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Apparatus

The main apparatus is liquid-liquid extraction unit (Model: BP 61)

Figure 1: liquid-liquid extraction until (Model: BP 61)

Procedures
General start-up procedures
1.
a)
b)
2.
3.

The following chemicals were prepared.


Feed (heavy phase): mixture of acetone-water solution at the desired composition
Solvent (light phase): pure toluene
Ensure all valves were closed (screwed in).
The feed tank B2 was filled with 5L to 20L of acetone water and the feed tank B1

was filled with 10L to 20L of pure toluene solvent.


4. The main power was turned on at control panel.
5. The feed pump P2 was switched on. The acetone-water solution (heavy phase)
was allowed to enter the column and it was filled to a level about 5-15cm above
the solvent inlet. The pump P2 was switched off.
6. The solvent pump P1 was switched on.
7. As the solvent (light phase) was entered the column, the interface level which
forms between the light and heavy phases was watched carefully. The interface
level was maintained at 5-10 cm above the solvent inlet by adjusting the height of
the overflow tube.
8. Once the liquid was started to overflow at top of column, the pump P1 was
stopped.
9. The unit was now ready for experiment.
General Shut-Down Procedures
1. The pumps P1 and P2 were switched off.
2. The valve V4 to V8 were opened to drain all liquid from the equipment
3. The power for the control panel was turned off.
Experimental procedures

Feed flows: Solvent: Toluene (light phase)


Feed: Acetone-water mixture (heavy phase)
Outlet flows: Extract: Toluene rich phase/ Raffinate: Water rich phase

1. Ensure that all the equilibrium and calibration data were obtained (Appendix D).
2. The general start-up procedures were performed.
3. The pumps P1 and P2 were switched on and flowrate of toluene was controlled at
2L/h and flowrate of feed solution at 5L/h using valve V1 and V2 respectively.
4. Both liquids were allowed 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).

5. Let the experiment was run for a while to attain steady state.
6. The valve V6 was opened to collect a 10 mL sample of raffinate and valve V4
was opened to collect a 10 mL sample of extract.
**Note: Take samples at suitable intervals and measure their refractive indices.
When the readings are consistent over time, steady state has been reached.
7. The refractive index of both samples at steady state was recorded and the
calibration curves (Appendix D) was used to determine the acetone (solute)
composition in each phase.
8. All data in the sample table in Appendix A were recorded.
9. The steps 4 to 8 were repeated by using different ratio of solvent to feed flow
rates. Same feed composition was fixed throughout the whole experiment.
**Note: Recommended flow rate for Pump 1, P1 and Pump 2, P2 are from 1 L/h
to 8 L/h for both pumps.

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