Distillation 1

Batch Distillation of a Binary Mixture

of Methanol-Isopropanol

Group Number 3
Date of 20/10/2016
Experimentation
Date of handing-in 27/10/2016
Name Nayantara Soni 023391
Names of Group Noorulain Iftikhar 023229
Members Newton Lo Well 023315
Tan Kin Long 014727

Table of Contents
No Content Page Number
1 Summary 2
2 Materials, Equipment and Operating Conditions 3
3 Results 4
4 Discussion 6
4.1 Variation of composition of methanol with time in the 6
reflux divider vessel and evaporator tank

4.2 Temperature profile in the distillation column 6

4.3 Discrepancies in the number of moles of methanol 7
4.4 Optimum number of stages and Efficiency of 7
Distillation
4.5 Method to increase yield and efficiency of distillation 8
5 Conclusion 9
6 References 10
7 Appendix 11

1. Summary

1
The purpose of this experiment is to study batch distillation of
methanol-isopropanol at a constant reflux ratio of 60%. The variation
of temperature along the column, and the variation of composition in both
the reflux divider vessel and the evaporator tank at different times is
recorded and analyzed.
From the experiment, it can be observed that both the percentage
compositions of methanol from the reflux divider vessel and the
evaporator vessel decreases with time. Another significant trend that is
observed is the decrease in temperature when moving upwards along
the column.
The initial and final number of moles of methanol were also calculated to
determine if there were any discrepancies. Besides that, the optimum
number of stages was calculated using the McCabe Method. Based on the
optimum number of stages and actual number of stages used, the efficiency
was determined. Suggestions on the method to improve efficiency were also
made.

2
2. Materials, Equipment and Operating Conditions
The main material used in this experiment is the 6000ml binary mixture of
methanol-isopropanol where methanol is the more volatile component(MVC)
and propanol is the less volatile component(LVC). Water is used as a cooling
agent in the condenser. Besides that, water and ice cubes also form an ice-
bath to collect the hot bottom product from the evaporator for safety reasons
as well as to cool it down. To clean the refractometer in between analyzing
samples, Kim Wipes are used.
The primary equipment used to carry out the batch distillation is the
distillation rig. A seven-plate sieve-plate column is fitted into the distillation
column. To analyze the refractive index of the top and bottom products a
refractometer is used. Moreover, test-tubes, beakers, pipettes, and a pail are
used for measuring, containing liquids and to set up an ice-bath. As a safety
measure, face masks and goggles are worn.
The rig is run at atmospheric pressure (760 mmHg) and is also
maintained at a range of 70-80 C above the boiling point of methanol which
is at 64.7C. Heating power of 14(heater on 14% of the time) is kept
constant after the wanted temperature range is achieved. Cooling water flow
rate is adjusted to 120 L/hour. The reflux ratios and times at which the
samples are tested and the temperature is recorded is shown in Table 1
below.
Table 1: Reflux ratios at the respected times when temperature and
percentage mole of methanol is recorded
Reflux Time Details
ratio (min)
(%)
- ti Initial sample taken before distillation is conducted.
100 t1 After 15 minutes of reflux at 100%
60 t2 After 15 minutes of reflux at 60%
60 t3 After 30 minutes of reflux at 60%
60 t4 After 45 minutes of reflux at 60%
- tf Final samples taken at evaporator tank, reflux divider
vessel and top product container after distillation is
stopped.

3
3. Results

Percentage mole of methanol in Reflux Divider Vessel and Evaporator Tank taken at different times

100

90

80

70

Percentage moleRefux
of methanol (%)
divider vessel Evaporator tank

60

50

40

30
ti t1 t2 t3 t4 tf

Times at which samples are taken

Figure 1: Percentage mole of methanol in Reflux Divider Vessel and

Evaporator Tank taken at different times
(Based on data from Table 3)

4
 Temperature(C) against tray number in distillation column

78.0

76.0

74.0

72.0

Temperature
70.0

68.0

66.0

64.0
2 3 4 5 6 7 8 9 13

Tray number

t1 t2 t3 t4

Figure 2: Graph of temperature (C) against tray number in distillation column

(Based on data from Table 4)

