Mass Transfer I

CLB 20803

Experiment 2
BUBBLE CAP DISTILLATION PROCESS
1.0

OBJECTIVES

2.0

To operate vapor liquid separation process using a Bubble Cap Distillation

Unit.
To analyze the sample for the Top and Bottom Product by Refractometer to
obtain the Refractive Index in order to determine their respective composition.
To calculate the number of stages by using McCabe Thiele method

OVERVIEW

Distillation is a separation method in which mixture components in a liquid mixture are

separated based on their relative volatilities. The distillation column provides an environment
where the liquid and vapour phases can approach equilibrium within a column. In the packed
column there is high surface area for contact between the vapor and liquid, whereas the plate
column provides distinct stages at which equilibrium can be approached. Separation is achieved
by condensed vapor flowing as a liquid down the column theoretically achieving equilibrium with
the vapor flowing up the column. The distribution of components differs in each phase and results
in the separation. In the case of a binary mixture in batch distillation under total reflux, the vapor
condensing at the top of the distillation column will be rich in one of the components. Liquid
leaving the reboiler at the base of the column rich in the other component. As the system reaches
equilibrium the separation process reaches steady state for that apparatus and set of operating
conditions. This experiment is designed to study the distillation of a binary mixture of Ethanol
Water in a tray distillation column. Figure 1 is a sketch of a tray with bubble cap and Figure 2
shows the schematic diagram of the apparatus in this experiment.

Figure 1: Bubble cap tray

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Figure 2: Bubble Cap distillation column

3.0

Experimental Procedures

3.1

Chemicals and ancillary equipments required:

Chemicals Required.
Ethanol industrial grade.
Deionized-Water
Ancillary Equipments Required:
Two 2000ml Jug and two 25ml beakers.
Refractometer for measurement of sample concentrations.
Calibration Curve of ethanol-water mixtures.

3.2 Calibration curve of ethanol-water mixtures

1. Prepare a 5% of ethanol-water solution in a test tube.
2. Using a refractometer, obtain the refractive index reading for solution.

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3. Using increments of 5%, obtain refractive index readings for ethanol-water mixtures
up to 100%.
4. Plot a refractive index vs % of concentration graph.
3.3

General start-up procedures.

1. Prepare 30 litres of 10 % mixture of ethanol in water by mixing appropriate
quantities of the Industrial Grade of ethanol in distilled Water.
2. Ensure valves V1, RCV1, V3, V4, V5, V6, V7, V9 and RCV2 are closed.
3. Ensure valves V2, V8 and V10 are open.
4. Ensure that the Bottom Product sampling valve V5 and Top Product sampling valve
V4 is closed.
5. Slowly turn on the Cooling Water to the Condenser. Make sure water is indeed
flowing through it.
6. Check water flows to the drain from the Cooling Water outlets. Do not start the
experiment until the Cooling Water flow is visible in the outlets to the drain.
7. Set water pressure to 6 L/min.
8. Ensure that the Reboiler Vessel is already charged with the Ethanol Water mixture
through the Charge Port (Refer to the diagram).Fill the reboiler vessel with the
Ethanol-Water mixtures.
9. Check that the liquid level in Reboiler vessel is satisfactory (Refer to instructor /
technician).Otherwise top up with the Ethanol Water mixture through the Charge
Port (Refer to instructor / technician).
10. Ensure that the concentration of feed in the reboiler is correct and the liquid level is
at the vessel equator. (Refer to Lecturer / Technician).
11. The Reboiler Vessel should never be filled with liquid above the maximum level
indicated. The level should never recede below the minimum level while on
operation.
12. Obtain a sample of the ethanol-water mixture from the reboiler through valve V7 and
test its composition with the refractometer.
13. Turn on the main power control switch.
14. Turn on the power switch of the heater.
15. Switch on electrical supply (green heater on button).
16. Set heater controller HC4 to maximum setting (about 230V@ 30A).
17. Close the Reflux Adjustment Valve and valve below Product Cooler.
18. When distillate liquid is seen to flow through R1.A1, reduce the heat input and set
HC.4 to roughly 20A.
19. Allow a period of 15 minutes for the equipment to maintain thermal equilibrium with
surroundings.
20. The unit is now ready to be used for an experiment.
21. Switch on the heaters of the reboiler unit at the control panel and wait until the
mixture is seen boiling and vapor is seen to reach the top of the column

3.4

Experiment: Operation under reflux ratio condition

1. Ensure that the valves for reflux ratio RCV adjustment are opened.
2. Adjust both valve for Reflux Ratio RCV1 and valve below product cooler V2 so that
both readings on R1 and R2 provide a reflux ratio of 1.0 for the operation.

