CEV452 Lab 2 Distillation Column
CEV452 Lab 2 Distillation Column
CEV452 Lab 2 Distillation Column
0 ABSTRACT
This experiment is conducted to study the effect of feed temperature on the number of
theoretical plates in a continuous distillation operating at constant reflux 2:2. The SOLTEQ
Bubble Cap Distillation Unit (Model: BP 681-80) was used to commence the experiment.
Generally, this unit was used for the separation of mixtures at atmospheric pressure in a
continuous operation. The desired feed temperature for this experiment is 25 ⁰C and 27 ⁰C and
the reflux ratio used was at 2:2. When the unit achieved the desired temperature, samples from
distillate and bottom product was taken. Refractive index (RI) readings are used to determine
the composition of ethanol-water mixture. Calibration curve of RI obtained is directly
proportional to the composition for the whole range of mixture. For distillation at reflux ratio of
2:2, the refractive index obtained for distillate and bottom are 1.3380 and 1.3298. The molar
composition for distillate (XD) and bottom (XB) obtained are approximately 17.97 and 4.76. From
the Figure 2 in the result, it is shown that the theoretical plate obtained is approximately 1. For
distillation at reflux ratio of 2:2, the refractive index obtained for distillate and bottom are 1.3356
and 1.304. The molar composition for distillate (XD) and bottom (XB) obtained are approximately
14.58 and 0. From the Figure 3 in the result, it is shown that the theoretical plate is
approximately 1.5. As for conclusion, The feed temperature at 25 ⁰C and 27 ⁰C does affect the
number of theoretical plates in a continuous distillation operating at constant reflux 2:2 where
the theoretical plate obtained is approximately 1. The recommendations for improvement of this
study are, firstly, use lower temperature as a variations for data collection as the unit took quite
some time to calibrate and achieved desired feed temperature. Secondly, make sure the
beakers are properly labeled when taking samples from the unit to avoid error in data analysis.
Thirdly, take more than one reading during data collection in order to get the optimum result.
2.0 INTRODUCTION
Distillation is a liquid-liquid separation process and can be carried out in a continuous or batch
system. Removal of heat is used to exploit differences in relative volatility in distillation. The
components with lower boiling points and higher volatility will vaporize and leaving less volatile
components as liquids (“Distillation Columns,” n.d). High relative volatilities mixtures are easier
mixtures can be separate using distillation. Variables such as column pressure, temperature,
size, and diameter can be determine by the properties of the feed and the desired products.
Continuous distillation is where the liquid mixture of two or more miscible components is
continuously fed into the process and physically separated into two or more products by
preferentially boiling the more volatile, which has lower boiling point components out of the
mixture. In a large scale, continuous distillation is used in the chemical process industries where
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large quantities of liquids have to be distilled. For example, as in petroleum refining, natural gas
and the liquefaction of gases such as hydrogen, oxygen, nitrogen, and helium.
Continuous distillation happens when a liquid mixture is heated until it boils. The evolved
vapor will have a higher concentration of the more volatile, lower boiling point components than
the liquid mixture from which it evolved (“Continuous Distillation,” n.d). The less volatile
components tend to condense in a greater proportion than the more volatile components when
a vapor mixture is cooled. Figure 1 shows a schematic illustrate about what happens in a
distillation column. A liquid mixture is fed into the distillation column. The heated feed is partially
vaporized and rises up on entering the column. As it rises, it is cools by contacting the
descending cooler liquid and partially condenses. While part of vapor continues to flow upward,
the condensed portion is enriched in the less volatile component and flows downward. As the
vapor continues to flow upward, it undergoes partial condensation a few times and each time it
becomes richer in the more volatile component. Parts of the feed liquid that did not vaporize on
entering the column will flows downward and is heated by contacting the upward flowing hot
vapor until it is partially vaporized. The resulting vapor flows upward and the residual liquid is
enriched in the less volatile component and flows downward. As the liquid continues to flow
downward, it undergoes partial vaporization a few times and each time it becomes richer in the
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Figure 1: Schematic diagram of a continuous binary distillation column
3.0 OBJECTIVE
To study the effect of feed temperature on the number of theoretical plates in a
4.0 THEORY
Various vapor and liquid contacting methods are uses to provide the required number of
are known as “plates” or “tray”. Each of these plates or trays have different temperature and
pressure. The tower bottom stage has the highest temperature and pressure. The temperature
and pressure decreases as the height of the tower increases. The vapor-liquid equilibrium for
each feed component in the tower are adjust to the different pressure and temperature
conditions at each of the stages so that each component establishes a different concentration in
the vapor and liquid phases at each stages and will results in the separation of the components.
