CEB 2072 Chemical Engineering Laboratory II

May 2022 Semester

21 June 2022

EXP 6: Batch Packed Distillation

GROUP 3D

NO. NAME STUDENT ID

1. Poh Ching Hong 19001325

2. Sashivarma A/L Saravanan 19001215

3. Mohamad Hafiz Fahmi bin Ahmad Shafie 19001324

4. Nur Athirah Munirah binti Mohd Fakhrurrozie 19001337

5. Wan Nur Alya binti Wan Abdul Manan 19001320

Chemical Engineering Department

Universiti Teknologi PETRONAS
 Table of Contents
1.0 Introduction & Objectives.................................................................................................... 1
1.1 Introduction ...................................................................................................................... 1
1.2 Objectives ........................................................................................................................ 4
2.0 Methodology/Experimental Procedures............................................................................... 5
3.0 Results & Discussion ......................................................................................................... 10
3.1 Results ............................................................................................................................ 10
3.1.1 Preparation of a Refractive Index (RI) vs Composition Plot .................................. 10
3.1.2 Experiment 1: Batch Distillation at Total Reflux ................................................... 13
3.2 Discussions .................................................................................................................... 17
4.0 Conclusion ......................................................................................................................... 19
5.0 References .......................................................................................................................... 20

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 1.0 Introduction & Objectives

1.1 Introduction
In the area of chemical engineering, the separation process is one of the necessary
processes that is extremely vital in plants, and this process always involves a lot of factors.
Additionally, it is one of the required processes for batch packet distillation unit. The
distillation column is one of the applications of the separation process. The distillation column,
which is separated into two segments (top column and bottom column), is one of the
applications of the separation process. Distillation processes are being established in order to
separate a mixture into two or more products based on variations in boiling point. Distillation
may also be used to purify organic liquids. In addition, to boost the purity of the product
created, a condenser at the top column and a reboiler at the bottom column will be used to re-
enter the various products formed into the distillation column. The liquid phase is less volatile
and has a higher boiling point, while the vapour phase is more volatile and has a lower boiling
point component. The distillation process is the most frequent separation utilised in industry
since it is known to be 90% efficient in separating and a substantial consumer of energy in the
necessary heating process.

Furthermore, the column that houses the distillation column is equipped with a wide
variety of trays, including bubble cap trays, filter trays, and packed bed columns. The principle
behind the bubble cap tray is a cross flow at each step, rather than a counter current flow, in
contrast to the flow pattern used by the sieve tray, which uses a counter current flow. In
addition, packing columns may have a reduced pressure drop and are an excellent choice for
handling liquids that are thermally sensitive. It will take into account the fouling propensity,
the permitted of pressure loss, and the turndown need in the column in order to decide which
tray is the most suited. These trays have typically been inserted within the distillation column
with the intention of boosting the purity of the product in response to an increase in the
resistance experienced inside the column. A good illustration of a tray is the figure.

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 Figure 1.1: Bubble cap tray working principle

Figure 1.2: example of sieve tray

In addition, the distillation process may separate the vapour phase from the liquid phase
by making use of the power provided by the heating process. A heating element that is put at
the base of the column serves to facilitate the evaporation of the liquid mixture across the whole
column. While the vapour phase travels upward into the condenser and the product travels
upward into the distillation tank, the liquid phase travels downhill as a waste or as bottom
products. Above the column that performs the distillation, there are two heat exchangers. The
vapour that is released from the first exchanger may be condensed by utilising the cooling water
provided by the second exchanger, which serves as its purpose. After that, the condensate that
flows from the condenser will be transferred into the reflux tank and it will be filled. The on/off
switching of the electromagnetic control in the column served as the control mechanism for the
reflux ratio. The residue that was left over from the reflux tank was transferred to the highest
point of the column. It is possible to do an analysis of the column's separating characteristics.

