TITLE:

Batch Distillation

OBJECTIVE:

1. To determine the principles of distillation column.

2. To determine the composition of a mixture by using refractive index.
3. To determine the variation of top product against time at constant reflux ratio.
4. To determine the effects of constant reflux ratio and regulating reflux ratio on product
composition.
5. To determine the temperature profile along the height of the column.

INTRODUCTION:

Distillation process is a process which a liquid or vapour mixture of two or more

substances is separated into its component fractions of desired purity by removal of heat.
Distillation processes depends on the distribution of components between gas and liquid phase.
The more volatile components which also called “light” or “low boiling” will concentrate in
the vapour. While, the less volatile components which also called “heavy” or “high boiling”,
will concentrate in the liquid phase. Separation of components from a liquid mixture via
distillation depends on the differences in boiling points and the concentrations of the individual
components.

Separation of binary mixtures is the simplest distillation. More volatile component is

usually plotted at the typical binary equilibrium curves shown in the Figure 1. Curve A is the
most common case where the more volatile component remains more volatile throughout the
entire composition range.

Azeotrope is a mixture of two liquids which has a constant boiling point and
composition throughout distillation. Curve B is a system with homogeneous azeotrope. The
component which is more volatile at low values of x1 and becomes less volatile at high values
of x1. While the x = y line mean that the vapour and liquid compositions are equal. The
maximum overhead product composition achievable with a feed of x1 = 0.25 is the azeotropic
composition. Similarly, the maximum bottoms product composition can be no lower than the
azeotrope composition for a feed with x1 = 0.9.
 Curve C is a system with heterogeneous azeotrope. It also can represent the two liquid
phases in equilibrium with one vapour phase. The azeotrope determines the maximum possible
separation achievable by simple distillation. Reflux ratio is the ratio of liquid flow rate from
the reflux drum to the flow rate of distillate.

Figure 1: Typical binary equilibrium curves

MATERIAL AND EQUIPMENT:

1. Batch distillation column

2. Refractometer
3. Beakers
4. Dripper
5. 40 v/v % ethanol-water mixture
6. 0 v/v % ethanol-water stock solution
7. 20 v/v % ethanol-water stock solution
8. 40 v/v % ethanol-water stock solution
9. 60 v/v % ethanol-water stock solution
10. 80 v/v % ethanol-water stock solution
11. 100 v/v % ethanol-water stock solution
Overhead condenser

Reflux drum

Vacuum pump
with pressure
Distillation column gauge

Flow meter

Main power switch

Top product tank

Reboiler

Figure 2: Batch distillation column

RESULTS AND CALCULATIONS

Table 1: Results of 60% reflux ratio in 30 minutes

60% conversion

Intervals 10 minutes 20 minutes 30 minutes

T1 (°C) 77.9 79.2 78.0
T2 (°C) 77.1 77.0 77.6
T3 (°C) 77.1 75.7 77.4
T4 (°C) 68.4 69.6 74.6
T5 (°C) 48.0 65.0 66.2
T6 (°C) 76.0 63.4 76.2
T7 (°C) 75.0 63.5 76.5
T8 (°C) 72.0 63.2 70.3
T9 (°C) 58.3 50.8 73.6
T10 (°C) 22.7 24.7 27.7
T11 (°C) 26.9 27.5 27.8
T12 (°C) 27.8 27.4 28.7
T13 (°C) 84.3 84.1 84.3
Heat power 0.0036 0.0036 35.80
(kW)
Reflux ratio 36.00 35.80 0.0036
Refractive 1st 2nd 3rd Av 1st 2nd 3rd Av 1st 2nd 3rd Av
index
Top 19.3 19. 19. 19.3 19.2 19. 19. 19. 18. 18. 18. 18.9
product(%) 3 3 2 2 2 9 9 9
Bottom 9.0 9.0 9.0 9.0 8.8 8.8 8.8 8.8 8.4 8.3 8.2 8.3
Product (%)

Table 2: Results of 50% reflux ratio in 30 minutes.

