Experiment 4

PULSED COLUMN LIQUID-LIQUID EXTRACTION UNIT

1.0

OBJECTIVE

Operate a Liquid Liquid Extraction Experiment using a Pulsed Column Liquid Liquid
Extraction Unit.

To determine the height equivalent theoretical plates (HETP) for column by using
equilateral triangular diagram.

2. 0

To investigate the effect of the pulsation stroke on the HETP.

INTRODUCTION

Extraction is a unit operation used to separate components based on their Chemical Differences
instead of differences in Physical Properties.

When separation of components of a Liquid

Mixture becomes ineffective or very difficult by means of Distillation, and then Liquid
Extraction is one of the main alternatives to consider.
Separation by liquid-liquid extraction can be defined as the selective removal of one or more
components either from a homogeneous liquid mixture or from a solution, using a second liquid
or solvent, which is partially or wholly immiscible with the first.
A widely used terminology describes the system in terms of :
o

Feed.

Solvent.

Raffinate.

Extract.

NA/Exp 4/SEPT 14

The equilateral-triangle diagram developed by Hunter and Nash is commonly used for multistage
extraction calculations involving ternary systems. In practice, toluene is used as solvent to
remove the solute, acetone, from water; the toluene-rich phase is called the extract, and the waterrich phase the raffinate.
The following diagram indicates the Flow of Streams And Components In a Liquid Liquid
Extraction System.

Components of Pulsed Column Liquid Liquid Extraction Unit are as follows :

o Feed Vessels (B1 / B2) Graduated Cylindrical Vessels with 25 L capacity.

o Column (K1) a DN 80 Packed Column with 10 mm Ceramic Saddles. Effective Height
of column is 2.5 m.

o Dosing Pumps (P1 / P2) 0.25 kW Piston Pumps with up to 42 L/h capacity.
o Pulsator (P3) 0.25 kW Pulsator Pump with a 20 mm stroke and 50 Hz frequency.
o Receiving Vessels (B3 / B4) Graduated Cylindrical Vessles with 25 L capacity.
o Pulsation Dampers (B5 / B6).

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NA/Exp 4/SEPT 14

3.0

EXPERIMENTAL PROCEDURES

3.1

Chemicals and Ancillary Equipments Required:

Chemicals Required.

Acetone (Solute).

Diionized-Water( Diluent)

Toluene (Solvent).

Ancillary Equipments Required:

3.2

Two 2000ml Jug and two 25ml beakers.

Refractometer index .

General Start-up Procedures.

1. Prepare the following chemicals :
a) Feed (Heavy Phase): Mixture of Acetone Water solution. Prepare 20 litres of
50wt % mixture of Acetone in Water by mixing appropriate quantities of the
Acetone in Distilled Water.
b) Prepare 20 litres of Solvent (Light Phase): Pure Toluene.
2. Ensure that all valves are closed.
3. Fill Feed Vessel B1 with the Acetone Water solution and Feed Vessel B2 with the Pure
Toluene Solvent. Determine the composition of the feed (heavy phase) using
refractometer.
4. Turn on the power supply
5. Turn on the main power control switch.
6. Open valves V3. Switch on Feed Pump P1.
7. Allow the Acetone Water Solution (Heavy Phase) to enter the column and fill to a level
of about 10 cm below the solvent inlet. Switch off Pump P1.
8. Open valve V4. Switch on Solvent Pump P2.
9. As the Solvent (Light Phase) enters the column, carefully watch the Interface Level
which forms between the Light and Heavy Phases. Maintain the interface level at 2-3 cm
above the solvent inlet.

NA/Exp 4/SEPT 14

10. The unit is now ready for experiment.

Experiment: Extraction of Acetone from Water Using Toluene.
In this experiment, there are two feeds to the Mixer and two outlet flows from the Settler.
Feed Flows:
Solvent: Toluene (Light Phase).
Feed: Acetone Water Mixture (Heavy Phase).
Outlet Flows:
Extract

: Toluene Rich Phase.

