Department of Chemical Engineering and Energy Sustainability

Faculty of Engineering

KNC3221 ENGINEERING LABORATORY 4

Laboratory Report on Experiment 2: Distillation

By

GROUP 8

Group Members : Alick Davidson Anak Elciana (58434)

Dayang Shafiqah Binti Awang Rapiee (58545)
Mutamilselvi A/P Muthukumar (56893)

Lecturer : Mr Mohd Farid Atan

Date of Submission : 25th February 2019

BACHELOR OF ENGINEERING WITH HONOURS

(CHEMICAL ENGINEERING)
ACADEMIC SESSION 2018/2019
 ABSTRACT
Distillation refers to the technique used to separate the component substance from
a miscible fluid mixture by evaporation and condensation. The distillation method
is very crucial in the food processing, gas-liquid separation and biochemical
industry. This experiment was focusing on the separation of mixture of ethanol and
distilled water by means of batch distillation whereby batch distillation is widely
used in specialty chemical industry with low volume of chemicals used. This
experiment was conducted with 10L of solution which consists of 2L of pure ethanol
and 8L of distilled water has the objective to study the effect of an operating
parameter (power) on the pressure drop in a distillation column. The pressure drop
is very important as it affects the efficiency of the distillation column. The
relationship of boil up rate with pressure drop and degree of foaming on trays
inside the distillation column will be analyzed. With the aim to obtain different
pressure drop of the column, the power was set up to 0.9kW, 0.95kW, 1.00kW,
1.05kW and 1.10Kw respectively. For every power, the sample of condensed ethanol
was collected in 5- minutes time to calculate the boil up rate. The degree of foaming
also increased with increased in power. The higher the heater power, the greater
the boil up rates will be and the degree of foaming will be increased with the
increment of pressure drop.

Keywords: Distillation; Boil up rate; Pressure drop; Foaming; Distillation

column
 TABLE OF CONTENT

Topic Page
1.0 INTRODUCTION 1
1.1 Theory Background 1
1.2 The aim of the experiment 1
1.3 Objectives of the Experiment 2
1.4 Problem Statement 2
2.0 LITERATURE REVIEW 2
3.0 METHODOLOGY 3
3.1 Safety Precautions 3
3.2 Experimental Procedures 3
3.3 Apparatus and Materials 5
3.4 Equation and formula 6
4.0 RESULT AND DISCUSSION 7
5.0 CONCLUSION AND RECOMMENDATION 10
6.0 REFERENCES 11
1.0 INTRODUCTION
1.1. Theory Background
This experiment was conducted using batch distillation. According to
Kim and Diwekar (2005), the reboiler which acts as a still is filled with feed
mixture (10L of ethanol solution) that evaporates and leaves the still in vapor
form. At the top of the distillation column, the ethanol vapor is collected in the
condenser and accumulated at the receiver. Tham (2018) mentioned that a
typical distillation contains the major components such as a vertical shell,
column internals 9trays), reboiler, condenser and reflux drum. Tham also
clarified that liquid mixture of ethanol and water that need to be processed is
the feed will be introduced to the middle tray known as feed tray. This tray will
divide the column into top 9rectifying) section and bottom (stripping section).
A liquid feed (ethanol and water) will contact at more than one points
where the liquid flows over the plates and vapor bubbles up through the liquid
via holes in the plates. As liquid goes down the column, the vapor comes in
contact with it several times due to the multiple trays. The liquid and vapor
phases brought into contact because one molecules of higher boiling point
(water) converts from vapor to liquid phase by energy release (exothermic) and
another molecule of low boiling point (ethanol) used the released energy
(endothermic) to convert from liquid to vapor phase (SRS Engineering
Corporation, 2016).
The separation of the components depends on the relative vapor
pressures of the substances. In distillation, the vapor formed at each stage is
assumed to be in thermodynamic equilibrium with the liquid and the relation
of the vapor composition (ethanol) and the liquid composition (water) is
depending on temperature and pressure. Power used will indicate the rise in
the velocity of the vapor as the temperature and pressure of the mixture will
increase and the distillate of ethanol will increase proportionally.