By the results of the analyses performed on the samples at each step. Consequently, the
value of the sample's refractive index was determined using a refractometer. The transfer of

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mass from one phase to the other during equilibrium constitutes the rectification process. In
the distillation column system, there are two primary methods that need to be followed in order
to carry out the experiment successfully. These methods are the batch distillation technique
and the continuous steady state distillation process. The batch distillation process is the process
that is used when there is no reflux and the vapour that is boiling the liquid mixture to be
separated and condensing vapour without allowing any liquid to return into the top column.
Batch distillation is the process that is used to separate liquids from liquid mixtures. As a result,
the process of continuous distillation is an example of vice versa. Both flash distillation and
rectification distillation are types of continuous distillation. Flash distillation is also known as
single-stage partial vaporisation. In contrast, only the batch distillation procedure will be
carried out in this particular experiment in order to separate the combination of ethanol and
water based on the disparities in their respective boiling points.

Figure 1.3: Process flow diagram for common distillation column process
Lastly, in the business world, there are a wide variety of product categories that rely on
distillation as a separation method. Some examples of these are petroleum refining,
petrochemical production, the processing of natural gas, and beverage production. The
common objective is to separate the light components from the heavier ones in the mixture.
Another industry that makes use of the distillation process is the food industry, where it is used
to remove odours from fats and oils while also concentrating essential oils and flavour.

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1.2 Objectives
Experiment 1:
I. To determine the height equivalent theoretical plates (HETP) at total reflex
II. To study the effect of the liquid and vapor loading on the height equivalent theoretical
plates (HETP) at total reflux

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 2.0 Methodology/Experimental Procedures

Figure 2.0: Process Flow Diagram for batch packed distillation unit.

Material:
a) Laboratory tap water
b) Ethanol-water mixture
Apparatus:
a) Evaporator
b) Control Panel
c) Main Cooling water valve
d) Refractometer
e) Product vessel

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General Operating Procedures

1. Valves Positions – Initially, all valves are closed except the vent valves.
2. Cooling Water System - Laboratory tap water is used as the cooling media. Hose
connections are such that the cooling water enter both the top condenser (W3) and
product cooler (W4) in parallel. Both cooling water flow rate were adjusted to maximise
cooling and condensation. The temperature of the cooling water leaving the two units
should not exceed 45°C.
3. Heater Power – The heater output power is adjustable between 0 and 100% so that one
may vary the flow rate of the vapor and liquid inside the distillation column. The heater
resistance knob located at the control panel was turned between a value 0 to 10.
4. Reflux Divider – The reflux divider controller KS-01 has 3 positions with the following
settings:
a) Position 0 : Total reflux
b) Position Hand : Total distillate offtake
c) Position Auto : Timer controlled reflux

The reflux timer and distillate timer were set on the control panel at KS-01 in order to
adjust the reflux ratio. The reflux timer is represented by the time in seconds on the
display, while the distillate timer is represented by the time in seconds with an
additional blinking light at the lower right corner of the display. The reflux ratio is equal
to the ratio between the total reflux time and the total offtake time.

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2.1 General Start-Up Procedures

1. All valves are ensured to be closed except valve (V3) and ventilation valve (V6).
2. A 15 L mixture containing ethanol and filtered water was prepared at the desired
composition. The charge port cap was opened and the evaporator B1 was charged with
the ethanol-water mixture. The charge port cap was closed.
3. The main power on the control panel was turned on.
4. The reflux divider was set to total reflux in order to prevent any distillate from escaping
when starting up the distillation unit.
5. The main cooling water valve V10 was opened. Valves V8 and V9 were opened in
order to let the cooling water flow into the condenser (W3) and distillate cooler (W4).
A flow of at least 20 L/min at the condenser and 10 L/min flow at the distillate cooler
were maintained.
6. The cartridge heaters W1 & W2 were switched on and the heater power was set to
100%. The liquid in the evaporator was allowed to boil. As the liquid boils, the liquid
level in the evaporator started to drop. The level switch was adjusted to ensure that the
tip of the level switch is above the cartridge heater.
7. The vapor rising from the boiling liquid into the column was observed. As the vapor
reaches the condenser, it condensed and flow back into the column as liquid. Mass
transfer took place between this liquid and vapor phase in the column.
8. If flooding was observed in the column (liquid being held up by the flow of vapor in
the packings), the vapor flow rate was reduced by reducing the heater’s power.
9. The condenser has been checked to have sufficient cooling water flow to minimize
escape of vapor into the vent.
10. The distillation unit was left for approximately 30 - 40 minutes until a stable condition
was observed. The stable condition was reached when all the temperature indicators on
the column give a constant reading with an allowable ± 0.2°C fluctuation.

