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EXPERIMENT 19

MIXER-SETTLER

20.1 OBJECTIVES

1) To determine the extraction efficiency of a single stage mixer settler as a liquid-


liquid extraction unit.
2) To investigate the effects of total flow rates on the extraction efficiency.
3) To investigate the effects of solvent to feed ratio on the extraction efficiency.
4) To investigate the effects of stirrer speed on the extraction efficiency.

20.2 INTRODUCTION

The equipment used is Single Stage Mixer Settler. It consists of two feed vessels, two
metering pumps with pulsation dampers, two receiving vessels and a single stage mixer
settler unit. The light phase and heavy phase liquids are first pumped from the feed
vessels at specific flow rates into the mixing chamber. Agitation of the two phases in the
mixing chamber will cause the transfer of solute component from one phase (raffinate) to
the other (extract). The mixture will then flow into the settling chamber where they are
settled and separated again into two different phases, before being collected in the
receiving vessels. Sample points are provided at key positions around the plant to allow
collection of both light and heavy phase liquid. In this way, effects of agitation and feed
flow rates of both phases on the extraction efficiency can be evaluated by means of
sample analysis. By using the unit, students shall be able to do experiments on the
followings:
a) demonstration of a single stage liquid-liquid extraction process.
b) determination of the extraction efficiency of a single stage mixer settler.
c) effect of total feed and solvent flow rates on the extraction efficiency.
d) effect of solvent to feed ratio on the extraction efficiency.
e) effect of stirrer speed on the extraction efficiency.

20.3 THE EQUIPMENT

20.3.1 Description and Assembly

All glass components of the SOLTEQ-QVF Single Stage Mixer Settler are made of
borosilicate 3.3 glass with PTFE gaskets. Please refer to the process flow diagram in
Figure 1.
1. Feed vessels (B1 & B2) Graduated cylindrical vessel with ports for filling, vent and
drain. Capacity: 20 L.
2. Mixer settler (MS1) Single stage mixer settler with an overhead stirrer motor and
adjustable interface level.
3. Stirrer motor (M1). Overhead motor with PTFE stirrer blades. Speed range: 50 to
2,000 rpm.
4. Metering pumps (P1 & P2). Diaphragm type pump with adjustable stroke length and
frequency, Stroke length: 30 to 100%, Stroke frequency: 0 to 180 strokes per min,
flow range: 0 to 12 L/hr.
5. Receiving vessels (B3 & B4). Graduated cylindrical vessel with ports for filling, vent
and drain. Capacity: 20 L.
6. Pulsation damper (B5 & B6). Cylindrical vessel with back pressure relief valve and
vent cap.
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EXPERIMENT 19

20.3.2 Safety Considerations

1. The unit must be operated under the supervision of an authorized staff.


2. All operating instructions supplied with the unit must be carefully read and
understood before attempting to operate the unit.
3. Feed stock which severely affects PTFE, PFA and borosilicate glass are not to be
used.
4. The system should not be subjected to shock, sudden impact, vibration, additional
load, or permanent external action of aggressive vapours.
5. Always check and rectify any leak. Leaking couplings should be carefully
retightened. Replace any gaskets or seals if necessary.
6. Do not touch the hot components of the unit.
7. Be extremely careful when handling hazardous, flammable or polluting materials.
8. Make sure the system is sufficiently ventilated when working at atmospheric
pressure.
9. Do not exceed the maximum pressure of 2 bar (g) for glass components.
10. Only properly trained staff shall be allowed to carry out any servicing. The technical
documentation and manufacturer's manual for each component must always be
observed.
11. Before any servicing, shut down the whole operation and let the system to cool down
and be properly ventilated.
12. Do not use any coarse or abrasive cleaners on glass components.

20.4 THEORY

When separation by distillation is ineffective or very difficult, liquid-liquid extraction is


one of the main alternatives to consider. Close boiling mixtures or substances that cannot
withstand the temperature of distillation, even under a vacuum, may often be separated
from impurities by extraction, which utilizes chemical differences instead of vapor
pressure differences. 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. The flow of streams and components in a liquid-liquid
extraction system is schematically shown in Figure 1. The following terms are widely
used to describe the different streams in a liquid-liquid extraction system:
F : Feed
S : Solvent
R : Raffinate
E : Extract

Figure 1: Flow of streams and components in a liquid-liquid extraction system.

