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EXPERIMENT 2:
INTRODUCTION
The Batch Packed Distillation Unit is developed primarily for teaching, training
and research purposes. It is used for the separation of mixtures at atmospheric
pressure in a batch operation. The unit has the following special features, which
are of particular value in training situations:
Direct heat input into the evaporator using cartridge heaters.
Silver coated and vacuum jacketed column minimizes heat loss to the
surroundings.
Vapour sampling and liquid sampling on the bottom and top to determine
the practical separation behaviour of the particular mixture.
The method of operation of a packed distillation unit for the separation of liquid
mixtures can be described in the following terms: The vapour mixture rises from
the evaporator, passes over the column packings and is fully condensed in the
condenser. The condensate runs down the column counter-current to the vapour
through the packings back into the evaporator. Among the packings, the rising
vapour attempts to achieve equilibrium with the liquid. In the ideal case the rising
vapour should be in equilibrium with the liquid. In actual columns, complete
exchange does not always take place.
The efficiency of batch packed distillation unit can be evaluated using the height
equivalent theoretical plates (HETP), which is defined as the height of the column
divided by the number of theoretical plates required to achieve the same
separation as the packed column. As the purity of a distillate is dependent to a
very large extent on the number of theoretical plates, determination of the
number of theoretical plates in a column is very important.
Cooling
Water
TI
05
FI
02
V9
V10
V8
Cooling
Water
TI
06
FI
01
W3
Vent
TI
03
V3
KS 01
TI
02
TI
07
V2
W4
TI
04
K1
PdI
01
B3
V4
V5
V6
PI
01
B2
TI
01
LS01
W1,2
V7
B1
V1
2. Cooling Water System Laboratory tap water is used as the cooling media.
Hose connections are such that the cooling water enters both the top
condensor (W3) and product cooler (W4) in parallel. Adjust both the cooling
water flow rate to maximise cooling and condensation. The temperature of the
cooling water leaving the two units should not exceed 45C.
Caution: In order to avoid water hammer, open the cooling water valves
slowly.
3. Heater Power The heater output power is adjustable between 0 and 100%
so that one may vary the flow rate of the vapor and liquid inside the distillation
column. Turn the heater resistance knob located at the control panel between
a value 0 to 10.
4. Reflux Divider The reflux divider controller KS-01 has 3 positions with the
following settings:
Position 0
Total reflux
Position Hand Total distillate offtake
Position Auto Timer controlled reflux
To adjust the reflux ratio, set the reflux timer and distillate timer on the control
panel at KS-01. The reflux timer is represented by the time in seconds on the
display, while the distillate timer is represented by the time in seconds with an
additional blinking light at the lower right corner of the display. The reflux ratio
is equal to the ratio between the total reflux time and the total offtake time.
EXPERIMENTAL PROCEDURES
General Start-Up Procedures
1. Ensure all valves are closed except valve V3 and ventilation valve V6.
2. Prepare a 15 L mixture containing ethanol and filtered water at the desired
composition. Open the charge port cap and charge the evaporator B1 with the
ethanol-water mixture. Close the charge port cap.
Note:
water.
You can use any suitable binary system other than ethanol-
Sampling Procedures
Samples can be taken from the distillate and the bottom product for analysis:
1. Distillate sampling:
a)
b)
c)
d)
e)
Open sampling valve V2 to drain the sample line of any remaining liquid.
Place a vial below valve V2.
Set the reflux divider to total distillate for a few seconds.
Collect a 10 mL sample and close sampling valve V2.
Switch the reflux divider back to total reflux.
2. Bottom sampling:
a) Place a vial below valve V1.
b) Open sampling valve V1 and collect a 10 mL sample. Be careful of the hot
liquid while collecting a sample.
c) Close sampling valve V1.
d) Cool the sample by immersing the sample vial in cold water.
Note: Always collect samples in vials with cap to avoid excessive evaporation
of ethanol before analysis.
PROCEDURES:
1.
2.
Once the distillation unit has reached stable condition, record the top and
bottom temperatures.
3.