Table 2: Temperatures of tray 10,11 and 12 at different times

Tray Number Temperature (C)
t1 t2 t3 t4
Tray 10 26.9 27.5 28.7 29.4

5
Tray 11 15.5 14.8 14.2 12.5
Tray 12 20.5 19.8 19.2 17.6

4. Discussion

4.1 Variation of composition of methanol with time in the reflux divider

vessel and evaporator
tank
Based on Figure 1shown above, the change in percentage composition of
methanol with time in both the reflux divider vessel and the evaporator tank
can be observed.
Overall, the percentage mole of methanol in the reflux divider vessel
is higher than that of the evaporator tank. This is due to the fact that
methanol is the more volatile component (MVC) and is therefore vaporized
and transferred to the top of the column.
As hypothesized, the percentage mole of methanol decreases with
time in both the reflux divider vessel and the evaporator vessel as
seen by the negative slopes of the graph. For the evaporator tank, the
percentage mole of methanol decreases from 53% to 36%. As time
progresses, more methanol is vaporized and less remains in the still of the
evaporator tank. Since the reflux ratio is kept constant, the overhead
composition varies. For the reflux divider vessel, percentage mole of
methanol decreases from 91% to 64%. This is because the composition of
the mixture in the top product is dependent on the composition of still in
evaporator tank. As the distillation operation runs, the liquid remaining in the
evaporator tank will become weaker in methanol, the MVC. As a result, the
purity of the top product will also steadily fall with time.
4.2 Temperature profile in the distillation column
The temperature profile of the distillation column at different times is plotted
in Figure 2. It can be seen from all the 4 graphs in Figure 2 that the
temperature decreases as the tray number increases when moving
up the column. The decrease in the temperature when progressing up the
column can be explained by the fact that the reboiler is located at the
bottom and the condenser is located at the top. Hence the bottom is at a
higher temperature whereas the top is at a lower temperature unlike the
expectation that the temperature should increase when going up the column
due to the vapours being at the top of the column.

6
Another observation made from the temperature profile in Figure 2 is the
relation between the temperature at the bottom and the LVC, isopropanol as
well as the relation between the temperature at the top and the boiling point
of the MVC, methanol. At any point in time, the temperature at the
bottom of the column is lower than the boiling point of
isopropanol(LVC) which is 82. 6C.This is to prevent the isopropanol from
vapourising. On the other hand, the temperature at the top of the
column is higher than the boiling point of methanol(MVC) which is
64.7C. This is to prevent the methanol from condensing.
However, it is also observed that there is an anomaly from tray 6 to 7
where the temperature increases and does not follow the general trend. It is
suspected that the equipment is faulty in between the two trays.
Exclusion of trays 10, 11 and 12 from the temperature profile is because
those trays do not indicate the temperature of the methanol-isopropanol but
instead indicate the temperature of the cooling water and condensate. As
can be seen in Table 2, the temperatures in trays 10,11 and 12 do not follow
the trend and are out of the normal temperature range which is from 70C to
80C. This is because the temperatures at those trays do not indicate the
temperature of the methanol-isopropanol but instead indicate the
temperature of the cooling water and condensate.
4.3 Discrepancies in the number of moles of methanol
Based on calculation carried out in appendix (Table 5), it is observed that the
total number of moles of methanol is not accounted for. In other
words, the initial number of moles of methanol does not equal to the final
number of moles of methanol. From the calculations carried out, the final
number of moles of methanol is less than the initial amount of moles of
methanol. The initial volume of mixture also does not tally with the
total final volume of mixture. There is approximately a 370ml difference
between the initial volume and the total final volume of the mixture.
With regards to the discrepancy in the number of moles of methanol, there
are a few possible causes. Firstly, evaporation of methanol occurred when
samples of the mixture were taken from the reflux divider vessel and the
evaporator tank. Evaporation of methanol was possible as the mixture was
exposed to air. Evaporation of samples taken from the evaporator tank is
also highly probable as the mixture was fairly hot and hence the methanol
evaporated into the air faster. The second cause of the discrepancy is that
some of the mixture was still retained in the evaporator tank, reflux divider
vessel, top product container and distillation column. The equipment was not
thoroughly drained of the mixture. The third cause was the inaccuracy of the
measuring equipment especially the beakers. Besides that, parallax error
might have occurred when recording the volume of the mixtures. This would