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2.2 General Shut-Down Procedures

1. The reflux divider was set to total reflux.

2. The cooling water was kept running through the condenser (W3) and distillate cooler
(W4).
3. The cartridge heaters W1 & W2 were switched off. The temperature drop in the
evaporator was monitored and waited until it has cooled down to room temperature.
4. All liquid from the evaporator B1 and product vessel B2 were drained.
5. The cooling water valves V8, V9 and V10 were closed.
6. The main power was turned off on the control panel.

2.3 Preparation of a Refractive Index (RI) vs. Composition Plot

1. A set of mixtures containing ethanol and water was prepared within a specified range
of composition between pure water and pure ethanol. The sample table in Appendix A
was referred.
2. The refractive index (RI) readings for each mixture were obtained using a
refractometer.
3. A plot of RI vs. composition was prepared for the whole range of mixtures. This served
as the calibration curve for further experiments.

2.4 Sampling Procedures

Samples can be taken from the distillate and the bottom product for analysis:

1. Distillate sampling:
a) Sampling valve V2 was opened to drain the sample line of any remaining liquid.
b) A vial was placed below valve V2.
c) The reflux divider was set to total distillate for a few seconds.
d) A 10 mL sample was collected and sampling valve V2 was closed.
e) The reflux divider was switched back to total reflux.

2. Bottom sampling:
a) A vial was placed below valve V1.

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 b) Sampling valve V1 was opened, and a 10 mL sample was collected. The hot liquid
was handled carefully while collecting a sample.
c) Sampling valve V1 was closed.
d) The sample was cooled down by immersing the sample vial in cold water.

Note: The samples in vials were collected with cap to avoid excessive evaporation of
ethanol before analysis.

Experiment 1: Batch Distillation at Total Reflux

PROCEDURES:

1. The general start-up procedures (Section 2.1) were performed.

2. The top and bottom temperatures were recorded once the distillation unit has reached
stable condition.
3. The samples from the distillate and bottom product were collected (Section 2.4).
4. The refractive index for both samples were measured, and their compositions were
determined.
5. For different liquid and vapor loading, the heater power settings were adjusted in W1
and W2. As a result, it decreased the heating duty and hence decreased the vapor flow
in the column. Consequently, the liquid flow also decreased.
6. The heater power settings were changed and waited for approximately 15 mins to allow
the distillation unit to achieve stable condition. Then, steps 2 to 5 were followed.

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 3.0 Results & Discussion

3.1 Results
3.1.1 Preparation of a Refractive Index (RI) vs Composition Plot
1) Determination of molar volume of ethanol and water

Table 3.1: Properties of pure components

Molecular Weight Molar Volume

Component Specific Gravity
(g/mol) (L/mol)
Ethanol 46.07 0.789 0.05839
Water 18.02 1.000 0.01802

𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡
Molar volume =
𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝑔𝑟𝑎𝑣𝑖𝑡𝑦 × 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟

𝑔
46.07
Molar volume (ethanol) = 𝑚𝑜𝑙
𝑔 = 0.05839 𝐿/𝑚𝑜𝑙
0.789 × 1000 𝐿

𝑔
18.02
Molar volume (water) = 𝑚𝑜𝑙
𝑔 = 0.01802 𝐿/𝑚𝑜𝑙
1.000 × 1000 𝐿

2) Determination of mole fraction given the volume of ethanol and water

Formula used:

𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 𝑖
𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 𝑖 =
𝑚𝑜𝑙𝑎𝑟 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 𝑖

𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 𝑖

mole fraction 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 𝑖 =
𝑡𝑜𝑡𝑎𝑙 𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑚𝑜𝑙𝑒

Sample calculation for volume of ethanol = 1.0 mL and volume of water = 9.0 mL,

1.0 𝑚𝐿 1𝐿
𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 = ( ) = 0.0171 𝑚𝑜𝑙
0.05839 𝐿/𝑚𝑜𝑙 1000 𝑚𝐿

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 9.0 𝑚𝐿 1𝐿
𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 = ( ) = 0.4994 𝑚𝑜𝑙
0.01802 𝐿/𝑚𝑜𝑙 1000 𝑚𝐿

0.0171 𝑚𝑜𝑙
mole fraction 𝑜𝑓 𝑒𝑡ℎ𝑎𝑛𝑜𝑙 = = 0.0331
0.0171 𝑚𝑜𝑙 + 0.4994 𝑚𝑜𝑙

0.4994 𝑚𝑜𝑙
mole fraction 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 = = 0.9669
0.0171 𝑚𝑜𝑙 + 0.4994 𝑚𝑜𝑙

Table 3.2: Data of Preparation for Refractive Index Vs Composition Plot

Volume of Volume of Water Mole Fraction of Mole Fraction of Refractive Index,

Ethanol (mL) (mL) Ethanol Water RI

0 10 0.0000 1.0000 1.33299

1.0 9.0 0.0331 0.9669 1.33695

2.0 8.0 0.0717 0.9283 1.34177

3.0 7.0 0.1168 0.8832 1.34860

4.0 6.0 0.1706 0.8294 1.35415

5.0 5.0 0.2357 0.7643 1.35804

6.0 4.0 0.3165 0.6835 1.36013

7.0 3.0 0.4186 0.5814 1.36267

8.0 2.0 0.5524 0.4476 1.36363

8.5 1.5 0.6364 0.3636 1.36356

9.0 1.0 0.7352 0.2648 1.36330

9.5 0.5 0.8545 0.1455 1.36258

10.0 0.0 1.0000 0.0000 1.35976

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3) Calibration curve

Graph of Refractive Index vs Mole Fraction of Ethanol

1.3750

1.3700

1.3650

1.3600
Refractive Index (RI)

1.3550
y = 0.0252x + 1.3445
R² = 0.5936
1.3500

1.3450

1.3400

1.3350

1.3300
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
Mole Fraction of Ethanol

Figure 3.1: Graph of refractive index against mole fraction of ethanol

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3.1.2 Experiment 1: Batch Distillation at Total Reflux
Height of column = 1120 mm
Table 3.3: Data for Batch Distillation at Total Reflux

Distillate Bottom Product

Heater Number of
HETP
W1, W2 Temp Refractive Mole Temp Refractive Mole theoretical
(mm)
Power plates
(ͦ C) Index Fraction (ͦ C) Index Fraction

100 % 78 1.36272 0.42 81.5 1.36255 0.41 1 1120

80 % 77.9 1.36277 0.43 81.3 1.36185 0.38 1 1120

60 % 77.7 1.36276 0.43 81.3 1.36179 0.38 1 1120

40 % 77.6 1.36273 0.43 81.3 1.36170 0.37 1 1120

20 % 77.4 1.36263 0.42 81.3 1.36207 0.39 1 1120

Sample calculation (For Heater W1, W2 Power = 100 %):

1) Determination of Mole Fraction of Ethanol

From Figure 3.1, the mole fraction of ethanol is determined accordingly as shown
below:

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As the Refractive Index of distillate is 1.36272, its mole fraction is determined to be 0.42. As
the Refractive Index of bottom product is 1.36255, its mole fraction is determined to be 0.41.

