EXPERIMENT 7: BATCH DISTILLATION AT CONSTANT REFLUX

1.0 Problem Statement

Under the condition of constant reflux, batch distillation is operated at a fixed reflux ratio.
Reflux ratio is the ratio of reflux returning to the distillation column to the reflux that is
collected as distillate. In constant reflux, the composition of distillate will keep varying and
the composition of the bottom product will be decreasing from time to time. In this
experiment, a mixture of ethanol is to be distilled at constant reflux. The composition of the
distillate and bottom product are to be determined and analysed using their refractive index
for every 10-minute intervals.

2.0 Hypothesis

The ethanol composition in distillate will increase over time whereas the ethanol composition
in bottom product will decrease over time.

3.0 Objectives
1. To operate a batch distillation unit at constant reflux.
2. To examine the change in top and bottom composition over time in a batch
distillation.
3. To identify the correlation of refractive index with the composition of ethanol in
the distillate and bottom product

4.0 Introduction

Distillation is a commonly used method for separation of components of a miscible fluid

mixture by means of selective evaporation and condensation. The distillation process
involves a change of state from liquid to vapour and back to liquid again. This separation
method is widely used in preparative chemistry and also in manufacturing industry for
purifying products and chemical intermediates. (Distillation - an overview | ScienceDirect
Topics, 2017) Distillation column is the apparatus to use in distillation of liquid mixtures to
separate the mixture into its component parts. There are many types of distillation columns,

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each type is designed to perform specific types of separations and each design differs in terms
of complexity. Besides, distillation can be categorised into batch distillation and continuous
distillation.

In batch distillation columns, the feed is charged into the reboiler at the beginning of the
operation and heat is provided at the reboiler to evaporate part of the liquid to generate a
vapor that rises through the column until it has reached the condenser where it is converted to
liquid and collected at the reflux tank. Then, from this reflux tank, a part is returned to the
column as liquid reflux that descends through the column contacting the vapor counter-
currently if the column is full of packing or contacting the vapor in a crosscurrent pattern if
the column contains plates. (Narvaez-Garcia et al., 2013)

The main characteristic of a batch distillation column is that concentrations and temperatures
are varying with time at any part of the column. In general, there are two main operating
methods for batch distillation columns which are constant reflux and variable reflux. For
batch distillation under constant reflux ratio, R is kept constant and distillation is continued
until the distillate composition xD reached a constant value.

Figure 1  Example Equilibrium Curve At  Constant Reflux Ratio

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From the operating line equation, note that if R is constant and xD is decreasing, then its slope
remains constant while its intercept decreases. Therefore, for batch distillation under constant
reflux ratio, the operating line shifts as distillation progresses. (Constant Composition, 2021)

5.0 Material & Apparatus

Materials: Ethanol-water mixture
Apparatus: Distillation Column, Refractometer, Beakers, Timer

6.0 Procedures

6.1 General Start-up Procedure

1. All valves were made sure to be closed.

2. The mixture of ethanol and water was prepared at desired composition. At instance,
4L of ethanol and 6L of filtered water.
3. The ethanol and filtered water were poured into feed tank B2 and B3 separately.
4. All valves are ensured to be in close position except V4,V5,V1 and V8.
5. The main power on the control panel was turned on.

6.2 Experimental Procedure

1. The general set-up procedures were performed.

2. The pump and heater were switched on.

3. The heater power control was set to 2.0kW. The reboiler temperature was set
approximately to 85°C.

4. The reflux control was kept at position 3 (constant reflux).

5.  The temperature was recorded when the top column temperature sensor, TT 112 has
reached a steady state value.

6. The timer was started when the distillate started to flow into the phase separator.

1. The reflux control was set to position 2 (total distillate offtake).

2. The distillate and bottom product samples were collected every 10 minutes.

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 3. The refractive index of the samples were measured and the values were recorded into
data table.

4. The collection of distillate and bottom product was stopped once the refractive index
reading reached constant.

6.3 General Shut-down Procedure

1. The reflux control was set to position 1 (total reflux).

2. The cooling water was kept running through the condenser(W2).
3. The heater power was switched off. The temperature drop in the reboiler was
monitored until it has cooled down to room temperature.
4. All liquid from the reboiler B1 and product tank B4 and B5 were drained.
5. The cooling water valves V1 and V8 were closed.
6. The main power on the control panel was turned off.