7
also explain the large discrepancy between the initial and total final volume
of the mixture.
4.4 Optimum number of stages and Efficiency of Distillation
In the experiment conducted, the number of trays used was seven.
To calculate the optimum number of stages, the McCabe method is used. The
vapor-liquid equilibrium x-y diagram for methanol-2-propanol at 1atm is first
plotted using the data given. The operating line is plotted on the graph to
obtain the number of optimum stages. The working for this is displayed in
the appendix. The optimum number of stages used based on the vapor-liquid
equilibrium x-y diagram for methanol-2-propanol at 1atm is 3. Therefore, the
number of actual stages used is more than the optimum number of
stages.
Efficiency= 3/7 x 100%
=43%

4.5 Method to increase yield and efficiency of distillation

In this experiment batch distillation was run at a constant reflux ratio of 60%.
This causes the overhead composition to vary. The efficiency of the operation
was calculated to be 43%. The efficiency and yield can be increased by
setting a desired purity for the top product. The reflux ratio is then
varied throughout the experiment to five a constant overhead composition.
As the operation progresses, the reflux ratio has to be continuously
increased. Amount of heat that has to be supplied increases when the reflux
ratio increases. There is a drawback to this method as the cost of heating will
be high when the reflux ratio is high. Therefore, the distillation is terminated
at a maximum economic reflux ratio, when still heat input cant sustain the
reflux ratio.

8
9
5. Conclusion
For a batch distillation of constant reflux ratio, it is observed that the
composition of the top product varies with time. MVC in the reflux divider
vessel and evaporator tank both decrease with time. Besides that, there is a
temperature gradient along the distillation column where the temperature
decreases going up the column as the reboiler is located at the bottom.
From various calculations performed it is determined that there is a
discrepancy in the number of volume of mixture and number of moles of
methanol. The difference between the initial and final volume of mixture and
number of moles of methanol is 370 ml and 11.6 moles respectively. It is
assumed that this is caused by evaporation of mixture and inaccuracy of
measuring equipment.
The optimum number of stages is calculated using the McCabe method and
found to be 3. Based on the optimum number of stages and actual number of
stages, the efficiency is calculated to be 43%.
The suggestion made to increase yield and efficiency is to set a desired
purity for the top product and to increase the reflux ratio to achieve this
standard of purity. However, the distillation is stopped when maximum
economic reflux ratio is reached.

10
6. References
i. McCabe, Warren L and Julian C Smith. Unit Operations Of Chemical
Engineering. New York: McGraw-Hill, 1976. Print.

ii. Richardson, J. F et al. Coulson And Richardson's Chemical

Engineering. Oxford: Butterworth-Heinemann, 2002. Print.

iii. Treybal, Robert Ewald. Mass-Transfer Operations. New York:

McGraw-Hill, 1980. Print.

iv. "Separation Processes Home Page". Separationprocesses.com.

N.p., 2016. Web. 25 Oct. 2016.

11
7. Appendix

Figure 3: A schematic representation of the distillation rig

Table 3: Percentage mole of methanol in the reflux divider vessel and the
evaporator tank at different times

Percentage mole of
methanol (%)
Reflux
divider
Sample Time vessel Evaporator tank
1 ti 53
2 t1 91 49
3 t2 79 48
4 t3 73 46
5 t4 71 43
6 tf 64 36

Table 4: Temperatures of trays taken at different times

12
 Temperature of trays taken at different
times

Tray t1 t2 t3 t4
2 73.9 75.4 75.8 75.9
3 72.4 75.3 75.3 76.2
4 71.0 75.0 75.0 75.9
5 70.2 74.7 75.0 75.6
6 67.8 73.5 73.9 74.5
7 67.9 74.2 74.4 75.5
8 66.9 73.7 74.0 74.6
9 66.5 73.3 73.7 73.8
13 65.1 72.1 72.8 72.7

Table 5: Calculation on the number of moles of methanol

(Refer to method of calculation for detailed steps)