Raffinate: Water Rich Phase.

PROCEDURES:
1. Check to ensure the liquid starts to overflow at the top of the column, stop Pump P2.
2. Turn on the both pumps P1 and P2 .
3. Turn on the Pulsator Pump P3 and set the Pulsation Stroke Length.
4. Let the experiment run for a while to attain steady state.
5. Allow both liquids to flow into the collection vessels B3 and B4 respectively. The
bottom product contains the Water Rich Phase (Raffinate ) while the top product contains
the Toluene Rich Phase ( Extract ).
6. Open valve V10 to withdraw a 10 ml sample of Raffinate and open valve V12 to collect a
10 ml sample of Extract .
Note: Take samples at suitable time intervals and measure their Refractive
Indices. When the readings are consistent over time, steady state has been
reached.
7. Record the Refractive Index of both samples and use the given Calibration Curves
(Appendix B) to determine the Acetone (Solute) composition in each phase.
8. Record all data in appendix B.
9. Repeat the experiment (steps 3 to 10) by turning on the pulsator pump P3 and changing
the pulsation stroke length. Fix the same flow rate and feed composition throughout the
whole experiment.

NA/Exp 4/SEPT 14

3.3 General Shut Down Procedures.

1. Switch off pumps P1, P2 and P3.
2. Close valves V3 and V4.
3. Open valves V5, V6 and V9 to drain all liquid from the experiment.
4. Open valves V13 and V14 to drain all liquid from the Receiving Vessels B3 and B4.
5. Turn off the power for the control panel.

4.0

ANALYSIS & DISCUSSION.

Discuss all your results. The questions below only serve as a guideline. Your discussion should
not only limit to these questions.
1. Plot the calibration curve for toluene rich phase and water rich phase (Refractive index vs
acetone weight percent) by refer data given in Appendix B.
2. Determine weight percent acetone of the raffinate and extract in Appendix A by refer to
calibration curve prepare in question 1.
3. Determine the required theoretical extraction stage from the pulsed column liquid-liquid
extraction experiment results by construct the graph using equilateral diagram given in
Appendix E. Refer to Appendix D for a step by step calculation guide.
4. Calculate the height equivalent theoretical plates (HETP) of the extraction column for
different pulsation stroke. No of theoretical plates are obtained from Question 3.
a. HETP = Effective column height / No of theoretical plates
5. From the available data, do a mass balance calculation around the extraction column and
obtain the extract and raffinate flow rates.
6. Discuss the various factors that would help to increase the rate of transfer of solute to
solvent phase.
7. Explain how pulsation frequency increases the transfer rate in pulsed columns.
5.0 REFERENCES
1. McCabe and Smith, (2005), Unit Operations of Chemical Engineering, 7th Edition, McGrawHill.
2. Robert E.Treybal., (1981), Mass Transfer Operations, 3rd Edition, McGraw-Hill.

NA/Exp 4/SEPT 14

APPENDIX A
Experiment: Extraction of Acetone from Water Using Toluene.
Results:
Feed RI
Feed Composition

Feed
flowrat
e
(L/hr )

Solvent
flowrat
e (L/hr

Solvent
to Feed
ratio

Pulsatio
n stroke
(mm)

Raffinate
Extract
(water rich phase )
(Toluene rich phase)
Time Refractive
Solute
Refractive
Solute
(min)
Index
(Acetone)
Index
(Acetone)
Composition
Composition
(wt %)
(wt %)

NA/Exp 4/SEPT 14

APPENDIX B
Data Calibration Curve for Toluene Rich Phase
No
1
2
3
4
5
6

Volume (mL)
Toluene Water Acetone
104.1
91.8
64.6
50.0
37.5
16.3

2.5
3.0
4.1
5.4
7.3
23.0

12.7
25.2
54.0
67.4
77.4
81.6

Average Weight (g)