7.0 Result & Calculation

Table 1 Composition data based on refractive index

Volume Mol
Volume Mass of Mass of Mole of Mol of
of fraction Refractive
of Water Ethanol Water Ethanol Water
Ethanol of index (RI)
(ml) (g) (g) (ml) (mol)
(ml) ethanol
0.55493
0 10 0 10 0 0 1.466
9
0.49944
1 9 0.789 9 0.017126 0.033153 1.472
5
0.44395
2 8 1.578 8 0.034252 0.071627 1.476
1
0.38845
3 7 2.367 7 0.051378 0.116813 1.484
7
0.33296
4 6 3.156 6 0.068504 0.170635 1.485
3
0.27746
5 5 3.945 5 0.085631 0.235832 1.488
9
0.22197
6 4 4.734 4 0.102757 0.316435 1.488
6

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 0.16648
7 3 5.523 3 0.119883 0.418637 1.491
2
0.11098
8 2 6.312 2 0.137009 0.552463 1.493
8
0.05549
9 1 7.101 1 0.154135 0.735276 1.496
4
10 0 7.89 0 0.171261 0 1 1.497

Calculations

Given data:

Density of water = 1 g/mL

Density of ethanol = 0.789 g/mL

Molecular weight of water = 18.02 g/mole

Molecular weight of ethanol = 46.07 g/mole

Sample Calculation

Volume of ethanol=1mL;Volume of water=9mL

g
1. Mass of ethanol=volume × density ¿ 1 mL ×0.789 ¿ 0.789 g
mL
g
2. Mass of water =volume × density ¿ 9 mL × 1 ¿9 g
mL
Mass of ethanol
3. Mole of ethanol=
Molar mass ofethanol

0.789 g
¿
46.07 g ¿ 0.017126 mol
mol

Mass of water
4. Mole of water =
Molar mass ofwater

9g
¿
18.02 g ¿ 0.49944 mol
mol

Mol of ethanol 0.017126

5. Mol fraction of ethanol= ¿
Mol of ethanol+ Mol of water 0.017126+0.499445

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 ¿ 0.033153

Graph of refractive index against mol fraction of ethanol

1.5

1.5

1.49

1.49
Refractive Index

1.48

1.48

1.47

1.47

1.46

1.46

1.45
0 0.2 0.4 0.6 0.8 1 1.2

Mol fraction of ethanol

Figure 2 Graph of Refractive index against mol fraction of ethanol

Mol fraction of Mol fraction of

Time(min) Distillate (RI) Bottom (RI)
ethanol ethanol

10 1.467 0.0055 1.497 1

20 1.478 0.0829 1.489 0.3504

30 1.483 0.1112 1.484 0.1168

40 1.488 0.2761 1.476 0.0716

50 1.495 0.6743 1.4755 0.0668

Table 2 Mol fraction of ethanol for distillate and bottom product with varying of time

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Sample Calculation

For 10 minutes:

Refractive index of distillate =1.467

1.467−1.466 x−0
Mol fraction of ethanol = =
1.472−1.466 0.0332−0

x=0.0055 mol

Refractive index of bottom=1.497

Refer to the graph,

Mol fraction of ethanol=1

X-Y Equilibrium Diagram for Ethanol-Water System at 1 atm (10 minutes)

1
0.9
0.8
Vapor mol fraction

0.7
0.6 Equilibrium
0.5 Distillate
0.4 Bottom
0.3
0.2
0.1
0
-0.2 0 0.2 0.4 0.6 0.8 1 1.2

Liquid mol fraction

Figure 3 Distillate and Bottom Composition on X-Y Equilibrium Diagram at 10-minute

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X-Y Equilibrium Diagram for Ethanol-Water System at 1 atm (20 minutes)
1
0.9
0.8
0.7
Vapor mol fraction

0.6 Equilibrium
0.5 Distillate
0.4 Bottom
0.3
0.2
0.1
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Liquid mol fraction

Figure 4 Distillate and Bottom Composition on X-Y Equilibrium Diagram at 20-minute

X-Y Equilibrium Diagram for Ethanol-Water System at 1 atm (30 minutes)

1
0.9
0.8
Vapor mol fraction

0.7
0.6 Equilibrium
0.5 Distillate
0.4 Bottom
0.3
0.2
0.1
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Liquid mol fraction

Figure 5 Distillate and Bottom Composition on X-Y Equilibrium Diagram at 30-minute

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X-Y Equilibrium Diagram for Ethanol-Water System at 1 atm (40 minutes)
1
0.9
0.8
Vapor mol fraction

0.7
0.6 Equilibrium
0.5 Distillate
0.4 Bottom
0.3
0.2
0.1
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Liquid mol fraction

F
igure 6 Distillate and Bottom Composition on X-Y Equilibrium Diagram at 40-minute

X-Y Equilibrium Diagram for Ethanol-Water System at 1 atm (50 minutes)

1
0.9
0.8
Vapor mol fraction

0.7
0.6 Equilibrium
0.5 Distillate
0.4 Bottom
0.3
0.2
0.1
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Liquid mol fraction

F
igure 7 Distillate and Bottom Composition on X-Y Equilibrium Diagram at 50-minute

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 Graph of Composition against Time
1.2

1
Composition of ethanol

0.8

Distillate
0.6
Bottom
0.4

0.2

0
5 10 15 20 25 30 35 40 45 50 55

Time(min)

