PROGRAM OF CHEMICAL-BIOPROCESS ENGINEERING

SKTB 3731 section 01

SEPARATION LABORATORY I
2019/2020 – 02
EXPERIMENT : 1. PACKED DISTILLATION COLUMN

LAB INSTRUCTOR : Assoc. Prof. Dr. Chua Lee Suan

SECTION : 1
GROUP NO. : 1
GROUP MEMBERS No. Name NRIC
1. ADRIAN TEOH JIA WEI 971231075045
2. CHAN BAO LI 971015065766
3. CHAN CHUN CHEN 971102075049
4. CHAN HUI MIN 971108015768
5. CHAN YEN HENG 971126355002
DATE OF : 20/02/2020
PREPARATION
DATE OF : 23/02/2020
EXPERIMENT
REMARK (if necessary)

Grading

Criteria Score (%) Comment Total Mark

Cover Sheet 5
Abstract (300 words) 10
Background of the study 10
Experimental Procedures 20
Results and Discussion (include 30
chart, graph, table etc. for visual
interpretation)
Conclusion 10
References 10
Appendix (raw data sheet) 5
ABSTRACT

The objectives of this experiment was about determining the effect of time taken to
operate the packed distillation column with the composition and volume of distillate which was
methanol water mixture, and the relationship between volume of distillate and its composition
of two components in the distillate. Since there is a distinct boiling point between methanol and
water, therefore distillation separation technique was applicable to separate methanol water
mixture. Based on the experiment, different composition of methanol-water mixtures was
prepared to determine their refractive indexes respectively. A graph of refractive index versus
mole percent of methanol was plotted to determine the composition of methanol in the distillate
collected from the distillation column. The distillate samples were collected for 60 minutes
with every 5 minutes interval. The volume of samples was measured, and the refractive index
were determined to obtain the composition of methanol. From the results obtained, it showed
that the composition of methanol in the sample reached optimum level which was 93.01% at
the first 10 minutes and the volume collected was 290 cm3. After 10 minutes, the composition
of methanol in the sample and the volume remained at 98.48% and around 290 cm3. This can
be proved that the distillation process had reached steady and equilibrium state after 10 minutes.
TABLE OF CONTENTS
1.0 BACKGROUND OF THE STUDY .................................................................................... 1

Figure 1.1 Packing in distillation column ........................................................................... 2

2.0 METHODOLOGY .............................................................................................................. 3

2.1 Materials and Apparatus................................................................................................... 3

2.2 Procedure ............................................................................................................................. 3

Table 2.1 Volume of methanol and water used in preparation of methanol-water mixture3

Figure 2.1 Lab scale packed distillation column. ............................................................... 4

Figure 2.2 2D schematic diagram of packed distillation column. ...................................... 5

3.0 RESULT & DISCUSSION .................................................................................................. 6

3.1 Experimental Data ............................................................................................................ 6

Table 3.1 Refractive index of methanol-water mixture ...................................................... 6

Table 3.2 Experimental data at different interval of time................................................... 7

Figure 3.1 Graph of refractive index vs % mole methanol ................................................ 8

Table 3.3 Mole fraction of methanol and volume of distillate at different time ................ 9

Figure 3.2 Graph of mole fraction of methanol in product distillate vs. time .................. 10

Figure 3.3 Graph of volume of product distillate vs. time ............................................... 10

4.0 CONCLUSION .................................................................................................................. 12

5.0 RECOMMENDATION ..................................................................................................... 13

6.0 REFERENCES .................................................................................................................. 14

APPENDIX A .......................................................................................................................... 15

APPENDIX B .......................................................................................................................... 16

APPENDIX C .......................................................................................................................... 17
1.0 BACKGROUND OF THE STUDY

