FACULTY OF ENGINEERING

DEPARTMENT OF CHEMICAL AND ENVIRONMENTAL ENGINEERING

UNIVERSITI PUTRA MALAYSIA

ECH3904 CHEMICAL ENGINEERING LABORATORY II

EXPERIMENT 11 & 12: Distillation Process

LECTURER: DR MUS'AB ABDUL RAZAK

DEMONSTRATOR: En. Abdul Raheem Channa

TECHNICIAN: En. Ismail Abdullah

PREPARED BY GROUP S2G2:

Nur Atiqah binti Mustapha 167151

Muhammad Danial bin Muhammad Rais 168709

Tan Hua Jian 169690

Aminur Rasyid bin Ahmad Zaini 169965

DATE PERFORMED: 4/29/2014

DATE SUBMITTED: 4/25/2020 15:14 a4/p4 (Do not change)

1. Abstract

The experiment is divided into two parts. First, sieve tray distillation at total reflux
condition and second is batch distillation with constant reflux and variable distillate composition.
The objectives for the first part are to determine the overall tray efficiency at total reflux
condition and to study the effect of liquid and vapor loading on overall tray efficiency at total
reflux. For the second part, the objective is to study the operation of a batch distillation column
with constant reflux and variable distillate composition. The experiment was started with
preparing a refractive index test on mixtures of different ratio of water-methanol. A RI against
methanol composition graph is plotted. Next, we collected product samples from top (distillate)
and bottom (reflux) at different power settings of heater that is at 80, 90 and 100 %. Next, the
experiment was conducted by taking the samples every 5 minutes intervals in 40 minutes. Based
on refractive index for bottom and distillate at constant reflux ratio of 5, the number of moles of
methanol present in each sample is determined using the RI against composition plot. Then, the
values obtained are transferred to plot x-y diagram for McCabe-Thiele Method to find the
theoretical tray of distillation column. The maximum efficiency of tray is 38% at heater power of
100% and the minimum overall efficiency tray is 30% which at 90% of heater power.

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2. Result and Discussions

2. Results and Discussion

Sieve Tray Distillation at Total Reflux

Power setting Number of Theoretical number Actual number of Overall tray

(%) heater of trays trays efficiency (%)
80 2 3.6 10 36.0
90 2 3.0 10 30.0
100 2 3.8 10 38.0
Table 1: Theoretical number of trays and overall tray efficiency with different heater power
setting

Distillation is a process of separating components from a liquid mixture through

vaporization and condensation processes when the components have different volatility. In this
experiment, two heaters are used throughout the process to heat water-methanol mixture to
obtain the overall tray efficiency of the distillation column. The distillate temperature is 63.9 ̊ C
which is close to the light key component (methanol) with boiling point of 65 ̊ C. This explains
why the distillate sample is almost pure methanol. However, there is still a little water in the
distillate as evaporation of water happens at any temperature.

Graph of Overall Tray Efficiency against Power

Setting
40
38
Overall tray efficiency (%)

36
34
32
30
28
26
24
22
20
80 90 100
Power Setting (%)

Figure 1 Graph of Overall Efficiency against Power

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 Based on Figure 1, the overall tray efficiency of the distillation process fluctuated with
the power setting. The highest efficiency obtained from the experiment is 38% where the power
setting is at 100%. The number of actual trays is 10 but the number of theoretical trays obtained
is much lesser than that which is 3.8.

The results fluctuated due to the high volatility of methanol. When the sample is
transferred to the refractometer, some methanol might evaporate and loss to the surrounding. The
refractive index reading might be inaccurate due to the residue left in the dropper and
refractometer. Although the liquid mixture is heated with 100% power setting, the solution
temperature doesn’t rise up till targeted temperature, the temperature is maintained when the
system reach steady state.

Batch Distillation with Constant Reflux

Number of Theoretical Actual number Overall tray

heater number of trays of trays efficiency (%)

Starting 2 3.75 10 37.5

5min 2 3.80 10 38.0
10min 2 7.40 10 74.0
15min 2 7.25 10 72.5
20min 2 3.80 10 38.0
25min 2 3.90 10 39.0
30min 2 4.85 10 48.5
35min 2 4.50 10 45.0
40min 2 5.50 10 55.0
Table 2: Theoretical number of trays and overall tray efficiency under constant reflux

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 Graph of Overall tray efficiency against Time
80
70
Overall Tray Efficiency (%)

60
50
40
30
20
10
0
0 5 10 15 20 25 30 35 40
Time (min)

Figure 2 Graph of
Overall Efficiency against Time

Based on Figure 2, there is some inconsistency in the results as the efficiency is

fluctuating throughout the experiment. The efficiency is almost similar as in the total reflux. This
might be due to some similar error as discussed earlier that affected the result.