13
 Mol Mol
es es
of of
Met Isop
han ropa
ol nol
Ti for a for a
m basi basi
e Loc s of s of
at ati 100 100
w on mol mol
hi s es es
ch fro of of M
sa m mixt mixt Ma Ma Mas as Mol
m whi ure( ure( ss Ma ss s s Ma es
pl ch take take of ss fra frac Den of ss of
es sa n n m of ctio tion sity Mi of me
ar mp fro fro et iso n of of xt Me tha
e les Vol Vol m m ha pro of isop mix ur tha nol
ta are um um perc perc no pan me rop ture e nol (m
ke tak e( e( enta enta l ol tha ano (kg/ (k (kg ole
n en ml) m3) ge) ge) (g) (g) nol l m3) g) ) s)
Init
ial
Vol
um
e
of
mi 0.3
xtu 16 75 0.6 788 4. 1.7 55.
re 98 28 45 245 .25 72 75 422
use 600 0.0 .1 24. 60 439 273 95 72 141
d 0 06 53 47 2 7 2 79 61 16 54 5
Sa ev
mp ap 0.3
les ora 16 75 0.6 788 0. 0.0 0.0
tak tor 0.0 98 28 45 245 .25 00 02 923
en tan 000 .1 24. 60 439 273 78 95 702
thr ti k 10 1 53 47 2 7 2 79 61 83 95 4
ou t1 refl
gh ux
out div 0.8
exp ide 29 43 0.1 791 0. 0.0 0.2
eri r 0.0 15 51 564 .06 00 06 145
me ves 10. 000 .6 54 40 859 108 81 87 097
nt sel 3 103 91 9 4 0.9 3 66 42 48 29 6
ev 18 0.0 49 51 15 30 0.3 0.6 788 0. 0.0 0.1
ap 000 69 65. 38 612 .03 01 04 499
ora 18 .9 1 71 859 228 41 80 537
tor 6 40 38 44 85 45 2

1
 tan
k 6
refl
ux
div 0.6
ide 25 67 0.3 790 0. 0.0
r 0.0 31 12 27 327 .00 00 05 0.1
ves 10. 000 .1 62. 82 217 366 82 53 727
sel 5 105 79 21 6 1 8 22 97 95 51 559
ev
ap 0.3
ora 15 29 0.6 787 0. 0.0 0.0
tor 0.0 37 31 80 701 .97 00 01 486
tan 000 .9 25. 49 950 882 47 55 665
t2 k 6 06 48 52 2 2 4 63 96 28 93 4
refl
ux
div 0.5
ide 23 90 0.4 789 0. 0.0 0.1
r 0.0 38 16 39 096 .54 00 04 498
ves 10. 000 .9 22. 48 051 236 81 80 520
sel 3 103 73 27 2 7 4 62 9 32 13 6
ev
ap 0.3
ora 14 12 0.6 787 0. 0.0 0.1
tor 0.0 73 32 30 876 .87 01 04 535
tan 000 .8 45. 45 954 382 57 92 933
t3 k 20 2 46 54 4 4 2 76 71 57 11 6
refl
ux
div 0.5
ide 22 66 0.4 789 0. 0.0 0.1
r 0.0 74 17 19 338 .39 00 04 464
ves 10. 000 .8 42. 89 010 719 82 69 742
sel 5 105 71 29 4 9 1 92 34 89 3 9
ev
ap 0.2
ora 13 86 0.7 787 0. 0.0
tor 0.0 77 34 82 131 .72 00 01 0.0
tan 000 .7 25. 06 793 092 55 58 493
t4 k 7 07 43 57 2 7 4 6 38 14 15 615
tf refl
ux
div 0.4
ide 20 86 0.5 788 0. 0.0 0.9
r 0.0 50 21 58 134 .91 06 30 584
ves 000 .5 63. 80 119 952 31 71 989
sel 80 8 64 36 6 6 7 26 84 14 03 6
top 100 0.0 79 21 25 12 0.6 0.3 790 0. 0.5 16.
- 0 01 31 62. 67 327 .00 79 27 452

2
 pro 27
du .1 82 217 366 00 15 942
ct 6 1 8 22 97 04 23 8
ev
ap 0.2
ora 11 30 0.7 787 3. 0.8 25.
tor 0.0 53 38 69 693 .38 50 08 228
tan 445 044 .4 46. 53 046 417 38 32 596
k 0 5 36 64 4 4 8 18 23 6 42 2
Tot
al
of
sa
mp
les
tak
en
thr
ou
gh
out
exp 43.
eri 817
me 563 575
nt 2.6 3

Difference in volume=6000-5632.6
=367.4ml

Difference in moles of methanol=55.42-43.82

=11.6 moles