Experiment 3 BKF3731 Unit Operation Laboratory

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1.0 ABSTRACT
This experiment is to study the effects of stirrer speed and temperature on the efficiency
of ethylene glycol-water separation in a short path distillation. The objectives of this
experiment are to study on the effects of the parameters on the thermal separation
efficiency using short path distillation. For this experiment, it is divided to 2 parts. Firstly
is test about the factor of stirrer speed and secondly is test about effect of temperature.
For part 1, ethylene glycol and water with a ratio of 5:5 at total of 1 litre is mixed and
stirred. Thermostat is set on 70 C, chiller at 12C, and vacuum pump at 250mbar. Then,
the stirrer and feed pump is on and set to 50rpm. After 5 minute, the volume of distilled
from V-104 and volume of concentrated V-105-107 is recorded. The experiments is
repeated by using 100rpm, 200 rpm and 220rpm. For the second part, the experiment is
test about the effect of temperature. The stirrer speed is maintained at 220rpm, the contact
time is 5 minutes and the vacuum pressure is 100mbar while ethylene glycol and water
with a ratio of 7:3 at total of 1 litre is mixed and stirred. Then the evaporator is set on
70 C. . After 5 minute, the volume of distilled from V-104 and volume of concentrated
V-105-107 is recorded. The experiments is repeated by changing temperature to 72C,
74C, 76C and 80C. Then we can calculate the separation efficiency. From the result,
graph of Separation Efficiency (%) against Stirrer Speed (rpm) and Separation Efficiency
(%) against Temperature (C) is plotted. From the graph, we can conclude that the higher
the stirrer speed and temperature, the higher the separation efficiency. When the stirrer
speed increased from 50 rpm to 220 rpm, the separation increased from 99.63% to
99.76%. While when the temperature increased from 70C to 80C, the separation
efficiency increased from 99.76% to 99.79%. Therefore, effects of stirrer speed and
temperature will affect the efficiency of ethylene glycol-water separation in a short path
distillation.








Experiment 3 BKF3731 Unit Operation Laboratory
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2.0 METHODOLOGY FLOWCHART





























Ethylene glycol and water are mixed
with a ratio of 5:5 at total of 1 litre in
a beaker.
The mixture is then stirred
homogeneously
Ensure that all the valves are initially
closed
The cold trap is filled with ice
Ethylene glycol and water mixture is
preheated to 50C
Switch ON the main power supply of
the control panel
Set thermostat at 70C and vacuum
pump pressure at 250mbar
To adjust the desired stirrer speed,
adjust knob button at stirrer
On the feed pump and set it to 10rpm
and on stirrer to desired speed
Run every set of experiment for 5
minutes and record the distillate
volume, concentrate volume,
composition of Ethylene glycol in
each distillate and concentrate in table
Repeat the experiment with different
operating parameters as shown in
result and discussion
Shut down the equipment by
following the operating procedure


Experiment 3 BKF3731 Unit Operation Laboratory
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3.0 RESULTS
3.1 Effect of stirrer speed
Vacuum pressure, PT-200 250mbar
Evaporator Temperature, TT-100 70C
Fed Flow Rate 19.656 ml/min
Contact time 5 min
EG-water ratio 5:5

3.2 Effect of evaporator temperature
Vacuum pressure, PT-200 250mbar
Stirrer speed, M-500 220 rpm
Fed Flow Rate 19.656 ml/min
Contact time 5 min
EG-water ratio 5:5
Time
Start
Stirrer
Speed
(rpm)
Distillate Concentrate Separation
Efficiency
(%)
Volume
(ml)
Composition
(%)
Volume
(ml)
Composition
(%)
1405 50 6.5 3.0 90 57.6 99.63
1410 100 8 2.4 95 58.6 99.66
1415 200 11 1.6 92 59.8 99.68
1420 220 11 1.2 90 60.0 99.76
Time
Start
Temp.
(C)
Distillate Concentrate Separation
Efficiency
(%)
Volume
(ml)
Composition
(%)
Volume
(ml)
Composition
(%)
1425 70 11 1.2 90 60.0 99.76
1430 72 11 1.2 92 62.0 99.77
1435 74 11 1.2 93 63.6 99.78
1440 76 11 1.2 94 65.0 99.78


Experiment 3 BKF3731 Unit Operation Laboratory
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4.0 DISCUSSION
In order to calculate the separation efficiency at different operating conditions, we use
this formula (H.B Moller, S.G. Sommer, B.K. Ahring):





x 100

Example 1:
Calculating the Separation efficiency at 220 rpm, 70C,
Separation Efficiency =

x 100
= 99.76%

To obtain the mass of Ethylene glycol in the mixture, we use this formula:




Example 2:
Calculating the mass of Ethylene glycol in 6.5 ml of distillate
Mass of Ethylene glycol = 6.5 ml x 1.0791g/ml x 0.03
= 0.21g
Density of the mixture which is 5:5 Ethylene glycol and water is 1.0791. (Ali Eliassi and
Hamid Modarress)