2) Determination of number of theoretical plates

Table 3.4: Equilibrium data for ethanol-water system at 1 atm

Mole fraction ethanol

Temperature (°C)
Liquid phase Vapor phase
100.0 0.0000 0.0000
95.5 0.0190 0.1700
89.0 0.0721 0.3891
86.7 0.0996 0.4375
85.3 0.1238 0.4704
84.1 0.1661 0.5089
82.7 0.2337 0.5445
82.3 0.2608 0.558
81.5 0.3273 0.5826
80.7 0.3965 0.6122
79.8 0.5079 0.6564
79.7 0.5198 0.6599
79.3 0.5732 0.6841
78.7 0.6763 0.7385
78.4 0.7472 0.7815
78.2 0.8943 0.8943

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 X-Y Equilibrium Diagram for Ethanol-Water System at 1 atm
1.0000

0.9000

0.8000

0.7000
Vapor mol fraction

0.6000

0.5000

0.4000

0.3000

0.2000

0.1000
Mol fraction of bottom Mol fraction of
product = 0.41 distillate = 0.42
0.0000
0.0000 0.1000 0.2000 0.3000 0.4000 0.5000 0.6000 0.7000 0.8000 0.9000 1.0000
Liquid mol fraction

Figure 3.2: X-Y Equilibrium diagram for ethanol-water mixture at 1atm

By using McCabe-Thiele method, the number of theoretical plates is determined to be 1.

3) Determination of height equivalent theoretical plates (HETP)

ℎ𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑐𝑜𝑙𝑢𝑚𝑛 1120 𝑚𝑚

𝐻𝐸𝑇𝑃 = = = 1120 𝑚𝑚
𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑝𝑙𝑎𝑡𝑒𝑠 1

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 4) Graph of HETP vs heating power

Graph of HETP vs heating power

1200

1000

800
HETP (mm)

600

400

200

0
0 10 20 30 40 50 60 70 80 90 100
Heating Power (%)

Figure 3.3: Graph of HETP vs heating power

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3.2 Discussions
In the first part of the experiment, the objective is to determine the height equivalent
theoretical plates (HETP) at total reflux of heater power ranging from 100% to 20%. According
to BAI, Song, Sheng and Li (2010), the total reflux is defined as the operating condition that
the vapor and liquid reactants are passing each other in the distillation column but no product
is removed. Firstly, 13 set of mixtures containing ethanol and water within a specified range of
composition between pure water and pure ethanol were prepared to plot the calibration curve.
The calibration curve is a graph of refractive index vs the mole fraction of ethanol to assist the
determination of the mole fraction of ethanol at the entire distillate and bottom product. During
the experiment, a refractometer was used to obtain the refractive index (RI) readings that will
be tabulated in Table 3.1 along with the calculated mole fractions for ethanol and water in the
appendix.

According to the plotted calibration curve in Figure 3.1, the curve gradually increases
before decreasing at a slow pace until the ethanol composition reaches 1. The refractive index
is increasing with the mole fraction of ethanol until it reaches 1.36363 at mole fraction of
ethanol at 0.5524, from there it slowly decreases until it reaches at mole fraction of ethanol at
1.0 and RI reading at 1.35976. According to Guo et al. (2014), the RI will be different for
differed fluid as it is a function of fluid composition and density. Theoretically, higher
refractive index indicates higher amount of the component in the mixture. In short, when the
density of a component increases, the reading of refractive index also increases. In our case,
the refractive index indicates the amount of ethanol in the mixture. Based on the graph, this
relationship was proven and hence, the calibration curve from Figure 3.1 serves as a calibration
curve for the Experiment 1which is Batch Distillation at Total Reflux that is being carried out
in Batch Packed Distillation experiment.