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Figure 2: A distillation column with a bubble-cap trays
Reboiler acts as an additional theoretical equilibrium stage. The number of physical trays
needed for a given separation is equal to the number of theoretical equilibrium stages or
theoretical plates if each physical tray or plate were 100% efficient. Usually, a distillation column
needs more actual plates than the required number of theoretical vapor-liquid equilibrium
stages.
the vapor between trays is well-mixed, has uniform composition and the liquid in the
downcomers is well-mixed, has uniform composition and the liquid on the tray is well mixed and
has the same composition as the liquid in the downcomer leaving the tray. It is defined for each
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tray according to the separation achieved on each tray. It is based on either the liquid phase or
the vapor phase. A given component is equal to the change in actual concentration in the
phase, divided by the change predicted by equilibrium condition. The Murphree Tray Efficiency
𝑦 𝑛 − 𝑦 𝑛 +1
Vapor phase: EMV =
𝑦 𝑛∗ − 𝑦 𝑛 +1
𝑥 𝑛 − 𝑥 𝑛 +1
Liquid phase: EML =
𝑥 𝑛∗ − 𝑥 𝑛 +1
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5.0 APPARATUS
Figure 1: Process flow diagram for the bubble cap distillation unit.
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Column trays Distillate
sampling
Reboiler Bottom
sampling
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Figure 3: Field unit controller.
Figure 1 shows the process flow diagram of bubble cap distillation unit (BP 681-80). The flow
diagram has been state clearly about the process of distillation unit. There are reboiler (B1)
which contain 20 kW electrical cartridge heaters. The unit also contain bubble cap column (K1)
which is 10 plates, silver coated and vacuum jacketed. The unit also contain top condenser
(W2) with cooling water connected to the unit. The feed vessel (B2) was installed to the unit for
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Figure 3 show the field unit controller of bubble cap distillation unit. The TT-101 until TT-
110 indicate the tray temperatures. The TIC-111 are for reboiler temperature controller. The TT-
112 indicate the distillate temperature and TIC-113 are indicate the feed temperature control for
this system.
6.0 PROCEDURE
Start-up Procedure
4. The reflux divider (KFS-101) was set to total reflux which is no. 2.
6. The cartridge heaters was switched on and allowing the ethanol solution to boil.
3. The reflux ratio was set to 1:1 (No. 3) and constant throughout the process.
4. The heater W5 was turned on to preheated the feed of ethanol-water to desired temperature
which is 25 ⁰C.
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5. Valve V7 was opened partially to let the flow out of the system.
6. The system was let until the inlet temperature are constant at desired temperature.
8. The Process was repeated with different inlet temperature which is 27 ⁰C.
Sampling Procedure
1. Distillate sampling:
3. The reflux divider (KSF-101) was set to distillate off take (No. 1) for a few seconds.
4. Valve V11 was opened and 5-10 ml of samples was collected and the valve was
closed.
5. The reflux divider was switched back to original setting (No. 3).
2. Bottom sampling:
3. Valve V8 was fully opened and V7 was partially opened, 5-10 ml samples were
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Composition Analysis of Ethanol in Concentrated samples procedure.