50 % conversion

Intervals 10 minutes 20 minutes 30 minutes

T1 (°C) 78.3 79.5 80.7
T2 (°C) 76.7 78.6 78.7
T3 (°C) 75.7 78.9 61.1
T4 (°C) 64.7 70.4 60.5
T5 (°C) 43.6 77.8 79.0
T6 (°C) 71.2 78.4 78.1
T7 (°C) 70.5 78.8 72.0
T8 (°C) 69.3 78.7 59.5
T9 (°C) 53.3 75.6 29.8
T10 (°C) 27.9 29.0 27.9
T11 (°C) 22.6 27.2 28.5
T12 (°C) 28.6 28.5 24.9
T13 (°C) 84.6 85.1 84.9
 Heat power 0.0039 0.0039 0.0038
(kW)
Reflux ratio 45.03 45.04 45.03
Refractive 1st 2nd 3rd Av 1st 2nd 3rd Av 1st 2nd 3rd Av
index
Top product 19.3 19.3 19.3 19.3 19.1 19.1 19.1 19.1 18.9 19.0 19.1 19.0
(%)
Bottom 8.2 8.0 8.1 8.1 7.6 7.2 7.1 7.3 8.6 8.4 8.2 8.4
Product (%)

For 60% conversion,

Average Refractive index of top product, RIav,1 = (19.3+19.2+18.9)/3 = 19.1

Average Refractive index of bottom product, RIav,2 = (9.0+8.8+8.3)/3 = 8.7

From graph,

The composition of ethanol in top product, y1= 0.84

The composition of ethanol in bottom product, x1= 0.29

For 50% conversion,

Average Refractive index of top product, RIav,3 = (19.3+19.1+19.0)/3 = 19.1

Average Refractive index of bottom product, RIav,4 = (8.1+7.3+8.4)/3 = 7.9

From graph,

The composition of ethanol in top product, y2= 0.84

The composition of ethanol in bottom product, x2= 0.25

Table 3: Refractive index readings for 60 % and 50% of reflux ratio
Reflux Top Product Bottom Product
Ratio Time Refractive Composition Time Refractive Composition
(min) Index (min) Index
60% 10 19.3 0.8528 10 9.0 0.3048
20 19.2 0.8474 20 8.8 0.2942
30 18.9 0.8315 30 8.3 0.2676
50% 10 19.3 0.8528 10 8.1 0.2569
20 19.1 0.8421 20 7.3 0.2144
30 19.0 0.8368 30 8.4 0.2729

Data set:
For top product at 60% reflux ratio and time = 10min, y = 19.3.
Equation for graph of Refractive Index vs Composition, y = 18.797x + 3.2706
19.3 = 18.797x + 3.2706
19.3−3.2706
𝑥=
18.797
= 0.8528
DISCUSSION:

Figure 3: The graph show that the average refractive index against with composition of ethanol
 Based on the figure 3, the line equation is y = 18.797𝑥 + 3.2706, where y represents the
refractive index and x represents ethanol composition in ethanol-water mixture. We set reflux
ratios of 50% as constant reflux ratio rate.

Data set for top product:

At t = 10 min:

Refractive index, for top product, y = 19.30

𝑦 = 18.797𝑥 + 3.2706

𝑦−3.2706
𝑥= 18.797

19.30−3.2706
= 18.797

= 0.8528

By substituting the refractive index into the line equation get from graph1, the ethanol
composition in the ethanol-water mixture for top product is 0.8528.

Reflux Top Product

Ratio Time Refractive Composition
(min) Index
50% 10 19.3 0.8528
20 19.2 0.8474
30 18.9 0.8315
 Graph of Ethanol Composition in
Top Product against Time
0.855
Ethanol composition 0.85
0.845
0.84 top product at 50%
0.835 reflux ratio

0.83
0 10 20 30 40
Time,min

Figure 4: Graph of Ethanol Composition in Top Product against Time

Reflux ratio is defined as the ratio of the liquid that has returned to the distillation
column to the amount of liquid being removed. From figure 4, ethanol composition in ethanol-
water mixture top reflux product against the time is set at the reflux ratio of 50%. From the
graph, we saw that the composition of ethanol decreasing from 0.8526 at 10th minute to 0.367
at 30th minute. This is due to the removal of ethanol from time to time from the tanks. However,
ethanol has higher volatility compare to water due to its lower boiling point and hence more
ethanol will be evaporated in top tanks as top products while less portion of ethanol will
evaporated in the reboiler as bottom products.