Distillation columns are used for separating the components in a liquid solution based
on the distribution of the components between vapour and liquid phase. Components with
higher volatility will vaporise faster and can be collected as distillate while the components of
lower volatility will be collected as the bottom. There are a few criterions for distillation
columns to be an effective method of distillation, namely, the components of the mixture must
have different volatilities, large difference in boiling points and cannot be azeotropes.
One of the main applications of distillation is in the petrochemical industry. The
fractional distillation of crude petroleum is carried out to obtain several different fractions of
different densities such as gasoline and kerosene. Another application of distillation is in waste
treatment to recover solvent from process waste. Distillation can also be applied to extract and
purify essential oils and alcohols. (Maxfield, 2018)
In a distillation column, components that are more volatile will be distilled first. A
component with higher volatility will have higher vapor pressure than a component with lower
volatility at any given temperature. The component with higher volatility also has lower boiling
point. A liquid boil when its vapor pressure rises until it is equal to atmospheric pressure. In
other words, methanol which has a lower boiling point will be distilled over first.
Distillation columns can be used to separate binary and multicomponent mixtures.
When separating binary mixtures, the 2 components can be separated as the distillate and
bottom with relatively high purity. However, when separating multi-component mixtures, the
distillate and bottom might contain more than one component. Therefore, more than one
column might be needed to completely separate the components. Controlling the boiling
temperature will cause the components to be separated differently.
To increase purity of the distillate, rectification with reflux can be done. The feed will
enter at the middle of the column. Liquid will flow downwards while vapor will flow upwards.
The counter current movement will cause the liquid and vapour to be in contact, causing heat
transfer to occur. This will cause the concentration of the more volatile component to increase
in the vapour, increasing the purity of the distillate. The vapour collected overhead will go
through a condenser and be collected as the distillate. The liquid will flow down to the heater
to be reheated (reflux). Theoretically, the vapour and liquid leaving the column is in equilibrium.
(Geankopolis, 2014)

1
 To increase the efficiency of a distillation column, trays or packing can be added. Trays
and packing increases contact area of vapor and liquid in the column, thus increasing the
efficiency of the column and the purity of the products obtained. Types of trays used includes
sieve tray, valve tray and bubble cap tray. Packing can be random packing or structured packing
and can be made in different shapes and material. The type of packing or tray used depends on
the targeted efficiency, price and suitability. The type of packing used in the distillation column
in this experiment is woven gauze stacked packing as shown in Figure 1.1. As condensed liquid
flows down the column through the packing, it comes into contact with the rising vapor. The
steam cools down slightly and the heavy component condenses and flows back down to the
heater. This process increases the purity of the product obtained.

Figure 1.1 Packing in distillation column (Taken on 23rd February 2020 at Separation
Laboratory)
In this experiment, packed distillation column is used to separate water and methanol.
A heater heats up the mixture. Methanol which has a lower boiling point than water will
vaporise first and move through the column, condense and collected every 5 minutes for 1 hour.
Reflux ratio is constant throughout the experiment. The collected distillate will be analysed to
determine its purity and volume.

The objectives of this experiment are to study the effect of operation time on the quality
and quantity of distillate obtained and to investigate the relationship between volume of
distillate obtained and composition of distillate.

2
2.0 METHODOLOGY

2.1 Materials and Apparatus

Packed distillation column
Refractometer
Beaker
Measurement cylinder
Dropper
Stopwatch
Water
Methanol

2.2 Procedure

1. 7 of the methanol-water mixtures were prepared by using pipette according to the

volume stated in Table 2.1

Table 2.1 Volume of methanol and water used in preparation of methanol-water mixture
1 2 3 4 5 6 7
Volume of methanol (ml)
0 2 5 10 15 18 20
Volume of water (ml) 20 18 15 10 5 2 0

A small drop of sample mixture was added into refractometer. The reading was
displayed on the refractometer when the mixture was cooled to 20oC. Record the
reading into table. This was used to obtain a standardization curve to analyse the results
that follows.
2. 32 litres of methanol-water feed mixture with composition of methanol 30% and water
70% were prepared.
3. All of the equipment was in place and packed distillation column was ensure in good
conditions before the experiment start.
4. The V2 valve was opened and the RCV1, V3, V4 valves were ensure closed before
turned on the power supply.
5. The electric heater and coolant flow pump were turned on simultaneously.