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In an extraction process, a quantity of feed liquid, F is mixed with a quantity of solvent,


S in an agitated vessel, after which the layers are settled and separated. The extract may
be lighter or heavier than the raffinate, and so it may be shown coming from the top of
the equipment in some cases and from the bottom in others. Since the feed is a two
component system, by convention, the material to be extracted is commonly referred to
as the solute while the other component is generally referred to as the diluent. The
raffinate stream has the same components as the feed, though the proportions are
different, with the raffinate having a much lower solute concentration (leaner). An ideal
unit with perfect extraction will yield a raffinate which has only one component, that
being pure diluent. The liquid used to strip the solute from the feed is referred to as the
solvent. However, solvent is a general term and should not be confused with the feed
solvent or diluent. The solvent after becoming enriched in solute leaves the system as the
extract. It is also important to define the composition of the four streams and this may be
done in several ways:
a) Molar concentration = mol/dm3 (note numerically this is the same as kmol/m3)
b) Molal concentration = mol/kg
c) Mole fraction, XA =moles of A/ no. Total moles
d) Mole ratio, XA/B =No. of moles of A / No. of moles of B
e) Mass fraction, XA =mass of A/Total mass
f) Mass ratio, XA/B =Mass of A/Mass of B

Note: Fractions and ratios are dimensionless and may also be expressed in percent (%).
The common bases used in most literatures are either mole or mass fraction.

Since liquid-liquid extraction involves a 3-component system, a graphical representation


of the liquid mixtures is usually employed. There are two graphical systems, namely: a)
Rectangular coordinates b) Triangular coordinates. The rectangular coordinates are easier
to plot, but the triangular coordinates offer a more representative view of the component
compositions. However, it is important to fix the basis for the representation before
doing any calculations. This manual will assume a composition basis of mole fraction
and plots all component compositions in triangular coordinates. The individual
components of the chosen ternary system are usually represented by symbols as follows:
A : Solute
B : Diluent
C : Solvent

The assignment of symbols is arbitrary. Confusion shall not arise as long as the apex for
the solute is at the top while the bottom apexes are for the solvent and diluent. Referring
to Figure 2, the curve on the triangular diagram is called the binodal or solubility curve
of the ternary system. The curve, which is essentially a combination of diluent-rich and
solvent-rich curves, separates the upper region of stable single phase mixture from the
lower region of unstable mixture, which tends to separate into two phases. The
compositions of extract, E and raffinate, R are connected by tie-lines having different
slopes (i.e. not parallel). The tie lines get shorter as they get away from the x-axis, and
eventually they converge at a point P (plait point). The point P is not normally the
highest part of the curve. The number of theoretical stages can be determined graphically
by constructing operating lines and tie-lines on the binodal/ solubility curves, as outlined
in Figure 3. Consequently, the effects of different stirrer speeds and feed flow rates on
the extraction efficiency can then be evaluated.
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Figure 2: A typical 3-component system representation on an equilateral triangular


diagram

Figure 3: Operating lines and tie lines constructions for determination of extraction
efficiency.

20.5 OPERATING PROCEDURES

20.5.1 General Operating Procedures

It is important that the user read and fully understand all the instructions and precautions
stated in the technical documentation supplied with the mixer settler prior to operation.
The following procedures will serve as a quick reference for operating the unit. The set
up of the unit is as shown in Figure 4.

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Figure 4: Process flow diagram for the single stage mixer settler.

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1. Metering pump settings (P1 & P2)

The feed flow rate can be adjusted by changing the stroke and frequency settings on the
pump. Adjust the stroke length by turning the knob on the pump, and set the frequency
on the pump’s control panel. Refer to the pump’s flow rate settings diagram in Appendix
to determine the required stroke and frequency value in order to achieve a specific flow
rate.
NOTE: It is advisable to change the pump settings with the pump switched on and
running.