1. 10 ml of measuring cylinder was placed on a weighing scale and the scale was set to zero.
2. By using a dropper, 1 to 2 g of samples were transferred into the measuring cylinder and the
3. Water was added into the measuring cylinder to dilute the sample and obtaining a total
4. The diluted solution was mixed well before measuring its refractive index (RI).
5. The diluted solution’s composition was obtained from the calibration curve.
1. A set of mixtures containing ethanol and water was prepared within a specified range of
2. The refractive index reading was obtained for each mixture using a refractometer.
3. The calibrating curve of RI versus composition for the whole range of mixtures was plotted.
4. The calibrating curve was used to determine the diluted samples solution’s composition of the
distillation process.
7.0 RESULT
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Density of ethanol: 789 kg/m3
1.36
1.355
Refractive Index (RI)
1.35
1.345
1.34
1.335
1.33
1.325
0 2 4 6 8 10 12
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B: Number of theoretical plates at constant reflux using x-y equilibrium diagram
Reflux ratio: 2:2 @ temperature : 25 ⁰C
Diluted Actual
Temperature Sample Solution Refractive solution’s sample’s
Tray (°C) weight (g) weight index composition composition
(g) (wt%) (wt%)
90
80
mole % ethanol in vapor (y)
70
60
50
40
30
20
10
0
0 10 20 30 40 50 60 70 80 90 100
xB xD
mole % ethanol in liquid (x)
Diluted Actual
Temperature Sample Solution Refractive solution’s sample’s
Tray (°C) weight (g) weight index composition composition
(g) (wt%) (wt%)
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C. Murphree efficiency for each tray in the column
90
80
mole % ethanol in vapor (y)
70
60
50
40
30
20
10
0
0 10 20 30 40 50 60 70 80 90 100
80
70
60
50
40
30
20
yn+1 10
yn 0
0 10 20 30 40 50 60 70 80 90 100
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𝑦𝑛 − (𝑦𝑛+1 )
Em =
𝑦 ∗𝑛 − (𝑦𝑛+1 )
18 − (5)
Em =
18 − (5)
Em = 1
90
80
mole % ethanol in vapor (y)
70
60
50
40
30
20
yn+1 10
yn 0
0 10 20 30 40 50 60 70 80 90 100
𝑦𝑛 − (𝑦𝑛+1 )
Em =
𝑦 ∗𝑛 − (𝑦𝑛+1 )
17 − (1)
Em =
17 − (1)
Em = 1
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8.0 SAMPLE CALCULATIONS
kg
Weight of ethanol g = amount of ethanol mL × density
m3
kg 1𝐿 1 𝑚3
= 1.0 mL × 789 m3
× 1000 𝑚𝐿 × 1000 𝐿
= 0.000789 kg
kg
Weight of water g = amount of water mL × density ( )
mL
kg 1𝐿 1 𝑚3
= 9.0 mL × 1000 m3
× 1000 𝑚𝐿 × 1000 𝐿
= 0.009 kg
weight of ethanol
Weight percent of ethanol = × 100%
weight of ethanol + weight of water
0.000789 kg
= × 100%
0.000789 +0.009 kg
= 8.0601%
0.000789 kg 1000 𝑔
= g ×
46.07 ( mol ) 1 𝑘𝑔
= 0.01713 mol
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weight of water (kg)
Mole of water mol =
kg
molecular weight ( mol)
0.009 kg 1000 𝑔
= g × 1 𝑘𝑔
18.02 ( mol )
= 0.499 mol
mole of ethanol
Mole percent of ethanol = mole of ethanol +mole of water
×100%
0.01713 mol
= 0.01713 +0.499 mol
×100%
= 3.3153%
3. XD calculations
𝑥𝐷 = 17.96
4. XB calculations
𝑥𝐵 = 17.96
9.0 DISCUSSION
or more miscible components is continuously fed into the process and physically separated into
two or more products by preferentially boiling the more volatile components out of the mixture.