3
6. The reflux ratio was set at 2.0 by slowly opening reflux control valve RCV1. The
product distillate will flow to RI 1B and the rest of the product distillate flowed through
RI 1A and returned to the reboiler vessel.
7. The product distillate that did not return to reboiler vessel was collected in a 1000mL
measuring cylinder by closing the V2 valve and opened the V3 and V4 valve.
8. The volume of the sample collected in step 7 was measured and the refractive index
was determined using refractometer.
9. Steps 7 and 8 were repeated every 5 minutes and readings were taken according to the
table.

Figure 2.1 Lab scale packed distillation column. (Taken on 23rd February 2020 at
Separation Laboratory).

4
Figure 2.2 2D schematic diagram of packed distillation column.

5
3.0 RESULT & DISCUSSION
3.1 Experimental Data
Table 3.1 Refractive index of methanol-water mixture
Volume of 0 2 5 10 15 18 20
methanol
(mL)
Volume of 20 18 15 10 5 2 0
water
(mL)
Moles of
Methanol 0.000 0.049 0.124 0.247 0.371 0.445 0.494
Moles of
Water 1.110 0.999 0.833 0.555 0.278 0.111 0.000
Mole % of
Methanol 0.000 4.676 12.957 30.798 57.165 80.036 100.000
Refractive 1.328 1.330 1.331 1.341 1.339 1.336 1.327
index

Sample calculation (For 2mL methanol in 18mL of water):

Reference density = 1.000 g/ cm3

Molecular Weight of Water = 18.015 g/mol
Specific Gravity of Water = 1.000
Molecular Weight of Methanol = 32.04 g/mol
Specific Gravity of Methanol = 0.792

i) Calculation of number of moles of methanol:

𝑣𝑜𝑙𝑢𝑚𝑒 × 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝑔𝑟𝑎𝑣𝑖𝑡𝑦 𝑜𝑓 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 2𝑚𝐿 × 0.792
=
𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 32.04 gmol − 1
=0.049 mole

ii) Calculation of number of moles of water:

𝑣𝑜𝑙𝑢𝑚𝑒 × 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝑔𝑟𝑎𝑣𝑖𝑡𝑦 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 18𝑚𝐿 × 1.000
=
𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 18.015 gmol − 1
= 0.999

iii) Calculation of mole percentage of methanol:

𝑚𝑜𝑙 𝑜𝑓 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 0.049

× 100% = × 100%
𝑡𝑜𝑡𝑎𝑙 𝑚𝑜𝑙 𝑜𝑓 𝑚𝑖𝑥𝑒𝑑 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 0.049 + 0.999
= 4.676%

6
 Table 3.2 Experimental data at different interval of time

TIME (min) 5 10 15 20 25 30 35 40 45 50 55 60
TI 67 66 65 65 65 65 64 64 64 64 65 66
1
TI 75 70 68 67 67 67 67 67 69 72 83 85
1B
TEMPERATURE IN PLATE

TI 76 71 69 67 67 67 67 68 71 76 81 81
2
TI 80 76 72 71 70 70 71 73 77 83 86 86
2A
TI 80 78 76 74 73 74 75 77 82 82 83 84
(℃)