Toluene Water Acetone
89.8
79.1
55.7
43.1
32.3
14.0

0.3
1.1
2.0
4.0
7.0
22.0

10.0
19.8
42.4
52.9
60.7
64.0

Ave. % Weight
Acetone Toluene
10.0
19.8
42.4
52.9
60.7
64.0

89.8
79.1
55.7
43.1
32.3
14.0

Refractive
Index
(Ave)
1.4753
1.4649
1.4304
1.4147
1.4006
1.3687

Data Calibration Curve for Water Rich Phase

No
1
2
3
4
5
6

Volume (mL)
Toluene Water Acetone
16.8
13.9
8.0
3.6
1.6
1.4

22.0
25.1
34.6
46.1
59.6
80.2

81.6
80.1
74.7
65.0
50.4
25.5

Average Weight (g)

Toluene Water Acetone
14.0
12.2
6.9
3.0
1.0
0.2

22.0
25.0
34.5
46.0
59.5
79.9

64.0
62.8
58.6
51.0
39.6
20.0

Ave. % Weight
Acetone Toluene
64.0
62.8
58.6
51.0
39.6
20.0

14.0
12.2
6.9
3.0
1.0
0.2

Refractive
Index
(Ave)
1.3681
1.3682
1.3661
1.3618
1.3556
1.3449

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APPENDIX C

Equilibrium data Binodal/ Solubility Data for Acetone-Toluene-Water System

Toluene Rich phase
Acetone (wt
%)
9.79
19.48

Water Rich phase

Water(wt%)

Toluene(wt%)

2.42
2.92

87.78
77.60

Acetone (wt
%)
63.93
63.14

41.61

3.97

54.42

52.30

5.27

60.67
63.58

Water(wt%)

Toluene(wt%)

21.68
24.88

14.39
11.98

58.84

34.27

6.59

42.43

51.22

45.68

3.10

7.20

32.14

39.65

58.97

1.38

22.54

13.89

19.94

78.86

1.20

Data for Solute Distribution (Tie lines)

No

1
2
3
4
5
6

Volume (mL)
Toluene

Water

Acetone

23.2
30.2
34.8
41.7
51.0
64.9

20.0
20.0
20.0
20.0
20.0
20.0

76.5
68.8
63.7
56.1
45.9
30.6

Heavy Phase (Water

Rich)
Refractive
% Weight
Index
(Acetone)
1.3621
1.3574
1.3544
1.3531
1.3494
1.3443

51.7
40.8
32.7
30.1
21.4
9.6

Light Phase (Toluene

Rich)
Refractive
% Weight
Index
(Acetone)
1.3735
1.3979
1.3943
1.4213
1.4084
1.4183

69.8
55.5
50.4
42.2
39.4
32.5

NA/Exp 4/SEPT 14

APPENDIX D
STEP BY STEP CALCULATION GUIDE
1. Obtain the equilibrium data from Appendix C. Draw the equilibrium data binodal/solubility curve for toluene rich phase and water rich
phase (Acetone fraction vs Toluene fraction) on a triangular plot (Appendix E).
2. Plot the corresponding tie lines of acetone for toluene rich phase and water rich phase on a triangular plot (refer to Appendix C).
3. Locate the each points for on a triangular plot based on:
Feed,F
Solvent ,S
Raffinate,R(refer to Table appendix A)
Extract ,E(refer to Table appendix A)
Feed and solvent mixture,M

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4. Locate the point R,where all operating lines should meet.

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5. Draw a tie line from point E to its equilibrium point on the bimodal plot. Connect an operating line from that equilibrium end of the tie
line to point R. Extend that operating line so that it intersects with the bimodal plot at the other end. Draw another tie line from that new
intersection and continue until a tie line has passed the operating line connecting R and S.

6. Count the number of tie lines contained inside the E-F-R-S quadrilateral(it may not be a rounded number).That will be the number of
required theoretical stage to achieve final raffinate and extract compositions.

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APPENDIX E

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