Group Number 3

Date of Experimentation 7/11/2019

Time of Submission
Name Lab Report
21/11/2019
Chong Jiu Li
Names of Group Members Goh Ke Xin
20003217
10280095

Distillation I
Sulaksanath Gunenthiran 20090152

The Batch Distillation of a Binary

Mixture of Methanol-Isopropanol

Chong Jiu Li
ebyjc3@nottingham.edu.my
 Table of Contents

Table of Contents...........................................................................................................1

Summary.................................................................................................................2

Introduction.............................................................................................................3

Experimental Procedure..........................................................................................4

Result and Discussion.............................................................................................7

Conclusion............................................................................................................13

Reference..............................................................................................................14

Appendix...............................................................................................................15

1
Summary

The intention of this experiment is to learn about the batch distillation under the laboratory scale at a

constant rate of reflux ratio, where the equipment was first operated at 100 per cent reflux ratio and started

to lower the reflux ratio until a new set point 60 per cent. Batch distillation of the binary mixture of

Methanol-Isopropanol was carried out for a period of time. The samples were obtained from both the

evaporator tank and the reflux divider vessel within the time frame of 15 minutes.

Based on the data collected, the results indicated that both the mole percentage composition of methanol

from the evaporation tanks and reflux divider vessel decrease with time as the refractive index of the

obtained samples were increasing. Besides that, there is a general trend of decreasing of the temperature as

the liquid moving upward along the distillation column. Furthermore, the McCabe-Thiele Graphical method

was used to determine the number of stages theoretically. Based on the theoretical results the efficiency of

the batch distillation column could be determined as well as whether the optimum number of stages is used.

To conclude, the mole percentage composition of methanol declines with time-based on the outcome of

the batch distillation of binary Mixture of Methanol-Isopropanol. The temperature profile indicates a

decreasing trend while moving up within the distillation column. Additionally, the number of stages of

determined by the McCabe method, the discussion for improving the efficiency and yield of the more

volatile component would be included.

2
Introduction

Distillation is one of the most popular methods among all separation processes which is able to apply to

most of the industries. There are two types of Distillation, Continuous Distillation and Batch Distillation.

Continuous Distillation operates with the feed continuously fed inside the distillation column and operates

under the steady-state, which is economically and environmentally friendly and ideal for large scale

production with constant composition. Batch Distillation is known as distillation in steps or in batches,

which is suitable for small quantity (Narvaez-Garcia et al. 2013). Batch distillation is suitable for separation

and “in the production of fine and speciality chemicals, pharmaceuticals, polymers and biochemical

products either for purification or recovery of small quantity and valuable solvent” (Sorensen 2014).

Batch distillation is one of the oldest separation techniques, it produces a single unit solution and able to

carry out the batch identity which is good for those productions that have high-quality control requirement.

However, the biggest advantage of the batch distillation is its ability to deal with various separation duties,

for instance, changes of feed composition or targeted product composition, by simply changing the operating

condition of the distillation column will be able to cope with the situations mention above. Even though

Batch Distillation has a lot of advantages such as simple, batch-wise, it still not ideal for larger-scale

production as it demands more energy compare to the continuous column.

Batch Distillation process started with loading the feed to the boiler, after the total reflux operation

where all the condensates recycle back to the column, the distillate was extracted, and the bottom left with

the more concentrated less volatile component. In this experiment the distillation is run under the 60% reflux

ratio, the sample was extracted from both the reflux divider vessel and evaporation tank with a time span of

15 minutes. The composition of methanol was determined by the refractometer by measuring its refractive

index and obtain by cross-reference with the refractive index calibration curve for Methanol-Isopropanol.

3
Experimental Procedure

Before entering the procedure, the equipment and material required in this experiment would be

introduced. The main equipment used is the Batch Distillation Rig, where the 7-plate sieve-plate column has

been fitted and 13 thermometers to monitor the temperature over the column. The second equipment used is

the refractometer, which exam the sample and provide the reflective index. Furthermore, the measuring

cylinder was used for measuring the volume of the top product which is from the reflux divider vessel. The

raw material in this experiment is 8 litres of Methanol-Isopropanol. The cooling agent for this experiment is

water which condensates the vapour into liquid in the condenser with a rate of 120 litres per hour.