1445 80 11 1.2 95 67.6 99.79


Experiment 3 BKF3731 Unit Operation Laboratory
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99.60
99.62
99.64
99.66
99.68
99.70
99.72
99.74
99.76
99.78
0 50 100 150 200 250
S
e
p
a
r
a
t
i
o
n

E
f
f
i
c
i
e
n
c
y

(
%
)

Stirrr Speed (rpm)












Figure 4.1: Separation Efficiency (%) against Stirrer Speed (rpm)

Figure 4.1 show the relationship between the stirrer speeds with the separation
efficiency under a constant temperature which is 70 C. When the stirrer speed is
increased from 50 rpm to 100 rpm, the separation efficiency increased from 99.63% to
99.66%. The stirrer speed was then increased to 200 rpm and the separation efficiency
also increased to 99.68. Last but not least the stirrer speed was then set to 220 rpm and
the separation efficiency also increase to 99.76%. Hence we can say that the separation
efficiencies increase when the stirrer speeds are increased and the separation efficiencies
increased because of the composition of ethylene glycol in the concentrate increase while
the composition of ethylene glycol of distillate decrease as the stirrer speed increase.
Short path distillation will also affected by the change of pressure. Short path
distillation is a distillation technique that usually carried out at reduced pressure. (
Michael Albers, Alzenau-Hrstein) Hence if the pressure is increased, the performance of
the short path distillation unit will be lower as the mixture need a higher temperature to
be separated. The higher the pressure, the higher the temperature needed for a liquid to
achieve boiling point.



Experiment 3 BKF3731 Unit Operation Laboratory
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99.75
99.76
99.76
99.77
99.77
99.78
99.78
99.79
99.79
99.80
99.80
68 70 72 74 76 78 80 82
S
e
p
a
r
a
t
i
o
n

E
f
f
i
c
i
e
n
c
y

(
%
)

Temperature (C)












Figure 4.2: Separation Efficiency (%) against Temperature (C)
Figure 4.2 show the relationship between the temperatures with the separation
efficiency with the stirrer speed set as constant at 220 rpm. When the temperature
increased from 70C to 80C, the separation efficiency increased from 99.76% to
99.79%. At temperature 74C and 76C, we can see that the separation efficiency remain
the same although the composition of ethylene glycol in the concentrate increase and the
composition of ethylene glycol of distillate decrease. The increase in temperature only
cause a slight increase in separation efficiency. From here we can say that the higher the
temperature the higher the separation efficiency and the increase in the separation
efficiency affected by temperature is more drastic compare to the increase in the
separation efficiency that cause by stirrer speed.
The higher the temperature, the higher the separation efficiency. This is because
in higher temperature, the kinetic energy of particles is higher. This will produce more
collision per unit time between the reactant particles. (H.B Moller, S.G. Sommer, B.K.
Ahring) Therefore the efficiency collision frequency will increase hence increase the
separation efficiency in short path distillation.



Experiment 3 BKF3731 Unit Operation Laboratory
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5.0 CONCLUSION AND RECOMMENDATION
As a conclusion, temperature and stirrer speed is the parameter that affects the
efficiency on the thermal separation. This was proven from Figure 4.1. When the stirrer
speed was increased from 50 rpm to 220 rpm, the separation increased from 99.63% to
99.76%. Besides, from Figure 4.2, when the temperature increased from 70C to 80C,
the separation efficiency increased from 99.76% to 99.79%. Therefore, effects of stirrer
speed and temperature will affect the efficiency of ethylene glycol-water separation in a
short path distillation. The faster the stirrer speed, the higher the separation efficiency,
and the higher the temperature, the higher the separation efficiency.
As recommendation, we must ensure the accuracy of stirrer speed and reduce the
lagging time for the stirrer to be at their exact speed. Besides, the RI meter which we use
to determine the composition of Ethylene glycol must be cleaned with soft tissue every
time after use to prevent inaccurate reading. The valve of chiller must opened to balance
the pressure in the chamber to prevent the distillate and concentrate undergo backflow.
The Ethylene glycol mixture must be also handled with care as it is quite corrosive to
human body.

6.0 REFERENCE
1) Christie John Geankoplis, Transport Processes and Separation Process Principles,
4
th
Edition
2) H.B Moller, S.G. Sommer, B.K. Ahring , Separation efficiency and partice size
distribution in relation to manure type and storage conditions
3) Ali Eliassi and Hamid Modarress, Densities of Poly(ethylene glycol)+Water
mixtures in the298.15-328.15 K Teperature Range
4) Michael Albers, Alzenau-Hrstein, 2012, Application of Short-Path Distillation
for Processing Edible Oils and Fats, Retreived from
http://www.dgfett.de/meetings/archiv/leipzig/abstract_ albers.pdf at 17th April
2012


Experiment 3 BKF3731 Unit Operation Laboratory
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7.0 APPENDICES
To calculate Feed Flow Rate (ml/min)
Distillate Concentrate Average = (Distillate + Concentrate)/5
6.5 90 19.3
10 95 21
11 92 20.6
11 90 20.2
11 90 20.2
11.5 60 14.3
12 93 21
12.5 88 20.1
13 88 20.2

Total 176.9

Average 19.656