In batch distillation with constant reflux, the overhead product purity decreases with time.
(Engineers Guide). Higher reflux ratio implied more re-contacting of the liquid with the rising
vapour, thus leading to more separation and better distillate purity and causes slower distillate
collection rate. (Analysis of Continuous Distillation). Therefore, the reflux ratio in a batch
distillation should not be kept constant but keep higher during the separation of a fraction.
 Graph of Ethanol Composition against Time in Top Product
0.855
0.85
0.845
Composition

0.84
0.835
0.83
0.825
0.82
10 20 30
Time (min)

Top product at 60% reflux ratio Top product at 50% reflux ratio .

Figure 5: Graph of Composition vs Time in Top Product

Graph of Ethanol Composition against Time in Bottom Product

0.35
0.3
0.25
Composition

0.2
0.15
0.1
0.05
0
10 20 30
Time (min)

Bottom product at 60% reflux ratio Bottom product at 50% reflux ratio .

Figure 6: Graph of Composition vs Time in Bottom Product

At constant reflux ratio of either 60% or 50%, the composition of ethanol decreases as
time increasing based on Figure 5 and Figure 6. For example, the composition of ethanol is
0.8528 at 10 minutes and falls to 0.8315 after 30 minutes for 60% reflux ratio at top product.
The concentration of ethanol decreases because there is less ethanol available for batch
distillation process as time increasing since it is constantly removed from top and bottom tanks.
 For regulating reflux ratio, the composition of ethanol falls more significantly for 60%
reflux ratio than 50% reflux ratio at top product based on Figure 5. This is due to the higher
recovery of ethanol at higher reflux ratio and faster using of ethanol in the distillation chamber.
Hence, the faster recovery of ethanol ended up with significant decreasing in ethanol
concentration from time to time at higher reflux ratio. However, at bottom product, the
composition of ethanol is lower for 60% reflux ratio as more ethanol is recovered at top product
compared to 50% reflux ratio as shown in Figure 6. Thus, higher reflux ratio results in higher
recovery of ethanol at top product.

Figure 7 shows the graph of Temperature Profile from T1 to T13 of Different Reflux Ratio at
10 min.
Figure 8 shows the Temperature Profile from T1 to T13 of Different Reflux Ratio at 20 min

Figure 9 shows the Temperature Profile from T1 to T13 of Different Reflux Ratio at 30 min.

By referring to Figure 7, 8 and 9, (T1 to T9 and T13 the temperature indicators of

the reboiler up to whole distillation column whereas T10 to T12 are the temperature indicators
located at the condenser) it is observed that the temperature of the ethanol-water mixture
decreases a little from the reboiler up along the height of the distillation column to the
condenser. The decrease in temperature is due to a few factors. First of all, the vapourization
of the ethanol-water mixture consumes heat energy. Besides, the reflux condensed mixture
from the condenser absorbs a portion of heat energy from the elevating vapourised mixture,
thus decreasing the temperature of the column. The temperature of the vapourised mixture
decreases gradually along the height of distillation column because each tray of the column
facilitates heat transfer between the condensed and vapourised mixture and this reduces the
temperature of the mixture cumulatively along the height of distillation column. Another factor
that will cause the decreasing of column temperature is the heat loss to surroundings.

CONCLUSION:

As conclusion, the brix index into a calibration curve can be apply in the composition
of mixture which the brix index (%) is the x-axis while the percentage of ethanol in water (%)
is the y-axis. When the reflux ratio is constant, the composition of ethanol in the distillate are
almost constant. Based on the results, the composition of ethanol in water is higher in the top
products than the bottom products due to the ethanol is more volatile compared with water.

REFERENCES:

1. Mass Transfer Distillation. (n.d.). Engineers Guide, retrieved 3 April 2018, from
enggyd.blogspot.my/2010/03/mass-transfer-distillation.html?m=1

2. Analysis of Continuous Distillation. (n.d.). Retrieved 3 April 2018, from

http://www.separationprocesses.com/Distillation/DT_Chp04-1.htm

3. BBC - Higher Bitesize Physics - Refraction of light: Revision, Page2.

(2014). Bbc.co.uk. Retrieved on 29 January 2018, from:
http://www.bbc.co.uk/bitesize/higher/physics/radiation/refraction/revision/2/

4. Distillation Process. 2017. Distillation Process. Retrieved on 29 January 2018, from:

http://www.separationprocesses.com/Distillation/DT_Chp04b.htm.