Collect samples from the distillate and bottom product (Section 3.4).
4.
Measure the refractive index for both samples and determine their
compositions.
5.
For different liquid and vapor loading, adjust the heater power settings in
W1 and W2. Doing so will decrease the heating duty and hence decrease
the vapor flow in the column. Consequently, the liquid flow will also
decrease.
6.
Change the heater power settings and wait for approximately 15 mins to
allow the distillation unit to achieve stable condition. Then, follow steps 2
to 5.
2.
Using the X-Y equilibrium diagram for ethanol-water system, mark the top
and bottom compositions on the diagram and determine the theoretical
number of plates in the distillation unit using the McCabe-Thiele method.
Refer to Appendix D.1 for a step-by-step guide.
3.
4.
Plot a graph of HETP vs. heating power and observe the relationship.
PROCEDURES:
1. Perform the general start-up procedures (Section 3.1). Record the initial
volume and composition of ethanol-water mixture in the reboiler.
2. Set the heater power to 70%.
3. Once the distillation unit has reached stable condition, record the top and
bottom temperature.
4. Collect samples from the distillate and bottom product (Section 3.4). Do not
discard the samples. Instead, return all distillate and bottom samples into
separate containers for mass balance calculations later.
5. Measure the refractive index for both samples and determine their
compositions. This will constitute the composition at the beginning of the
experiment.
6. Set the reflux divider to give a reflux ratio of 1 (e.g. reflux timer 5 sec, distillate
timer 5 sec), and allow the process to run for 10 minutes.
7. Collect samples from the distillate and bottom product (Section 3.4). Measure
the refractive index for both samples and determine their compositions.
8. Measure the distillate flow rate as follows:
a)
b)
c)
d)
3. Determine the theoretical number of plates for each sampling time in the
distillation column using the McCabe-Thiele method. Refer to Appendix D.2
for a step-by-step guide.
4. Calculate the height equivalent theoretical plates (HETP) by dividing the
effective column height with the number of theoretical plates.
5. Using the Rayleigh equation, calculate and plot the amount of ethanol left in
the evaporator against time.
6. Carry out a mass balance calculation on the distillation column at the end of
the experiment and compare with the experimental results.
Safety Considerations
1. The unit must be operated under the supervision of an authorized staff who
has been properly trained to handle the unit.
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 affect 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.
6. Do not touch the hot components of the unit.
7. Be extremely careful when handling hazardous, flammable or polluting
materials.
8. Restore the system to operating conditions after any repair job.
9. Make sure the system is sufficiently ventilated when working at atmospheric
pressure.
10. Do not exceed the maximum coolant pressure of 2 bar(g) for the top
condenser (W3) and product cooler (W4).
11. Only a properly trained staff shall be allowed to carry out any servicing.
Manufacturer's manual must always be observed.
12. Before any servicing, shut down the whole operation and let the system to
cool down and be properly ventilated.
13. Do not use any coarse or abrasive cleaners on glass components.
14. Leaking couplings should be carefully retightened. Replace any gaskets or
seals if necessary.
REFERENCES
1. McCabe, Smith & Harriott, Unit Operations of Chemical Engineering,
McGraw Hill, (Singapore), 2001.
= ____ mol/L
Volume of
ethanol (mL)
Volume of
water (mL)
10
1.0
9.0
2.0
8.0
3.0
7.0
4.0
6.0
5.0
5.0
6.0
4.0
7.0
3.0
8.0
2.0
8.5
1.5
9.0
1.0
9.5
10.0
0.5
0.0
Mole fraction
ethanol
Mole fraction
water
Refractive index
(RI)
APPENDIX B
SAMPLE TABLE FOR EXPERIMENT 1: BATCH DISTILLATION AT TOTAL REFLUX
Heater
W1,W2
power
100 %
80 %
60 %
40 %
20 %
Distillate
Temp
(C)
Refract.
index
Bottom product
Mole
fraction
Temp
(C)
Refract.