For constant reflux ratio, the R is kept constant and distillation is continued until the
distillate composition dropped below a certain pre-specified level. However, the result obtained
from the raw data shows the opposite result. The problem arises because the distillate is not
cleared off each time we collect the sample. This might cause accumulation of methanol in the
distillate. However, the concentration of reflux is decreasing steadily with time. This is because
more and more methanol is evaporated and condensed in the reflux drum to make up the
distillate. The mixture is boiled slowly and the vapor is withdrawn as rapidly as they form in the
condenser where the condensed vapor or distillate is collected. The first portion of vapor
condensed will be richest in the more volatile methanol.

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3. Conclusion and Recommendations

From the data collection, the theoretical tray is determined through McCabe-Thiele
method by using equilibrium curve methanol-water (x-y plot). The overall tray efficiency at
total reflux does not achieved 100%. The maximum efficiency of tray is 38% at heater power of
100% and the minimum overall efficiency tray is 30% which at 90% of heater power. Based on
refractive index for bottom and distillate at constant reflux ratio of 5, the number of moles of
methanol for each sample is determined using the refractive index against composition plot.
Then, the values are later used to find the number of theoretical trays.

There are some recommendations that needed in this experiment. Since the vapor of
methanol solution are potentially irritants on eye and respiratory, hence the experiment could be
performed under a fume cupboard to prevent any unexpected accidents. Next, set time for sample
to be collected in 30 minutes after start-up as the system takes time to approach stabilization.
Carefully clean the refractometer after each reading to reduce the error. The U-tube holding the
distillate should be emptied at each interval to avoid accumulation.

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4. Raw Data Sheet

Vmethanol (ml) Vd (ml) Refractive Index

0 10 1.34289
2 8 1.34713
4 6 1.35023
6 4 1.34996
8 2 1.34603
10 0 1.33511
Table 1: Refractive Index of Various set of Water-Methanol mixture (Standard)

nMethanol (mol) nwater (mol) xMethanol xwater

0 0.556 0 1
0.049 0.444 0.099 0.901
0.099 0.333 0.229 0.771
0.148 0.222 0.4 0.6
0.198 0.111 0.641 0.359
0.247 0 1 0
Table 2: Molar composition of Water and Methanol in mixture

Power of heater Refractive x (mol) of Refractive x (mol) of

(%) Index,RI for bottom Index for distillate
bottom column methanol distillate methanol
column
80 1.34797 0.12 1.33735 0.94
90 1.34728 0.11 1.33851 0.90
100 1.34723 0.11 1.33759 0.93
Table 3: Refractive index, RI and number of mole for bottom and distillate at different heater power (%).

Refractive x (mol) of Refractive x (mol) of

Index, RI of bottom Index, RI of distillate
Bottom methanol Distillate methanol
Starting 1.34921 0.162 1.33717 0.940
5min 1.34900 0.160 1.33658 0.952
10min 1.34879 0.150 1.33566 0.990
15min 1.34882 0.152 1.33608 0.988
20min 1.34896 0.158 1.33680 0.950
25min 1.34894 0.157 1.33642 0.946
30min 1.34892 0.156 1.33623 0.970
35min 1.34893 0.156 1.33635 0.960
40min 1.34888 0.153 1.33613 0.975
Table 4: Tabulated data of refractive index, RI for bottom and distillate at constant reflux ratio of 5.

5. Sample Calculation

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For experiment 11:

g
Density of water = 1
ml

g
Density of methanol = 0.7918
ml

g
Molecular weight of water = 18.02
mol

g
Molecular weight of methanol = 32.04
mol

g
(10 ml)(0.7918 )
ml
Mole , n Methanol=
g
32.04
mol

¿ 0.247 mol

Experiment 11&12:

Overall tray efficiency:

N theoretical
Eo =
N actual

At 90% of power heater:

3.0
Eo = x 100%
10

¿ 30 %

In percentage, the overall tray efficiency, Eo at the power heater of 100% is 38.0%.

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 McCabe-Thiele Tray Method
1.0

0.9

0.8

0.7

0.6

0.5
y

0.4

0.3

0.2

0.1

0.0
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0

Figure 2: McCabe-Thiele Tray Finding Method at Total Reflux at Power Setting 90%