2B
TI 84 84 85 85 85 86 86 87 87 87 88 88
2C
TI 86 86 86 87 87 88 88 88 89 89 89 90
2D
TI 86 86 86 87 87 88 88 88 89 89 89 90
2F
TI 86 86 86 87 87 88 88 88 89 89 89 90
3
Temp. TI 88 89 89 89 89 89 90 90 91 91 91 92
original 4
solution
(℃)
Temp. TI 31 31 31 31 32 32 32 32 33 33 33 33
cooling 5
water
(℃) TI 57 57 57 56 56 56 57 56 57 57 57 59
6
Reflux RI 3 2.8 2.9 3.1 3.0 2.9 3.0 2.8 3.2 3.1 2.9 3
1A
RI 2 2 2 2 2 2 2 2 2 2 2 2
1B
Reflux ratio 0.667 0.714 0.690 0.645 0.667 0.690 0.667 0.714 0.625 0.645 0.690 0.667
Volume 240 290 300 290 300 300 300 280 300 290 290 290
distillate(mL)
Refractive 1.335 1.330 1.328 1.328 1.328 1.328 1.328 1.328 1.328 1.328 1.328 1.328
index
Voltage (V) 150V
Current (A) 25A

7
 Refractive index vs %-mole methanol
1.342
1.34
1.338
Refractive Index

1.336
1.334
1.332
1.33
1.328 y = -5E-06x2 + 0.0005x + 1.3274
R² = 0.9277
1.326
0 20 40 60 80 100 120
%-mole methanol

Figure 3.1 Graph of refractive index vs % mole methanol

Figure 3.1 shows the graph of refractive index versus percentage mole of methanol for
benchmark mixture of methanol-water. According to the graph, refractive index increases with
increase of percent mole of methanol until it reached the maximum point where refractive index
obtained at 1.341 and 30.798% mole methanol. After it reached the maximum point, the value
of the refractive index will decrease until 100% mole percentage of methanol has achieved,
which is at 1.327. Therefore, bell-like shaped curve downward graph is obtained. From the
graph, a pure solution of methanol and water at 25oC gives the refractive index of 1.327 and
1.328 respectively. The result obtained is almost similar with the standard refractive index for
pure water and methanol, which is 1.333 and 1.328 respectively.

Besides that, Figure 3.1 also acts as the benchmark for determining composition of
methanol in the product distillate. The mole fraction of methanol can be calculated using
equation from Graph 4.1 and refractive index obtained from Table 3.2. The equation that related
the refractive index of product distillate to the mole percentage of methanol is  y =
−4 × 10−6 𝑥 2 + 0.0004x + 1.3274 , where y = refractive index and x= %-mole of methanol

8
 Table 3.3 Mole fraction of methanol and volume of distillate at different time

Time Volume Refractive Index Mole Percent Mole Fraction

(minute) distillate (cm3) (%)

5 240 1.335 74.49 0.7449

10 290 1.330 93.01 0.9301

15 300 1.328 98.48 0.9848

20 290 1.328 98.48 0.9848

25 300 1.328 98.48 0.9848

30 300 1.328 98.48 0.9848

35 300 1.328 98.48 0.9848

40 280 1.328 98.48 0.9848

45 300 1.328 98.48 0.9848

50 290 1.328 98.48 0.9848

55 290 1.328 98.48 0.9848

60 290 1.328 98.48 0.9848

Sample calculation:
y = −4 × 10−6 𝑥 2 + 0.0004x + 1.3274
Where, x = mole fraction of methanol,
y = refractive index
0 = −4 × 10−6 𝑥 2 + 0.0004x + (1.3274 − 𝑦)
a = −4 × 10−6 b = 0.0004c = (1.3274 − 𝑦)
−𝑏 ± √𝑏 2 − 4𝑎𝑐
x=
2𝑎
At time = 5 minutes, refractive index = y = 1.335,
−(0.0004) ± √(0.0004)2 − 4(−4 × 10−6 )(1.3274 − 1.335) 1
x= ×
2(−4 × 10−6 ) 100
x =  0.7449