1.2. The Aim of the Experiment

The aim of this experiment is to vary the value of the power controller and study
the relationship between the boil-up rate with pressure drop and the degree of
foaming on trays.

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 1.3. Objective(s) of the Experiment
The objective of the experiment is to study the effect of an operating parameter
on the pressure drop in a distillation column.

1.4. Problem Statement

This experiment was designed and conducted to analyse how does heater power will
affect the boil-up rate with pressure drop and the degree of foaming on trays within
the distillation column. Besides that, this experiment was conducted to determine the
pressure drop for various boil-up rates in a batch distillation, the degree of foaming
on trays each time the power increased.

2.0 LITERATURE REVIEW

Distillation is a process in which liquid or vapour mixture of two or more
substances is separated into its component fractions of desired purity by the
application and removal of heat. The vapor of the boling mixture will be richer in the
components that have lower boiling points. When this vapour is cooled and condensed,
the condensate will contain more volatile components and the original mixture will
contain more of the less volatile material. As the operation of the distillation column
involved the binary mixture throughput, the variation of pressure need to be
monitored. Liu and Jobson (1999) said that the changes in the increment and
decreasing in pressure which depends on the latest operating pressure can affect the
throughput amount.
Many references have been discussed the effect of operating pressures on the
distillation column efficiency. Liu and Jobson (1999) proposed that the effects of
pressure is on the hydraulic performance of a distillation column. When the pressure
increases, relative volatility between the components will decrease and this will
increase reflux ratio and molar flow rates in the column. Therefore, the area required
for vapour flow will increased. In connection to this research, Winkle (1967) noted that
vapour volume increases as pressure decreases and larger diameter columns are
required to occupy the increase in vapour volume.
In the other hand, decreasing pressure can increase the capacity of the column.
Capps (1993) clarified that decreasing in the operating pressure will lead to increasing
feed rate. This is due to the increasing in volatility and flooding capacity. Kister and

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 Townsend (1984) analysed that low pressure in the 𝐶2 splitter in an ethylene plant
helps to reduce the capital cost and operating cost due to the smaller reflux ratio,
column diameter and less number of trays compared to high pressure operation.
Foaming also being observed in this experiment. Yirka (2017) said that
foaming is the expansion of liquid that provides high interfacial liquid-vapor contact
and can decrease decreases the vapour-liquid equilibrium, thus slowing down the
distillation process. Yirka also mentioned that foaming may due to the passage of
vapour or gas or gas velocity is too high or rate of evaporation is too fast. Senger and
Wozny in their research paper entitled ‘Impact of Foam to Column Operation’ found
that foam may result in increasing the pressure loss, reduced capacity, reduced
separation efficiency and there will be contamination of the products. The appearance
of foam in packed columns results in high-pressure drop, a lack of mass transfer and
unexpected low capacities. The degree of foaming increases when the power increases.
The appearance of foam in packed columns results in a high pressure drop. The
specific pressure drop profiles as a function F-factor are defined by Equation 1 (Senger
& Wozny, 2012)

F − factor = w
̅ gas √ρgas (1)

3.0 METHODOLOGY

3.1 Safety precautions

1. Avoid touching the hot component of the units.

2. Wear protective clothing, gloves and safety spectacles when handling the chemicals.
3. All the operating instructions supplied with the unit must be carefully read and
understood in advance before attempting to operate the unit.

3.2 Operating procedure

1. 2L of pure methanol is diluted with 8L of distilled water to obtain 10L of diluted

solution.
2. The unit operation is set at total reflux by switching “Off” the reflux ratio timer on the
console.
3. All valves are closed.