8 litres of the binary mixture of Methanol-Isopropanol is measured via measuring cylinder before

inserting into the evaporator, a funnel is recommended. A small sample (approximately 15ml) would be

retained in the beaker for testing of the refractive index. The vacuum pump was shut by the hand valve for

regulating the vacuum pump (11) and the hand valve for atmospheric/vacuum (14a) was opened. The

cooling stream was introduced to the system first by turning on both the valves for inlet and outlet cooling

stream.

4
 Figure 1: The schematic representation of the rig.

Figure 2: The control panel of the rig.

The main power switch was turned on in order to let the rig operate, at first the reflux ratio was set to

total reflux which is reflux ratio is 100%. The setting on the temperature controller was set to manual while

the heater switch was turned on to 18 heating power. The temperature sensors on the rig were monitored

instantaneously. The heating power would be lower to 14 when the mixture boil and the temperature reading

for T13 reach 70 degrees Celsius.

The timer will start for 15 minutes when there is product appear in the reflux divider. All the sample

from the reflux divider will be drained after a quarter of an hour as well as a small sample from the

evaporator. The volume extracted from the reflux divider would be measured by measuring cylinder while

all the monitors’ temperature will be recorded. The sample will undergo the refraction index test.

5
 The reflux ratio was then set to 60 % and based on the same time interval for 15 minutes. But instead of

a single result, it requires three continuous results, therefore the second stage of the experiment would last

for 45 minutes, 3 samples will be collected. The temperature along the distillation column from T1 to T13

were recorded. The refractive index of the samples were all measured with a refractometer. Small samples

around 15 ml from the reflux divider vessel and evaporator were obtained at regular intervals of 15 minutes

and the volumes of the samples were recorded.

After the 45 minutes, the master switch was turned off, all the sample withdrawn were poured back into

the original storage container, followed by shutting the inlet and outlet valve for cooling water supply. the

content of the evaporator would be empty into its original storage tank as well when its temperature drops.

To sum up, the temperature and refractive index was recorded at the required reflux ratio and scheduled

time intervals.

Reflux ratio Time Data Should be collected

(%) (min)

N/A T0 The initial sample for Refractive index

100 T1

60 15
Temperatures for all thermometer
60 30

60 45 Volume & Refractive Index Value for Reflux Divider Vessel

60 Tf
Refractive Index Value for Evaporator

Table 1: the data should be collected according to the time intervals as well as the required reflux ratio.

The Batch Distillation was operated at the atmospheric pressure of 1 atm (760mmHg)
6
 Results and Discussion

The results indicate that the refractive index in the reflux divider vessel with different time period are

1.3365, 1.3515, 1.355 and 1.3565. Whereas, the refractive index in the evaporator at different times are

almost the same 1.3675, 1.3675, 1.3685 and 1.3678. The percentage mole of methanol in the samples was

determined based on the refractive index by referring to the refractive index calibration curve for methanol-

isopropanol. Thus, the percentage mole of methanol in the reflux divider vessel at different times are 88%,

65%, 61% and 57%. Whereas the percentage mole of methanol in the evaporator at different times are 33%,

33%, 26% and 30%.

The results show there is a decreasing trend of the temperature from T2 to T9 while moving up the

distillation column, however, at T6 the temperature fluctuate and drop significantly but recovered at T7 still

show a general decreasing trend.

Sample Time Refractive index Percentage mole of methanol (%)

(min)
Reflux divider vessel Evaporator Reflux divider vessel, XD Evaporator, XS

1 T0 - 1.3675 30 -

2 T1 1.3365 1.3675 88 33

3 15 1.3515 1.3675 65 33

4 30 1.3555 1.3685 61 26

5 45 1.3565 1.368 57 30

6 Tf 1.3565 1.368 57 30

Table 2 Refractive Index and Percentage of Methanol based on Refractive Index Calibration Curve

7
Mole Percentage of Methanol in Reflux Divider Vessel and Evaporator at Different time
100
90
Mole Percentage of Methanol (%) 90

80
69
70
61
60 57 57

50

40
33 33
30 30
30 26

20

10

0
T1 15 30 45 Tf

Time

Reflux Divider Vessel Evaporator

Table 3 Graph of the Mole Percentage of Methanol in Reflux Divider Vessel and Evaporator at different
times.