Figure 8 Graph of Composition against Time

8.0 Discussion

1. Compare the quality of distillate among the sieve tray column and the packed
column.

Sieve Tray Column

Sieve trays are simply metal plates with holes in them. Vapour passes straight upward
through the liquid on the plate. Each tray has 2 conduits, one on each side, called downcomer.
Liquid falls through the downcomers by gravity from one tray to the one below it. If the
vapor velocity is much lower than design, liquid will begin to flow through the perforations
rather than into the downcomer. A weir on the tray ensures that there is always some liquid
on the tray and is designed such that the holdup is at a suitable height. Being lighter, vapour
flows up the column and is forced to pass through the liquid, via the openings on each tray.
The area allowed for the passage of vapour on each tray is called the active tray area. The
sieve tray has good capacity and moderate efficiency compared to the valve tray and bubble
cap tray but has limited flexibility in the operating range. The sieve tray has low maintenance
cost and low fouling tendency when compared to other conventional trays.

Packed Column

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Packed columns are used for distillation, gas absorption and liquid-liquid extraction. The gas-
liquid contact in a packed column is continuous. The liquid flows down in the column over a
packing surface and the vapor moves counter-currently, up the column. The performance of a
packed column is very dependent on the maintenance of good liquid and gas distribution
through the packed bed. The packing types can be divided into two broad classes: structured
and random packings. The packing provides a large surface area for vapor-liquid contact,
which increases the column's effectiveness. The packing increases the time of contact, which
increases the separation efficiency. The exiting vapor contains the most volatile components,
while the liquid product stream contains the least volatile components.

2. Using the X-Y equilibrium diagram for ethanol-water systems, mark the top and bottom
compositions for each sampling time on the diagram. Observe the change of composition
over time in the batch distillation column.

Mol fraction of ethanol was calculated and tabulated in Table 2 above. The mol fraction and
refractive index were recorded every a 10-minute interval. Based on Table 2, the refractive
index of distillate is increasing as the process takes longer from 1.467 at 10-minute up until
1.495 at 50-minute. Meanwhile, the refractive index of the bottom is slightly decreasing from
1.497 mol at 10-minute, down until 1.4755 at 50-minute. The mol fraction of ethanol for
distillate is having a significant increment as the process takes longer from 0.0055 at 10-
minute up until 0.6743 at 50-minute. On the other hand, the mol fraction of ethanol for
bottom is significantly decreasing from 1 mol at 10-minute until 0.0688 at 50-minute. X-Y
Equilibrium Diagram for Ethanol-Water System was plotted for every 10-minute interval.

3. Plot graph of composition vs time

Graph of composition versus time was plotted in Figure 8. It shows that the composition of
ethanol at bottom is decreasing. Meanwhile, the composition of ethanol at distillate is having
an upward trend.

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9.0 Limitation/Precaution

The first limitation is the assumptions made by using the McCabe-Thiele method. There are
some assumptions of the Mc-Cabe-Thiele method. Firstly, constant molar overflow where
flow rates of vapor and liquid are constant throughout the column. Second, constant pressure
during column operation and molar heat of vaporization of components in feed are equal. In
this experiment, there is no monitor of the pressure and the pressure is becoming unknown.
As a result, we cannot control the distillation column at a constant pressure. Furthermore, the
expected data given was not suitable to find the number of stages. The data given plotted in
the graph do not intercept the reading in X-Y Equilibrium Diagram for Ethanol-Water
System at 1 atm. As a result, the number of stages cannot be determined.

For the precautions part, the ethanol is a volatile and flammable liquid. It must be careful
to handle and follow the steps of the lecturer to avoid accidents. Besides, ensure that the
outlet to the atmosphere downstream of the condenser is functioning, as this prevents a blow-
out due to excessive pressure build-up. Furthermore, the pressure-relief valves must be tested
periodically to ensure they still function. If possible, the experiment should be carried out at
least three times and calculate the average result to get a more accurate result. Lastly,
laboratory coats and gloves must be worn throughout the experiment to prevent any injuries.

10.0 Conclusion

The objectives of this experiment were achieved successfully. The separation process was
carried out in a batch distillation unit at constant reflux. Next, mass balance equations were
used to analyse the mole fraction of ethanol to plot the graph of refractive index against mol
fraction of ethanol. According to the graph, it helps us to correlate the composition ethanol
and refractive index. When the composition of ethanol increases, the refractive index
increases as well. The graph of composition against time was plotted to show the composition
changes against time where it can be concluded that distillate composition increases over
time and bottom composition decreases over time.

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11.0 References

‌Constant Composition. (2021). Separationprocesses.com.

http://www.separationprocesses.com/Distillation/DT_Chp05c.htm

‌Distillation - an overview | ScienceDirect Topics. (2017). Sciencedirect.com.

https://www.sciencedirect.com/topics/earth-and-planetary-sciences/distillation

Narvaez-Garcia, A., Zavala-Loria, J. del C., Vilchis-Bravo, L. E., & Rocha-Uribe, J. A.

(2013). Design of Batch Distillation Columns Using Short-Cut Method at Constant
Reflux. Journal of Engineering, 2013, 1–14. https://doi.org/10.1155/2013/685969

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