qt

Volumetric flow rate of toluene, LPH.

Qw

Volumetric flow rate of water, LPH.

V1

Volume of sample, ml

VTT

Volume of NaOH used in titration of top sample for Tolune, ml

VTB

Volume of NaOH used in titration of bottom sample for Tolune, ml

VWB

Volume of NaOH used in titration of bottom sample for Water, ml

Effective volume of packed section, ml

Vt

Superficial velocity of water phase, LPH/m2

Vw

Superficial velocity of toluene phase, LPH/m2

Packed height, m

PRECAUTIONS & MAINTENANCE INSTRUCTIONS:

1.
2.
3.
4.
5.
6.

Interface should not be disturbed during the experiment.

Dont exceed the flow rate above 15 LPH.
Always use clean water & ensure that there are no foreign particles in it.
Always clean the column feed tanks & collecting tanks properly after experiment is over.
Never use feed tanks to store the chemicals used in the experiment.
Always drain the column once before running the experiment on desired second flow rates.

TROUBLESHOOTING:
1. If any type of suspended particles are come in the Rotameter. Remove the Rotameter clean the tube and fit
that at its place.
2. If there is any leakage tight that part or remove that and refix that again after wrapping Teflon tape.
3. If Rotameter fluctuating more than average tight control knob of it.
REFERENCES:
1. Coulson & Richardsons, Chemical EngineeringVol-2, 4th ed, Asian Books Pvt. Ltd, ND, 1998, Page 519520, 584-591.
2. Binay K.Dutta, Principles of Mass Transfer and Separation Processes, Prentice Hall of India Pvt Ltd., ND,
2007, Page 128-132, 455-456.