From the table above, Overall the mole percentage from the reflux divider vessel is higher than that of

the evaporator tank. Which is expected as the Methanol is the more volatile component (MVC) and

evaporate in the evaporation tanks and shifting to the top of the column. The Mole Percentage of the

methanol also display a general decreasing trend with the time. For the Evaporator the Mole Percentage of

Methanol show a trend of decrease but not much decline in the number of moles, this is due to the effect of

distillation where the MVC, methanol evaporated, leaving the evaporation tank with LVC, however there

are 8 litres of liquid entering the Evaporation tank, the effect of distillation is minor which results in small

change in the mole percentage in the Evaporator. As the reflux ratio fixed at 60%, the overhead composition

varies, the mole percentage of methanol decrease in the evaporation tank, less methanol is vaporized to the

reflux divider vessel, as a result, the composition of the Methanol in reflux divider vessel decrease. As the

process continues, both the top and bottom composition for MVC will decrease (Diwekar and Kim 2005).

Tray The temperature of trays at different times (°C)

8
 Trend of Temperature along the Tray
79 T1(100% Reflux) 15 min (60%) 30 min (60%) 45 min (60%)

1 78 78.4 78.5 78.5 78.7

2 77.0 78.3 78.2 78.6

77
Temperature (°C)

3 77.0 78.3 78.2 78.6

76
4 76.7 78.0 78.0 78.4
75
5 76.6 78.0 78.1 78.5

6 74 74.8 76.6 76.6 76.9

7 73 75.6 77.5 77.5 77.8

8 74.8 77.0 77.0 77.2

72
2 3 4 5 6 7 8 9
9 75.2 76.3 76.2 76.3
Tray Number
10 26.2 28.5 28.9.7 29.4

11 15.1
100% Reflux 14.7
60% Reflux 15min 14.8
60% Reflux 30min 60% Reflux 45min15.0

12 19.4 19.4 19.5 20.2

13 74 74.8 74.8 75.0

Table 4: Temperature of trays at different time

Table 5 Trend of temperature along the Tray 2 to Tray 9

The two tables above show the temperature profile obtained during the distillation from the table, there

is a trend of decreasing of the temperature as the vapour moving up the distillation column, it could be

explained by the vapour is moving away from the boiler and start to enter the condenser at the top. The

temperature of the evaporator is maintained below 80°C, which is below the boiling point of the LVC

(Isopropanol), as a result, it minimized the evaporation effect of LVC and kept at the evaporator tank.

On the other hand, keeping the temperature of the evaporator below 80°C ensure the process could be

carried out properly as the boiling point for the more volatile component Methanol is 64.7 °C. the

temperature will guarantee the efficiency of the process. As the vapour reaches the top of the distillation

column the temperature is still maintained above 64.7°C which is still higher than the MVC boiling point

9
that ensures the process could be carried out properly, by prevent the MVC condensed before entering the

condenser or flow back to the evaporator.

There might be some errors in the experiment, one of them is the Parallax Error, as we used the

measuring cylinder to measure the volume of the extracted solution. They might have residue within the

measuring cylinder, or the solution would evaporate during the process, the parallax error would also occur

when obtaining the results visually. Furthermore, the parallax error would occur when operating the

refractometer, the border would hard to determine, therefore the results might vary.

Besides that, human error would also take place while using the stopwatch. There will be a time delay

when the following stopwatch, as human have reaction time. In addition to this, another possible source of

error is the error from the machine itself, the readings of the temperatures on the control panel kept

fluctuating from T1 to T13. Thus, it was hard to determine which temperatures were the correct and

appropriate for each tray. Last but not least, the equipment should be calibrated as the binary mixture of

methanol-isopropanol was used repeatedly, it might have impurities or contamination within the solution

and that would affect the accuracy of the data.

There are discrepancies at the amount of methanol, the initial number of moles of methanol does not

equal to the final number of moles of methanol. Here are some possible reasons, the reaction is carried out,

the vapour might escape where the valve is loosened. The parallax error would be another source of error as

the volume of sample is measured by the measuring cylinder and the refractive index is determined by the

refractometer, the border of the colour changes would hard to determine and affect the refractive index of

the methanol. Furthermore, while extracting the sample from the evaporator the sample is still hot, the

process of evaporation would still be taking place, therefore the results may not be accurate. Last but not

least, as the Methanol-Isopropanol is recycled used, there might be impurities existed.