index
Mole
fraction
HETP
(mm)
APPENDIX C
SAMPLE TABLE FOR EXPERIMENT 2: BATCH DISTILLATION AT CONSTANT REFLUX
Heater power = _____ %
Reflux ratio
Time
(min)
= _____
Distillate
Temp
(C)
Refract.
index
Mole
fraction
0
10
20
30
40
50
60
= _____ L
= _____ L
= _____ L
Bottom product
Flow rate
(mL/min)
Temp
(C)
Refract.
index
Mole
fraction
APPENDIX D.1
MCCABE THIELE CALCULATION FOR BATCH DISTILLATION AT TOTAL REFLUX
1. Start with the X-Y equilibrium diagram and
locate the following points on the X axis:
a) Distillate, D
b) Bottom product, B
B
Bottom
Distillate
B
Bottom
Distillate
3. The number of theoretical stages required to achieve the separation obtained from the
distillation column can be calculated from the number of steps drawn on the diagram. In this
case, it is 3.
APPENDIX D.2
MCCABE THIELE CALCULATION FOR BATCH DISTILLATION AT CONSTANT REFLUX
1. Start with the X-Y equilibrium diagram
and locate the following points on the X
axis for every sampling time:
a) Distillate, D
b) Bottom product, B
(2 sets will be shown together here for
comparison)
D1
D2
B1
B2
D1
D2
x D1
R 1
x D2
R 1
B1
B2
D1
D2
B1
B2
5. Use the Rayleigh equation to find the amount of ethanol left in the reboiler at time t 1.
n0
n1
dn
n
dx
x0
x1
ln
n0
n1
n0
n1
exp
x0
dx
x1
y x
t0 = initial condition
t1 = final condition
x = bottom composition
y = top composition
n = total number of moles of ethanol in the reboiler
a) Calculate the values of
1
for every value of x.
y-x
1
against x.
y-x
c) For a change of composition between x1 and x0, find the area below the graph from x1
x0 dx
to x0. That will be the integration value of
.
x1 y
x
b) Plot a graph of
APPENDIX E
PHYSICAL PROPERTIES OF COMPONENTS
E.1
Ethanol
Water
CH3CH2OH
H2O
46.07
18.02
0.789
1.000
112.0
0.0
78.4
100.0
514
647.13
62.2
217.7
Formula
E.2
Temperature
(C)
Liquid phase
Vapor phase
100
0.0000
0.0000
95.5
0.0190
0.1700
89.0
0.0721
0.3891
86.7
0.0996
0.4375
85.3
0.1238
0.4704
84.1
0.1661
0.5089
82.7
0.2337
0.5445
82.3
0.2608
0.5580
81.5
0.3273
0.5826
80.7
0.3965
0.6122
79.8
0.5079
0.6564
79.7
0.5198
0.6599
79.3
0.5732
0.6841
78.7
0.6763
0.7385
78.4
0.7472
0.7815
78.2
0.8943
0.8943
0.9000
0.8000
0.7000
0.6000
0.5000
0.4000
0.3000
0.2000
0.1000
0.0000
0.0000
0.1000
0.2000
0.3000
0.4000
0.5000
Liquid mol fraction
0.6000
0.7000
0.8000
0.9000
1.0000
20C
25C
30C
0.99823
0.99708
0.99568
0.98938
0.98817
0.98670
10
0.98187
0.98043
0.97875
15
0.97514
0.97334
0.97133
20
0.96864
0.96639
0.96395
25
0.96168
0.95895
0.95607
30
0.95382
0.95067
0.94741
35
0.94494
0.94146
0.93790
40
0.93518
0.93148
0.92770
45
0.92472
0.92085
0.91692
50
0.91384
0.90985
0.90580
55
0.90258
0.89850
0.89437
60
0.89113
0.88699
0.88278
65
0.87948
0.87527
0.87100
70
0.86766
0.86340
0.85908
75
0.85564
0.85134
0.84698
80
0.84344
0.83911
0.83473
85
0.83095
0.82660
0.82220
90
0.81797
0.81362
0.80922
95
0.80424
0.79991
0.79555
100
0.78934
0.78506
0.78075
Density (kg/m3)
-18-