Furthermore, it was observed that when the heater power reduced gradually from 100%
to 20%, the temperature of the distillate decreased. This is due to the decrease in the heater
duty which resulted in less heat being transferred to the ethanol-water mixture. Moreover, it
was also observed that the temperature of the distillate product is slightly lower than the
temperature of its corresponding bottom product. This is because the bottom products consist
of less volatile components that have higher boiling point temperatures.

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 Subsequently, the theoretical number of plates in the distillation column was
determined by using the McCabe-Thiele method as shown in Figure 3.2. It was found that the
theoretical number of plates of a batch distillation at total reflux was one plate regardless of the
changes in the heater power. This was attributed to the total reflux condition in which all the
vapour that travelled to the top of the distillation column was condensed and recycled back into
the column. As a result, the separation process of the ethanol-water mixture was optimised and
at total reflux, the number of theoretical plates required is a minimum.

Moreover, the height equivalent theoretical plates (HETP) at total reflux were
determined by dividing the effective column height with the number of theoretical plates. Since
the number of theoretical plates at different heater power is one, the HETP for all various
heating power has the same value as the effective column height, that is, 1120 mm. Therefore,
it can be concluded that the liquid and vapour loading at different heater power does not affect
the HETP value if the number of theoretical plates of the distillation column is one.

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 4.0 Conclusion

In conclusion, this experiment is about a distillation process which is one of the oldest
and efficient separation process applications that is widely used in the industry. It is a
crucial process which involves the separation of a mixture that is mainly based on the
difference in the boiling point of the components where the components in the mixture will
be separated into two parts which are the top and bottom products. In addition, distillation
processes are done to also purify organic liquids. In this experiment, students are tasked to
determine the height equivalent theoretical plates (HETP) at total reflex and to study the
effect of the liquid and vapor loading on the HETP at total reflux.

From the results obtained, a calibration curve was plotted where it is seen that the curve
is gradually increasing up until one point which is at refractive index (RI) of 1.36363 before
it starts to decrease slowly to RI = 1.35976 when mole fraction of ethanol is equal to 1. The
recorded RI values are actually indicating the amount of ethanol in the mixture.
Theoretically, if the density of a component which expresses the amount of the component,
increases, the reading of refractive index will also increase, hence, from the results attained,
our data is provenly correct. The calibration curve for the Batch Distillation at Total Reflux
in this experiment is plotted as shown in Figure 3.1 in Results & Discussion section. In
addition, from the experiment, it is also observed that the distillate segment has higher
temperature than the bottom segment in the distillation unit which is due to the lower
volatility of the components in the bottom products which have higher boiling point
temperatures.

Morevover, McCabe-Thiele method is being applied to determine the theoretical

number of plates in the distillation column whereby in in this experiment, the theoretical
number of plates of a batch distillation at total reflux is found to be one plate. Subsequently,
the height equivalent theoretical plates (HETP) at total reflux are determined which is
calculated to be 1120 mm and are the same for all various heating power since the number
of theoretical plates at different heater power is the same (equal to one). Hence, it is deduced
that if the number of theoretical plates of the distillation column is one, the liquid and
vapour loading at different heater power will not affect the HETP value at total reflux.

In short, all objectives of this experiment are successfully achieved and the theories in
this experiment have been proven appropriately.

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 5.0 References

Basic equipment and operation of distillation columns. (n.d.). Retrieved June 27, 2022, from
https://www.rccostello.com/distil/distileqp.htm

S., W. (n.d.). Distillation column internals. Distillation Column - Column Internals, Bubble
cap trays, Valve trays, Sieve trays, Structured packing. Retrieved June 27, 2022, from
https://www.wermac.org/equipment/distillation_part2.html

S., W. (n.d.). What is a distillation column? Distillation Column - Basic Distillation Equipment
and Operation. Retrieved June 27, 2022, from
https://www.wermac.org/equipment/distillation_part1.html#:~:text=A%20distillation%
20column%20is%20an,as%20large%20scale%20industrial%20distillations.

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