10
 One of the possible pathways to improve the yield and the efficiency of the distillation, as the

composition of top component is relatively fixed, the only solution for increasing the reflux ratio, as the

reflux ration increase, the gradient to the operation will tend to go toward 1, as a result, the more MVC will

be recycled back to the distillation column, as a result the process will results in higher composition which

result in higher yield, yet the method is not practical in the real life as the reflux ratio is too high, it will not

be economically friendly. Furthermore, adjusting the volume of the vapor flow would also result in changes

of separation efficiency, too much vapour will result in liquid entrained in the upper column results in

depletion of distillation capacity and increase of pressure which called flooding, if the vapour is too thin the

liquid in the upper plate will no receive enough support ad fall back, which also decrease the efficiency

(Tham 1997). Last but not least we could make improvement on the equipment itself by replacing the sieve

tray to valve tray which has a bigger surface area, or adjusting the diameter of the column, or changing the

packed column to increase the efficiency.

11
The optimum number of stages

Table 6 The McCabe Thiele table for this Experiment

In the experiment conducted, the number of trays used was 7.

McCabe Thiele method is used, in order to determine the optimum number of stages used in this

experiment. The operating line with gradient of 0.63 and 0.252 for y-interception is drawn. The optimum

number of stages used can be determined. Based on table 6, the results show the optimum stages in this

experiment should be 5. The step of the calculation is in the appendix.

5
Efficiency (%) ×100 % ≈ 71.43 %
7

12
Conclusion

This experiment was operating under the condition of constant reflux ratio of 60%. The outcomes of the

experiment indicate the composition of the top product changes according to time. Furthermore, the mole

percentage of methanol in both reflux divider vessel and evaporator decline with time. It also illustrates that

the temperatures decreased while the vapour moving up the distillation column.

Errors exist throughout the experiment, for instance, the parallax error which took place when

measuring the volume of the solution and refractive index. Human error due to the reaction time when

operates with a stopwatch. Lack of insulation of the distillation column or calibration also would vary the

precision of the results. Beside

McCabe Thiele diagram was used to determine the optimum number of stages, 5 stages were obtained.

The efficiency of this Batch distillation column is 71.43%. The yield of the MVC or efficiency of the

distillation column is achievable by simply changing the diameter of the distillation column, preventing

flooding and weeping by adjusting the vapour flow. Besides that, valve tray, bubble tray and packed column

are recommended to improve the efficiency. Increasing the reflux ratio throughout the process would reach

targeted purity.

In this experiment, errors occurred, such as parallax error; measuring the volume of the solution and human

error due to the human reaction time when using the stopwatch. Lack of heat insulation and Calibration of

the distillation column also will influence the accuracy and percision of results.

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References

Diwekar, Urmila, and Ki-Joo Kim. 2005. “Batch Distillation.” In , 107–50.

http://www.crcnetbase.com/doi/abs/10.1201/9781420028164.ch5 (November 19, 2019).
Narvaez-Garcia, Asteria, Jose Del Carmen Zavala-Loria, Luis Enrique Vilchis-Bravo, and Jose Antonio
Rocha-Uribe. 2013. “Design of Batch Distillation Columns Using Short-Cut Method at Constant
Reflux.” Journal of Engineering (United States) 2013.
Sorensen, Eva. 2014. “Design and Operation of Batch Distillation.” In Distillation: Fundamentals and
Principles, Elsevier Inc., 187–224.
Tham, M.T. 1997. “Factors Affecting Distillation Column Operation.” COSTELLO.
https://www.rccostello.com/distil/distilop.htm (November 21, 2019).

