1.

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

to separate. Separations of close-boiling and azeotropic feeds will be difficult so special

distillation techniques is needed to separate these mixtures. Binary and multi-component

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

processing, petrochemical production, hydrocarbon solvents production, coal tar processing,

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

less volatile component.

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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

continuous distillation operating at constant reflux.

4.0 THEORY

Various vapor and liquid contacting methods are uses to provide the required number of

theoretical equilibrium stages in distillation columns(“Continuous Distillation,” n.d). The devices

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.

Figure 2 shows example of trays.

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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 Murphree Tray Efficiency, EM is based on a semi-theoretical models that assumes

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

can be calculated by using the equation below:

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

Feed Vessel for

continuous
system. Outlet vessel for
distillate product

Reboiler Bottom
sampling

Outlet vessel for

bottom product

Figure 2: Bubble cap distillation column unit.

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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

the continuous process.

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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

Pump and Pressure.

1. All valves were closed.

2. The power on control panel was turned on.

3. 20L of mixture containing ethanol and water were prepared.

4. The reflux divider (KFS-101) was set to total reflux which is no. 2.

5. Let the cooling water flows into the condenser.

6. The cartridge heaters was switched on and allowing the ethanol solution to boil.

7. Let the distillation column to stabilize.

Continuous Process Procedure

1. The system was allowed to be stabilized at temperature approximately 0.2 ⁰C.

2. The pump P1 was turned on and valve V2 was opened.

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.

7. Sampling Procedure was conducted.

8. The Process was repeated with different inlet temperature which is 27 ⁰C.

Sampling Procedure

1. Distillate sampling:

1. The remaining liquid in the sampling valve V11 was drained.

2. A vial was placed below valve V11.

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:

1. Stagnated liquid remain in the valve V8 was drained.

2. A vial was placed below valve V8.

3. Valve V8 was fully opened and V7 was partially opened, 5-10 ml samples were

collected and both valves are closed.

4. The samples was cooling before analyzed.

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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

sample weight was recorded.

3. Water was added into the measuring cylinder to dilute the sample and obtaining a total

solution weight in the range 5 to 10 g. The solution weight was recorded.

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.

6. The actual sample’s composition was calculated.

Preparation of Calibrating Curve Procedure.

1. A set of mixtures containing ethanol and water was prepared within a specified range of

composition between pure water and pure ethanol.

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

A: Calibration curve of refractive index (RI) versus wt% ethanol

Purity of ethanol: 96%

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Density of ethanol: 789 kg/m3

Density of water: 1000 kg/m3

Amount of Amount of water Ethanol composition Refractive index

ethanol (mL) (mL) wt% mol% (RI)
0.0 10.0 0 0 1.3303
1.0 9.0 8.0601 3.3153 1.3363
2.0 8.0 16.4444 7.1627 1.3406
3.0 7.0 25.2615 12.1545 1.3455
4.0 6.0 34.4692 17.0635 1.3505
5.0 5.0 44.1029 23.5832 1.3469
6.0 4.0 54.2020 31.6435 1.3572
7.0 3.0 64.8011 41.8637 1.3588
8.0 2.0 75.9384 55.2463 1.3597
9.0 1.0 87.6558 73.5276 1.3600
10.0 0.0 100 100 1.3593

Refractive Index (RI) versus Ethanol composition (wt%)

1.365

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

Ethanol composition (wt%)

Figure 1: Graph for RI versus Ethanol composition (wt%)

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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%)

Distillate 37.3 1.207 8.237 1.3387 16.67 17.96

1 54.6
2 42.2
3 31.3
4 30.6
5 31.1
6 49.0
7 50.5
8 49.7
9 50.8
10 51.2
Bottom 89.0 1.390 8.200 1.3316 16.71 4.76

x-y equilibrium diagram

100

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)

Figure 2: Graph of ethanol-water at reflux ratio 2:2

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 Reflux ratio: 2:2 @ temperature : 27 ⁰C

Diluted Actual
Temperature Sample Solution Refractive solution’s sample’s
Tray (°C) weight (g) weight index composition composition
(g) (wt%) (wt%)

Distillate 76.4 1.255 8.388 1.3385 16.81 14.58

1 85.6
2 85.3
3 85.8
4 85.6
5 86.0
6 79.1
7 78.0
8 78.9
9 78.0
10 78.3
Bottom 86.0 1.230 5.991 1.3332 15.86 0

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 C. Murphree efficiency for each tray in the column

x-y equilibrium diagram

100

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)

Figure 3: Graph of ethanol-water at reflux ratio 2:2

1. Reflux ratio 2:2

x-y equilibrium diagram

100
90
mole % ethanol in vapor (y)

80
70
60
50
40
30
20
yn+1 10

yn 0
0 10 20 30 40 50 60 70 80 90 100

mole % ethanol in liquid (x)

xB xD
Figure 4: Graph of ethanol-water at reflux ratio 2:2

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 𝑦𝑛 − (𝑦𝑛+1 )
Em =
𝑦 ∗𝑛 − (𝑦𝑛+1 )

It is assumed that yn=y*n as the data is insufficient to locate the y*n.

18 − (5)
Em =
18 − (5)
Em = 1

D. Temperature and composition profile versus tray number

Reflux ratio 2:2

x-y equilibrium diagram

100

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

xB xD mole % ethanol in liquid (x)

Figure 5: Graph of ethanol-water at reflux ratio 2:2

𝑦𝑛 − (𝑦𝑛+1 )
Em =
𝑦 ∗𝑛 − (𝑦𝑛+1 )

It is assumed that yn=y*n as the data is insufficient to locate the y*n.

17 − (1)
Em =
17 − (1)
Em = 1

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8.0 SAMPLE CALCULATIONS

1. Weight percentage of ethanol:

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%

2. Mole percent of ethanol:

weight of ethanol (kg)

Mole of ethanol mol =
kg
molecular weight ( mol)

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 − 16.4444 1.3380 − 1.3370

=
25.2615 − 16.4444 1.3428 − 1.3370

𝑥𝐷 = 17.96

4. XB calculations

𝑥𝐵 − 16.4444 1.3380 − 1.3370

=
25.2615 − 16.4444 1.3428 − 1.3370

𝑥𝐵 = 17.96

9.0 DISCUSSION

Continuous distillation is an ongoing separation process in which a 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 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

in the distillation column.

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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

number also cannot be plotted as we just achieved only one plate.

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

approximately 1. The objective of this experiment is achieved.

11.0 Recommendation

The recommendations of this study are:

1) Use lower temperature as a variations for data collection as the unit took quite some time to

calibrate and achieved desired feed temperature.

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

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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

recycle. Chemical Engineering And Processing: Process Intensification, 108, 189-196.

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

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Engineering, 17(5-6), 549-560. http://dx.doi.org/10.1016/0098-1354(93)80043-m

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Experimental study of the production of high purity ethanol using a semi-continuous

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6. Springer, P., Baur, R., & Krishna, R. (2003). Composition Trajectories for Heterogeneous

Azeotropic Distillation in a Bubble-Cap Tray Column. Chemical Engineering Research And

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Citizendium, n.d. Continuous

Distillation. http://en.citizendium.org/wiki/Continuous_distillation (accessed 7.04.2017).

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13.0 APPENDICES

Murphree efficiency equation

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

Figure 1: Use of Murphree efficiency to determine actual number of trays.

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