2. Pulsation damper (B5 & B6)

The vent cap should always be tightly closed and the damper vessels should be half full
during operation for optimal performance. The back pressure relief valves V5 & V6 can
be adjusted by using a small screwdriver to change the back pressure and consequently
the liquid level in the damper vessels. If the damper vessels are overfilled with liquid,
drain the liquid by opening the vent and bottom caps.
CAUTION: Do not adjust the back pressure relief valves too often as this may affect the
accuracy of the back pressure control.

3. Stirrer motor speed control (M1)

Turn the knob on the stirrer motor to control the rotational speed of the stirrer blades.
The actual and setpoint speed values are indicated on the display.4. Interface level
adjustment (V13) Turn the overflow valve V13 on top of the settler to adjust the
interface level between the light and heavy phases. Moving the valve up will raise the
interface level, while moving it down will lower the interface level.
WARNING: Do not adjust the overflow valve lower than the middle of the settling
chamber to prevent breaking the glass beneath.

20.5.2 General Start-Up Procedures

1. Ensure that all valves are closed.


2. Switch on the power supply for the unit.
3. Prepare the desired chemicals and fill feed vessel B1 with the feed solution (solute +
diluent) and feed vessel B2 with pure solvent.
4. Open valves V1 and V2.
5. Switch on metering pumps P1 & P2 and adjust the stroke and frequency settings to
mid range. Allow both the feed solution and solvent to enter the mixing chamber.
6. Switch on the stirrer motor M1 and set the speed to about 200 rpm.
7. Observe the flow of the mixed liquids into the settling chamber to form two layers.
Watch the interface level and position it at the middle of the settling chamber by
adjusting valve V13.
8. Allow both liquids to overflow into their respective collection vessels B3 and B4.
Vessel B3 will contain the heavy phase while vessel B4 will contain the light phase.
9. The unit is now ready for experiment.

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20.5.3 General Shut-Down Procedures

1. Switch off both metering pumps P1 and P2.


2. Switch off the stirrer motor M1.
3. Switch off the power supply for the unit.
4. Close valves V1 and V2.
5. Open valves V7 and V8 to drain all liquid from the mixer settler.
6. Open valves V11 and V12 to drain all liquid from the receiving vessels B3 and B4.
7. If required, open valves V3 and V4 to drain all liquid from the feed vessels B1 and
B2.

20.6 EXPERIMENT PROCEDURES

Solvent : toluene (light phase)


Feed : acetone (solute) + water (diluent), (heavy phase)
Extract : toluene rich (light phase)
Raffinate : water rich (heavy phase)

1. Prepare the following chemicals


a) Feed (heavy phase) – 20-L of acetone-water solution at the desired composition
between 30 to 50 wt%
b) Solvent (light phase) – 20-L of pure toluene
3. Perform the start-up procedures as described in Section 21.5.2.
4. Ensure that both pumps P1 & P2 settings are set at the desired flow rates. The flow
rates to be used are given in Appendix E. Please refer to the Pump Flow Rate Setting
Diagram as given in Appendix A to set the flow rates.
5. Set the stirrer M1 speed to between 200-600 rpm and let the experiment run for about
5–10 minutes.
6. Collect samples as follows:
a) Sample at valve V9 and label as R (raffinate)
b) Sample at valve V10 and label as E (extract)
7. Measure the refractive index for both samples and use the calibration curves to
determine the acetone (solute) composition in each sample. Please the calibration
curves in Appendix C and D for the determination of acetone composition in the
samples.
8. Repeat the sample collection and analysis (steps 6 to 7) at every 5–10 minutes. When
the composition values are constant over time, steady state has been reached.
9. Record the steady state composition values for the particular operating condition in
the table as given in Appendix E.
10. All equilibrium and calibration data for the acetone toluene-water system are given as
Appendix F and G.