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3. Wait for about 15 minutes until the flow rate shown by R1 and the temperature
readings at the top and bottom of the columns are steady. (Refer to instructor /
technician).
4. Collect samples from the Reboiler and the overhead from the Sampling Port for every
5 minutes.
5. Observe the temperature of the reboiler T14.If the temperature is already 90 OC,
reduce the current of the reboiler to between 10A to 15A.
6. Observe the flow rate at R1. Adjust the valve for Reflux Ratio adjustment to ensure
that the Reflux Ratio is maintained at 1.0.
7. The concentration of the samples drawn is measure using the refractive index method
8. Record the reading of temperature for every 5 minutes
9. Readings are recorded in the provided table of results.
10. Then, the experiment is repeated with Reflux ration of 1.5 and 2.0.

3.5

General shut down procedures.

1.
2.
3.
4.
5.

Adjust heater controller HC.4 to minimum setting.

Switch off electrical supply (red heater off button).
Turn off the power switch of the reboiler.
Turn off the Main power control switch.
Do not drain the hot liquid from the Reboiler. If necessary, the liquid within the
system could be drained only when the liquid is already cooled.
6. Allow the cooling water to run for some time.
4.0

ANALYSIS AND DISCUSSION

Discuss all your results. The questions below only serve as a guideline. Your discussion
should not only limit to these questions.
1. Use the table for data collection in Appendix B.
2. Plot Calibration Curve for ethanol-water mixtures (Refractive index vs %
concentration.
3. Referring to calibration curve, estimate the mole fraction ethanol of the Top and
Bottom product samples for each reflux.
4. Plot the Equilibrium Curve for ethanol-water mixture. The data is given in Appendix
A.
5. Calculate the complete overall and component mass balance of the process.
6. By using McCabe Thiele Method, construct the graph to determine the number of
stages that occur in the processes for each reflux.
7. Discuss the results obtained and effect of reflux ratio for ethanol-water mixture
separation
8. Discuss any possible errors in the experiment and state any recommendation to
improve the process.

5.0

REFERENCES
1. Treybal, R.E., Mass Transfer Operations, 3rd ed., Mc-Graw-Hill, 1981
2. McCabe & Smith, Unit Operations of Chemical Engineering, 5th ed, Mc-Graw-Hill,
1993
3. Geankoplis,C. J. Z., Mass Transport Phenomena, 4th Ed., Rine Hart Winston, New
York.

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4. Coulson & Richardson, Chemical Engineering. Vol. 2 Pergamon Press, Oxford.

APPENDIX A
Equilibrium Data for Ethanol-Water Mixtures
Mole fraction of ethanol in liquid, x
0.00
0.05
0.10
0.40
0.60
0.80
0.94
0.90
0.94
0.96
0.98

Mole fraction of ethanol in vapor, y

0.00
0.38
0.53
0.75
0.79
0.86
0.94
0.91
0.94
0.96
0.99

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APPENDIX B
Table of Results
Reflux ratio

= 1.0

Rotameter reading R1 (L/hr)

= __________________

Rotameter reading R2 (L/hr)

= __________________

Temperature T4 (oC)

= __________________

Temperature T2 (oC)

= __________________

Time, t
(min)

TOP PRODUCT
Refractive index
Mole fraction
(RI)

BOTTOM PRODUCT
Refractive index
Mole fraction
(RI)

0
5
10
15
20
25
30
Reflux ratio

= 1.5

Rotameter reading R1 (L/hr)

= __________________

Rotameter reading R2 (L/hr)

= __________________

Temperature T4 (oC)

= __________________

Temperature T2 (oC)

= __________________

Time, t
(min)

TOP PRODUCT
Refractive index
Mole fraction
(RI)

BOTTOM PRODUCT
Refractive index
Mole fraction
(RI)

0
5
10
15

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20
25
30
Reflux ratio

= 2.0

Rotameter reading R1 (L/hr)

= __________________

Rotameter reading R2 (L/hr)

= __________________

Temperature T4 (oC)

= __________________

Temperature T2 (oC)

= __________________

Time, t
(min)

TOP PRODUCT
Refractive index
Mole fraction
(RI)

BOTTOM PRODUCT
Refractive index
Mole fraction
(RI)

0
5
10
15
20
25
30

FG/exp2/July2012