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Appendix

15
 Raw Data from the Experiment

Table7 : Table for the vapor-liquid equilibrium data for methanol-2-propanol at 1atm (760mmHg)
Table 8: Refractive Index Calibration Curve for Methanol-Isopropanol

16
 Time (min) Percentage mole of methanol (%)

Reflux divider vessel, XD Evaporator, XS

15 65 33

30 61 26

45 57 30

Average 61 29.67

Table 9: Calculation for the average percentage mole of methanol

Calculation Step

L L0
Reflex Ratio 0.6¿ =
L+ D V 1

400
¿ =1.5
R= 800
3

XD
Y-intercept =
R +1

Yn+1=0.63 Xn + 0.252

Average volume obtained

300+230+270 800
= =266.67
3 3

Average RI Value for Top obtained

1.3515+ 1.355+1.3565
=1.3543→ 0.63
3

Average RI Value for Top obtained

1.3678+ 1.3685+1.3675
=1.3646 →0.3
3

17
 Table10: Chemical Health Risk Assessment Form

Substance Name: Methanol-Isopropanol

SYNONYMS: Methanol-isopropanol
CAS Number: Storage location: Lab Used location: Lab
Suppliers name, address, telephone, and catalogue number: CHRA Reg. No By FSO*:
O
Cat. N .:

Hazard and risk information – retrieved from MSDS/CSDS

Hazard description: Toxic and flammable
Risk phrase description: Toxic to the human body if vapours are inhaled
Safety phrase description: Lab coat, goggles and face masks must be worn throughout the
experiment
Permissible exposure limit (PEL):
Degree of hazard guidelines
Hazard rating
Safety phrase Hazard Risk Phrase
(HR)
Green Relatively safe Not classified No known adverse health affect
HR1 as hazardous
Blue Can be carried Skin sensitizing R36 Irritating to eyes
HR2 out on the open Skin irritants R38 Irritating to skin
bench with R42 May cause sensitization by inhalation
caution R43 May cause sensitization by skin contact
Orange Can be carried Harmful R20 Harmful by inhalation
HR3 out on an open Corrosive R21 Harmful in contact with skin
bench with Irritant R22 Harmful if swallowed
caution Sensitising R30 Can become highly flammable in use
R34 Causes burns
R37 Irritating to the respiratory system
R40 Possible risk of irreversible effect/ Limited evidence of
a carcinogenic effect
R41 Risk of serious damage to eyes
Red Great care Very corrosive R23 Toxic by inhalation
HR4 necessary Toxic R24 Toxic in contact with skin
Carcinogenic R25 Toxic if swallowed
(category 2) R31 Contact with acids liberates toxic gas
Mutagenic R33 Danger of cumulative effects
(category 2) R35 Causes severe burns
Teratogenic R39 Danger of very serious irreversible effects
(category 2) R48 Danger of serious damage to health by prolonged
exposure
Gold Dangerous Very toxic R26 Very toxic by inhalation
HR5 Avoid exposure Carcinogenic R27 Very toxic in contact with skin
(category 1) R28 Very toxic if swallowed
Mutagenic R32 Contact with acids liberates very toxic gas

18
 (category 1) R45(1) May cause cancer
Teratogenic R46(1) May cause heritable genetic damage
(category 1) R47(1) May Cause birth defects
R49 May cause cancer by inhalation
Safety Analysis Checklist
Hazards to health
HR2 Sensitising HR2 Irritant HR3/4 Corrosive
HR3 Harmful HR4 Toxic HR5 Very Toxic
HR4/5 Teratogen HR4/5 Mutagen HR4/5 Carcinogen
Physicochemical properties
Biohazard HR2 Flammable HR3 Highly Flammable
HR4 Extremely Flammable HR4 Oxidizing HR5 Explosive
Exposure route
Inhalation Eye Skin
Ingestion Other NO YES
If YES, please state:
Factor increases the risk
Fine powder Fume
Containment classification
Local exhaust ventilation system (LEV) Fume hood
Others NO YES
If YES, please state:
Personal protective equipment (PPE)
Lab coat Eye protection Nitrile gloves
Chemical resistant
Face mask Respirator
glove
Other NO YES If YES please state:
Storage method: The mixture is stored in the container.
Disposal method: The waste was disposed of the waste container.
Accidental release measure –
The rig will be switched off immediately is spill or leak occurs.
spills/leaks:
Firefighting measure:
First aid measures
Eyes - Immediately flush eyes with plenty of water for 15 minutes, get medical aid
Skin - Immediately flush skin with plenty of water for 15 minutes, get medical aid
Ingestion - Get medical aid by medical personnel
Inhalation - Remove from exposure and move to fresh air immediately, get medical aid
Assesses by: Chong Jiu Li Signature: JiuliChong
Hp : 0178916128 Date:
Reviewed by project’s supervisor: Signature:
Reviewed by FSO*: Signature:
*FSO – Faculty Safety Office

19