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CLB 20804
Experiment 1
PACKED COLUMN DISTILLATION PROCESS
1.0
OBJECTIVES
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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Mass Transfer I
CLB 20804
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Mass Transfer I
CLB 20804
3.0
EXPERIMENTAL PROCEDURES
3.1
NA/Exp1/SEPT 2014
Mass Transfer I
CLB 20804
Volume of
Ethanol(ml)
0
Volume of DeionizedWater(ml)
20
Refractive
Index(RI)
1.331
A2
19
1.332
A3
18
1.334
A4
17
1.337
A5
16
1.339
A6
15
1.341
A7
14
1.343
A8
13
1.346
A9
12
1.349
A10
11
1.350
A11
10
10
1.352
A12
11
1.354
A13
12
1.355
A14
13
1.356
A15
14
1.357
A16
15
1.358
A17
16
1.360
A18
17
1.361
A19
18
1.361
A20
19
1.361
A21
20
1.361
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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
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CLB 20804
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 1.5 and 2.0
3.3
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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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
= __________________
= __________________
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
= __________________
= __________________
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
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CLB 20804
Reflux ratio
= 2.0
= __________________
= __________________
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
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APPENDIX B
Equilibrium Data for Ethanol-Water Mixtures
Mole fraction of ethanol in liquid, x
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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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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