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4. Valve 𝑉10 is opened on the reflux pipe.10L of the prepared solution is injected into the
reboiler via filler cap and the filter cap is ensured to be replaced firmly.
5. The power is turned on to the control panel.
6. The temperature 𝑇9 (temperature in the boiler) is set.
7. Valve 𝑉5 is opened until the cooling water flow rate (𝐹11 ) to the condenser is
approximately at 3L/min as 3L/min is the maximum flow rate than can be supply from
the water pipe.
8. On the control panel, the power controller of the reboiler heating element is fully
turned (fully anti-clockwise) and the power of the heating element is turned to ‘Power
On’ position. Red lamp is appeared to indicate the heating element is ‘On’.
9. The power controller is turned in clockwise direction until a reading approximately at
0.75 kW mentioned at digital wattmeter. The warm-up temperature of the reboiler
content can be read at readout meter (The boil- up rate can reach up to a maximum
of 1.5kW by adjusting the boiler heater power controller on the control panel). This is
because the maximum power supply to the heater is 3.0kW and 1.5kW is restricted as
the lowest power to avoid faulty to the unit.
10. 𝑉6 and 𝑉7 is opened which connect base and top of the distillation column respectively
to the manometer. There will be no pressure difference in the column and no reading
at the manometer. 𝑉6 and 𝑉7 is closed.
11. 1st and 5th plates in the column sections are observed. The appearance of these trays
is observed throughout the distillation process.
12. Vapour is commenced to climb up in the column progressively by switching the
selector temperature on 𝑇8 , 𝑇7 , 𝑇6 ,𝑇5 , 𝑇4 , 𝑇3 ,𝑇2 and 𝑇1 . The vapour entered the
condenser and reappeared as droplets into the glass-walled distillate receiver vessel
(11). The distillate is build up a small level in the receiver and eventually overflow to
the reflux regulator valve Since the valve is not ‘On’ (on the control panel) and it will
not be necessary to have it on this experiment which is run under total reflux, the
condensed vapour will return to the column.
13. The cooled distillate is returned on the top of the column and cascade down the trays
forming a liquid level on the trays and bubbled of vapour passed through the liquid.
The system reached an equilibrium condition when temperature 𝑇8 , 𝑇7 , 𝑇6,𝑇5 , 𝑇4 , 𝑇3 ,𝑇2
and 𝑇1 are constant.

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 14. The boil up rate is measured by performing a timed volume collection
15. V3 is operated so that all the condensate is diverted into a measuring cylinder
16. The time required to collect a set of quantity is measured by using stopwatch. The
equilibrium conditions in the column provided a liquid level is maintained in the
condensate feeding pipe.
17. V3 is partially opened and the condensate is drained (in a separate measuring
cylinder) when the sample is taken from the reflux system until a steady flow
obtained. (The liquid is ensured remain in the flexible connecting tube to prevent
vapour from escaping)
18. The sample for collection and timing is started at the same time and is collected at a
sizeable amount (The volume of condensed ethanol is collected within 5 minutes for
every power value to calculate the boil up rate).
19. The first non-representative collected amount is poured in a bottle labelled the name
of the chemicals used.
20. After the sample is taken, the reading of the pressure drop over both the rectifying
(top) and the stripping (bottom) sections is taken by opening the valves V6 and V7 on
the manometer. When the valve is opened, V6 and V7 are opened to prevent vapour
from the column entering the manometer.
21. The valves are closed in the same order after the pressure drop reading is taken.
22. The reading is repeated until two in a row agree fair closely. The next set of
measurement is started after 5 to 10 minutes between each set of measurement in
order for the system to reach equilibrium.
23. The boil-up rate is stepped up in 250 W increments up to a maximum of 1.5kW by
adjusting the boiler heater power controller (on the control panel). Similar reading of
the boil-up rate and pressure drop is taken after column is stabilized at least 10
minutes.
24. The shutdown procedure is performed after the experiment is finished by following
the SOP provided by the assistant engineer.