20.7 ANALYSIS AND DISCUSSION:

1. Use the sample table in Appendix E for data collection.


2. Determine the theoretical extraction for a single stage mixer settler
3. Calculate the extraction efficiency of the mixer settler for different total flow rates
and stirrer speed. The solvent to feed ratio must be the same. Please refer to
Appendix H.

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Extraction efficiency = No. of theoretical stages


No. of actual stages1

= No. of theoretical stages


1

4. Plot a graph of extraction efficiency vs total flow rate.


5. Plot a graph of extraction efficiency vs stirrer speed.
6. From the available data, do a mass balance calculation around the mixer settler and
obtain the extract and raffinate flow rates. Calculate the separation efficiency for
different solvent to feed ratios.

Separation efficiency = Amount of extracted solute


Amount of solute in feed

= Extract flow rate x Extract composition


Feed flow rate x Feed composition

7. Plot a graph of separation efficiency vs solvent to feed ratio.

20.8 REFERENCES

1. McCabe, Smith & Harriott, “Unit Operations of Chemical Engineering”, McGraw


Hill, (Singapore), 2001.
2. Robert E. Treybal, “Mass Transfer Operations”, Third Edition, McGraw Hill Book
Co. (Singapore), 1980.
3. Robert E. Treybal, “Liquid Extraction”, Second Edition, McGraw Hill Series, 1963.
4. Institution of Chemical Engineers, “Standard Test Systems for Liquid Extraction”,
Second Edition, 1985.

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APPENDIX A

Pump Flow Rate Setting Diagram

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APPENDIX B

Physical Properties of Pure Components in the Ternary System

Component T (oC) Density Viscosity Surface Refractive


(kg/m3) (10-3 Pa.s) Tension Index (RI)
(10-3 Nm-1)
Water 20 998.2 1.003 72.75 1.333
25 997.02 0.8903 72.58 1.332
Toluene 20 866.7 0.586 28.4 1.497
25 862.3 0.552 27.6 1.494
Acetone 20 790.5 0.322 23.4 1.359
25 784.4 0.304 23.2 1.356

Acetone (CH3COCH3) : A colourless, volatile, extremely flammable liquid,


miscible with water, used as a solvent and reagent. Also known as 2-propanone.

Toluene (C6H5CH3) : A colourless, aromatic liquid derived from coal tar or from
the catalytic reforming of petroleum naphthas, insoluble in water, soluble in alcohol and
ether, used as a chemical intermediate, for explosives and in high-octane gasolines. Also
known as methylbenzene, phenylmethane and toluol.

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APPENDIX C
Calibration Curve for Toluene Rich Phase

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APPENDIX D
Calibration Curve for Water Rich Phase

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APPENDIX E

EXPERIMENTAL RESULT

Solvent Extract (E) Raffinate (R)


Feed flow Total flow Solvent to Stirrer speed Time
Run flow rate Solute Solute
rate (L/hr) rate (L/hr) feed ratio (rpm) (min) R.I. R.I.
(L/hr) composition (%) composition (%)
1 4 4 8 1.0 200

2 6 6 12 1.0 200

3 8 8 16 1.0 200

4 4 8 12 2.0 200

5* 6 6 12 1.0 200

6 8 4 12 0.5 200

7* 6 6 12 1.0 200

8 6 6 12 1.0 400

9 6 6 12 1.0 600

* Use data in Run 2.

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APPENDIX F

Binodal Composition for Acetone-Toluene-Water at 30oC

Acetone Toluene Water


(wt.%) (wt. %) (wt. %)
0 0.035 99.965
4.997 0.06 94.943
31.2 0.5 68.3
44.1 1.5 54.4
48.78 2.44 48.78
54.32 4.15 41.53
60.67 9 30.33
64.02 14.03 21.95
64 26 10
59.51 34.48 6.01
48.6 48.28 3.12
41.9 56.1 2
19.79 79.13 1.08
4.996 94.868 0.136
0 99.926 0.074

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APPENDIX G

Equilibrium (Tie Line) Composition at 30oC

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APPENDIX H

Sample of Data Analysis

APPENDIX I

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Triangular Plot for Ternary Diagram

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