In this particular experiment, this process is operating at constant feed temperature at 25 ⁰C and
27 ⁰C as we need to study the effect of constant reflux ratio on the number of theoretical plates
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Based on the experiment A, refractive index (RI) readings are used to determine the
composition of ethanol-water mixture. Figure 1 shows that the calibration curve of RI is directly
proportional to the composition for the whole range of mixture. For distillation at reflux ratio of
2:2, the refractive index obtained for distillate and bottom are 1.3380 and 1.3298. The molar
composition for distillate (XD) and bottom (XB) obtained are approximately 17.97 and 4.76. From
the Figure 2, it is shown that the theoretical plate obtained is approximately 1. For distillation at
reflux ratio of 2:2, the refractive index obtained for distillate and bottom are 1.3356 and 1.304.
The molar composition for distillate (XD) and bottom (XB) obtained are approximately 14.58 and
0. From the Figure 3, it is shown that the theoretical plate is approximately 1.5. The Murphree
efficiency for both reflux ratio is the same unfortunately. This is due to insufficient amount of
data to allocate the value of y*n. Besides, the temperature and composition profile versus tray
10.0 Conclusion
The feed temperature at 25 ⁰C and 27 ⁰C does affect the number of theoretical plates in a
continuous distillation operating at constant reflux 2:2 where the theoretical plate obtained is
11.0 Recommendation
1) Use lower temperature as a variations for data collection as the unit took quite some time to
2) Make sure the beakers are properly labeled when taking samples from the unit to avoid error
in data analysis.
3) Take more than one reading during data collection in order to get the optimum result.
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12.0 REFERENCES
1. Chang, H., Lin, T., Chan, H., Ho, C., & Cheng, T. (2017). Experimental and optimization
2. Chen, H., Zhang, L., Huang, K., Yuan, Y., Zong, X., Wang, S., & Liu, L. (2016). Reactive
distillation columns with two reactive sections: Feed splitting plus external
http://dx.doi.org/10.1016/j.cep.2016.08.008
3. Delgado, J., Águeda, V., Uguina, M., Sotelo, J., García-Sanz, A., &García, A. (2015).
Separation of ethanol–water liquid mixtures by adsorption on BPL activated carbon with air
http://dx.doi.org/10.1016/j.seppur.2015.06.011
4. Dhole, V., &Linnhoff, B. (1993). Distillation column targets. Computers & Chemical
extractive batch dividing wall distillation column. Chemical Engineering And Processing:
6. Springer, P., Baur, R., & Krishna, R. (2003). Composition Trajectories for Heterogeneous
Page | 20
7. Zhao, L., Lyu, X., Wang, W., Shan, J., &Qiu, T. (2017). Comparison of heterogeneous
http://dx.doi.org/10.1016/j.compchemeng.2017.02.007
8. Seader, J.D & Henley, E.J. (1998). Distillation of Binary Mixtures. John Wiley & Sons Inc.,
http://faculty.kfupm.edu.sa/CHE/binoushousam/files/Introduction%20to%20distillation.pd
10. The Separation of a Binary Water/Ethanol Solution via a Continuous Feed Distillation
Column as a Function of Feed Stage Location and Reflux Ratio. (2015). International
http://dx.doi.org/10.21275/v4i12.nov152084
11. Geankopolis C. J. (2014). Transport Process & Separation Process Principles (includes Unit
Page | 21
13.0 APPENDICES
𝑦𝑛 − 𝑦𝑛+1
Em =
𝑦 ∗𝑛 − 𝑦𝑛+1
Where,
𝑦𝑛 is the average actual concentration of the mixed vapor leaving the tray n
𝑦𝑛+1 is the average actual concentration of the mixed vapor entering tray n
𝑦 ∗𝑛 the concentration of the vapor that would be in equilibrium with the liquid of
concentration leaving the tray to the downcomer
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