3.3 Apparatus and Materials

Equipment: Distillation Column Unit

Apparatus: Stopwatch (timing device)

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Materials: 1) 2L of pure ethanol, C2H3OH

2) 8L of Distilled Water

3.4 Equations and Formula

The Taverage is calculated as the following formula:

T1+T2+T3+T4+T5+T6+T7+T8
Taverage = (2)
8
The boil-up rate is calculated based on the following formula:
l volume(ml) l 60min
Boil up rate, = × × (3)
hr time(min) 1000ml hr
Volume = 100 ml = 0.1 L
The formula to calculate the pressure drop:
Pressure drop  cm H 2O  = Highest – Lowest (4)

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 4.0 RESULTS AND DISCUSSION

Table 4.1: Collected data of temperature of the distillation column

Power(kW) T1(ºC) T2(ºC) T3(ºC) T4 (ºC) T5(ºC) T6(ºC) T7(ºC) T8(ºC) Tavg (ºC) T9(ºC)
(reboiler)
0.90 87.4 88.4 88.9 88.2 89.3 89.7 89.7 89.3 88.86 90.6
0.95 88.8 89.1 89.3 89.1 89.7 90.0 98.5 89.6 90.51 91.1
1.00 89.3 90.2 90.6 90.0 90.9 90.8 91.3 90.7 90.48 92.0
1.05 90.8 91.8 91.3 91.0 91.5 91.9 92.2 91.3 91.48 92.7
1.10 91.7 92.1 92.6 91.8 92.9 92.8 93.2 92.6 92.46 93.7

Table 4.2: Calculated data from distillation experiment

Power Boil-Up Rate Pressure Drop (cm Degree of Foaming on Trays

(kW) (L/hr) 𝑯𝟐 𝑶)
0.90 1.98 4 Foaming vigorously at the most
bottom of the part
0.95 2.02 8 Foaming robustly until tray 6
1.00 2.16 13 Foaming robustly until tray 7
1.05 2.16 14 Foaming aggressively until upper
part of the column
1.10 2.28 14 Foaming actively until upper part of
the tray

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 Boil Up Rate vs Average Temperature of Boil Up Rate vs Pressure Drop
Distillation 2.3
2.35 y = 0.0265x + 1.8475
y = 0.078x + 1.894 2.25

Boil Up Rate (L/hr)

2.3 R² = 0.8822
R² = 0.9676
Boil Up Rate (L/hr)

2.25 2.2
2.2 2.15
2.15
2.1 2.1
2.05 2.05
2
1.95 2
1.9 1.95
1.85
1.8 1.9
88.86 90.51 90.48 91.48 92.46 0 5 10 15
Average Temperature (ºC) Pressure Drop (cmH20)

Figure 4.1. Boil up rate against Average Temperature of Figure 4.2. Boil Up Rate against Pressure Drop
Distillation Column
The blue line indicates the power from 0.90kW to 1.10kW The blue line indicates the power from 0.90kW to 1.10kW
The black line is the linear line of the blue line and The black line is the linear line of the blue line and
represented by the equation y and the quadratic of the represented by the equation y and the quadratic of the
coefficient of correlation R2. coefficient of correlation R2.

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 Table 4.2 above shows the pressure drop of the mixture of column, the boil-up rate and
the observation of the degree of foaming on each tray. The data is obtained based on the
different power intensities of 0.90, 0.95, 1.00, 1.05 and 1.10 kW respectively. Figure 4.1
depicts the relationship of the average temperature inside the distillation column against
the boil up rate of the ethanol. From the graph plotted above, it is clearly seen that as the
temperature increases the boil up rate increases as well. The trend can be observed clearly
where from the starting temperature of 88.86 ℃ to 90.51℃ there is a gradual increase
because the boil up rate increases causing the temperature of distillation column to
increase. This is because the ethanol and water starts to separate where the lower key
component will vaporise through the upper part of the distillation column. As for the
liquid in the column, it foams vigorously at the most bottom part of the distillation column.
From the temperature of 90.51℃ to 90.48 ℃, the trend shows a sudden increase. This is
due to the increase in temperature and power causing the boil up rate to suddenly increase
because the molecules move faster and further apart thus releasing slightly more heat
energy due to the exothermic reaction thus the liquid foams robustly till tray 6. In addition
to that, aluminium foil is used to cover the distillation column to prevent heat loss from
the column causing the heat to be accumulated in the column and the rate of evaporation
of ethanol to increase which contributes to the steep increase of the boil up rate. The same
pattern that is observed from the starting temperature of 88.86 ℃ to 90.51℃ is also seen
from temperature of 90.48℃ to 91.48℃ where this phenomenon corresponds with the
actual theory that states that the increase in the power supplied increases the
temperature inside the distillation column and the temperature of the mixture of water
and ethanol causing the boil up rate of ethanol to increase as well. Besides for the
temperature of 91.48℃ to 92.46℃, the trend of the graph records a steady increase. This
is because the heat accumulated is evenly distributed in the column which is shown in
the graph itself where the boil up rate line is aligned with the linear line. The liquid foams
actively till the upper part of the tray. The R2 value is 0.9676 where it shows that the
correlation is positive and reaches nearly to 1. This proves that the boil up rate is
increasingly linearly with the average temperature.

