MASS TRANSFER 1 CLB 20804

Experiment 1
PACKED COLUMN DISTILLATION PROCESS

1.0 OBJECTIVES

 To operate vapor – liquid separation process using a Packed Column Distillation

Unit.

 To analyze the effect of reflux ratio on separation of ethanol-water system.

 To determine the number of stages by using McCabe Thiele method

2.0 OVERVIEW

Distillation is one of the important unit operations in many chemical industries and has
been used from the inception of chemical and process industry. Distillation is used for the
separation of components in a liquid mixture of volatile constituents. The Distillation Column is
usually a vertical column where the liquid and vapor phases of the mixture are made to mix and
approach equilibrium.

The two types of distillations utilized in industry are batch and continuous. Batch
distillation is desirable when small quantities of high valued chemicals need to be separated. In a
batch system, the column can handle different mixtures by simply changing its operating
conditions. In this lab, the packing in the column is rachig rig glass. The distillation column also
contains a condenser, which cools and condenses the vapor leaving the top of the column. A
reboiler is connected to the bottom of the distillation apparatus and it provides the reboil heat that
is necessary for distillation.

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Figure 2 shows the schematic diagram of the apparatus in this experiment.

Figure 2: Packed distillation column

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3.0 EXPERIMENTAL PROCEDURES

3.1 Chemicals and Ancillary Equipments Required:

PART A: Calibration curve of ethanol-water mixtures

Chemicals required:
 Ethanol industrial grade.
 Deionized-Water.

Ancillary equipments required:

 Test Tube( 20 test tube per group)
 Beakers (50 ml).
 Dropper
 Glass rod
 Refractometer

PART A: Calibration curve of Ethanol-Water mixtures

1. Obtain 21 test tubes; label the test tubes with A1 until A21. Total volume in each test
tube is 20 ml.
2. Prepare the mixture of ethanol and deionized water to each test tube according to
volume indicate by Table 1.
3. Note that, Stir the mixture of solution (A1 until A21) with glass rod.
4. Obtain the refractive index reading for solution in each tube using refractometer.
5. Record the refractive index reading for each tube tests using Table 1.

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Table 1: The volume of chemical needed in each test tube

Test tube Volume of Volume of Deionized- Refractive

Ethanol(ml) Water(ml) Index(RI)
A1 0 20
A2 1 19
A3 2 18
A4 3 17
A5 4 16
A6 5 15
A7 6 14
A8 7 13
A9 8 12
A10 9 11
A11 10 10
A12 11 9
A13 12 8
A14 13 7
A15 14 6
A16 15 5
A17 16 4
A18 17 3
A19 18 2
A20 19 1
A21 20 0

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PART B: Operate vapor -liquid separation process using a Packed Column Distillation Unit
under reflux ratio.

Chemicals required:
 Ethanol industrial grade.
 Deionized-Water.

Ancillary equipments required:

 Dropper
 Beakers (50 ml)
 Tissue
 Refractometer

3.2 General start-up procedures.

1. Prepare 30 litres mixture of ethanol-deionized water by adding 10% of ethanol from

total volume of the mixture.
2. Ensure valves V3, V4 and V5 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 are closed.
5. Slowly turn on the Cooling Water (CW) supply to the Condenser. Make sure water is
indeed flowing through it by makesure 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.
6. Set water flowrate of Cooling Water (CW) to 6 L/min by adjusting water flow
control FCV2.
7. Open valve V6, fill the reboiler vessel
8. (B1) with the 30 L Ethanol-Water mixtures.
9. Close the valve V6 and open valve V2 after finish fill reboiler vessel with the 30 L
Ethanol-Water mixtures.
10. 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 Turn on the main power control switch.
11 Turn on the power switch of the heater.
12 Switch on electrical supply (green ‘heater on ‘button).
13 Set heater controller HC4 to maximum setting (about 230V@ 30A).

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14 Allow a period of 15 minutes for the equipment to maintain thermal equilibrium with
surroundings.
15 The unit is now ready to be used for an experiment.

Experiment: Operation under reflux ratio condition

1. When mixture is start to boil, close valves V2.

2. When distillate liquid is seen to flow through R1.1C, adjust both valve for Reflux
Ratio RCV1 so that both readings on R1 and R2 provide a reflux ratio of 1.0 for the
operation.
3. Ensure that the Reflux Ratio is maintained at 1.0.
4. Collect samples for bottom product from valve V5 and the overhead product from
valve V4 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 20A.
6. Concentration of the samples drawn is measure using the refractive index method
7. Record all data obtained in appendix A.
8. Repeat the experiment (steps 2 to 6),for reflux ratio of 2.0

3.3 General shut – down procedures.

1. Adjust heater controller HC.4 to minimum setting.

2. Switch off electrical supply (red ‘heater off’ button).
3. Turn off the power switch of the reboiler.
4. Turn off the Main power control switch.
5. 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.

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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. Make a calibration graph based on your data obtained from Experiment A by

plotting Refractive index (RI) on the y-axis against mole fraction of ethanol on the x-
axis.
2. Determine the mole fraction of ethanol for the top and bottom product for each reflux
by refer to calibration graph.
3. Calculate the complete overall and component mass balance of the process.
4. Determine the number of stages that occur in the processes for each reflux by
construct the graph McCabe Thiele Method. Equilibrium data for ethanol-water
system is given in Appendix A.
5. Discuss the results obtained and effect of reflux ratio for ethanol-water mixture
separation
6. 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.
4. Coulson & Richardson, Chemical Engineering. Vol. 2 Pergamon Press, Oxford.

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APPENDIX A

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 TOP PRODUCT BOTTOM PRODUCT

(min) Refractive index Mole fraction Refractive index Mole fraction
(RI) (RI)
0
5
10
15
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 TOP PRODUCT BOTTOM PRODUCT

(min) Refractive index Mole fraction Refractive index Mole fraction
(RI) (RI)
0
5
10
15
20
25
30

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APPENDIX B

Equilibrium Data for Ethanol-Water Mixtures

Mole fraction of ethanol in liquid, x Mole fraction of ethanol in vapor, y

0.00 0.00
0.05 0.38
0.10 0.53
0.40 0.75
0.60 0.79
0.80 0.86
0.94 0.94
0.90 0.91
0.94 0.94
0.96 0.96
0.98 0.99

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STEP BY STEP TO CONSTRUCT GRAPH MCCABE THIELE METHOD

1. Draw the equilibrium curve based on data given in Appendix B, by plotting mole fraction
of ethanol in vapor on the y-axis against mole fraction of ethanol in liquid on the x-axis.
2. Draw the 45-degree line( y =x)
3. Indicate distillate (xD), bottom (xB) and feed (xF) composition on the graph based on
data obtained from experiment.(refer to appendix A).
4. Draw the feed line (q line). For saturated liquid, this is a vertical line running from the
feed composition (xF) through the equilibrium curve.
5. For a specified reflux ratio, r, draw the 'rectifying' line (ROL). This rectifying line begins
at the point xD on the 45-degree line and has intercept on y-axis.

ROL equation:

6. Draw the 'stripping' line (SOL) by connecting the intersection of the feed line and the
rectifying line and the point xB on the 45-degree line.
7. Beginning at the point xD on the rectifying line, draw a horizontal line to the equilibrium
curve and then a vertical line to the operating (rectifying or stripping) line.
8. Repeat step 7 forming a staircase until you reach or pass the point x B on the 45-degree
line.
9. Each point where the staircase intersects the equilibrium curve denotes one stage in the
column.

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Sample Graph of McCabe Thiele Method

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