On the other hand, in Figure 4.2 which shows the relationship of the boil up rate and
the pressure drop in the distillation column records a trend that gradually increases then
a sudden increase followed by a sharp increase. The gradual increase of the boil up rate
against the pressure drop is shown when the pressure drop is from 4 to 8. The value of
the pressure drop is slightly smaller which shows that a small amount of vaporised
ethanol starts to rise to the upper part of the distillation column. There is only a small

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amount of vaporised ethanol although the temperature reached above boiling point of
ethanol due to the heat loss to the surrounding from the distillation column due to the
absence of the insulator which is the aluminium foil. When the pressure drop is from 8 to
14, the trend shows a sudden increase. This is due to the presence of the insulator to cover
the distillation column which accumulates more heat energy that caused more ethanol to
boil and move upwards creating a big difference in pressure as more vapour is in the upper
part and more liquid in the lower part of the distillation column. The steep increase
observed in the trend is due to the random error. The pipe connecting the condenser
disconnected from the water supply causing the phase change of the ethanol vapour into
liquid phase to become slower. Thus, more vapour ethanol will accumulate at the upper
part of the distillation column that resulted in a big difference in pressure between the
upper and lower part of the distillation column. The R2 value is 0.8822 proving that the
correlation is positive and near to 1 which approves that boil up rate increase to pressure
drop linearly.

5.0 CONCLUSION AND RECOMMENDATIONS

The objective of the experiment was successfully achieved. From the R2 value is
proved to be linearly proportional with both the temperature and pressure drop as
observed from the data obtained from the experiment. The increase in the power supplied
will cause the increase of temperature within the distillation column. The pressure drop
increases as there is difference between the pressure between the upper part and bottom
part of distillation column. Therefore, further recommendation should be imposed to
achieve a more accurate result in the future. For instance, the usage of an insulator to
cover the glass wall of the distillation column to reduce the time for boiling the solution.
Moreover, the distillation unit should be frequently checked and maintained because
when the experiment was carried out the level sensor in the reboiler was faulty causing
an inability to detect the level. Last but not least, the water hose should be secured tightly
to the pipe to ensure that the flow of water to the condenser is continuous.

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6.0 REFERENCES
Capps, R.W. (1993). Consider the Ultimate Capacity of Fractionation Trays. Chem.
Eng. Prog, 89 (3), 37-42.

Kim, K.J., & Diwekar, U. (2005). Batch Distillation. Chicago: University of Illinois.

Kister, H.Z., & Townsend, R.W. (1984). Ethylene from NGL Feedstocks for Low-
pressure 𝐶2 Splitter. Hydro. Proc., 63 91), 105-108.

Liu, Z.Y., & Jobson, M. (1999). The Effect of Operating Pressure on Distillation
Column Throughput. Computers and Chemical Engineering Supplement, 23, 831-
834.

SRS Engineering Corporation. (2016). How Columns Work?. Retrieved from

www.srsengineering.com at February 22, 2019

Tham, M.T., & Costello, R.C. (2018). Distillation: An Introduction. Retrieved from
www.rccostello.com at February 22, 2019

Winkle, M.V. (1967). Distillation. McGraw-Hill, New York, p 168.

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