9
 Time

Figure 3.2 Graph of mole fraction of methanol in product distillate vs. time

Graph of volume of product distillate vs time

350
Volume of product distillate

300

250
y = 0.3287x + 278.48
200
R² = 0.1249
150

100

50

0
0 10 20 30 40 50 60 70
Time

Figure 3.3 Graph of volume of product distillate vs. time

Figure 3.2 shows the relationship between the mole fractions of methanol in product
distillate with time of the distillation. According to the graph, mole fraction of methanol in
product distillate increases with time at the beginning. The range value of mole fraction of
methanol in overall is between 0.70-0.98. Therefore, a high composition of methanol in the
distillate product showed that packed distillation column is a suitable method in separating
methanol from water. When distillation times longer, methanol molecules which is most
volatile component possess enough kinetic energy to escape from liquid phase into vapor phase
and giving higher mole fraction of methanol in product distillate. From the time of 15 minutes,
mole fraction of methanol in product distillate remain constant. This indicated that effective
distillation process is carried out during the experiment.

Figure 3.3 showed the relationship between volume of product distillate and time.
According to the graph, distillate volume obtained almost constant throughout the experiment
after 10 minutes. Therefore, this indicated that the distillation column had attained its steady
state. The volume of product distillate fluctuated in the range between 290 cm3 and 300
cm3.When the time is 5 minutes at the beginning of experiment, the distillate volume obtained

10
is the lowest which is 240 cm3 and it increase to 290 cm3 at 10 minutes. This may be due to
some error occurred during the experiment such as parallel error when take the reading. Closing
the valve require some time for every collection of distillates and there might cause overflow
of distillate into the receiver.
In this experiment, packed distillation column was used for vapor liquid separation. Hence,
there are some advantages of using it compared other distillation column as mentioned below.
1. Packed distillation column has low pressure drop properties that allow the usage in
vacuum distillation process.
2. Packed column only require small diameter which is less than 0.6m and usually be
cheaper than other plate distillation column.
3. Packed column suitable for handling foaming system due to the low relative
disturbance degree of liquid by gas.
4. The packing in the column is made of inert materials which enable the acidic solution
and erosion material operated with it.
5. Liquid hold up is lower in packed column and enable it for handling thermally sensitive
and flammable liquids.
6. The installation of packed column is easier than other plate column.

There are some safety regulation and precautions that need to be considered during the
experiments in order to avoid accidents to happen such as:
1. Avoid direct contact with the instrument since the distillation operation usually deals
with very hot and highly flammable materials. Extreme care must be taken when
handling the apparatus, taking readings and collecting samples.
2. Safety helmet and goggle should be wear especially taking the reading of distillation
temperature at high place.
3. When handling the methanol-water mixture, gloves and goggle should be wear in order
to avoid direct contact with the chemicals.
4. The waste of the distillate should be discharged properly into the specific bottles instead
of discharging it to sink
5. Report to the instructor or technician if the equipment found any damaged.
6. Ensure the valve tight enough to avoid leakage and affect the distillation process.

11
4.0 CONCLUSION

All in all, the operational time required to achieve maximum distillate volume is around
10 minutes, whereby the volume fluctuates around 290 cm3 and 300 cm3. During the
experiment, the methanol composition at distillate ranged between 0.7449 and 0.9848. After
the 15th minute, the composition of methanol in the distillate peaked at 0.9848 and remained
constant until the end of experiment which indicate that it has achieved steady state like
condition. The packed distillation column is effective in separation a liquid-liquid mixture with
difference in boiling temperature such as methanol-water mixture as shown in this experiment.
It also required a short timespan to achieve steady-state condition and thus maximizing the
wanted content from the mixture.

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5.0 RECOMMENDATION

In this experiment, there are a few recommendations to help minimize the error and
obtain a more preferable result. The recommendations are:

a) The time taken to close and open the valve to collect distillate should be kept to minimal
to avoid any loss in volume as it enters the receiver.
b) Ensure the methanol-water mixture is mixed well and without impurities to obtain a
more accurate refractive index value
c) Eyes should be perpendicular to the reading taken to avoid parallax error.
d) Significant figure of 4 or more should be used during calculation to ensure highest
possible accuracy.
e) Devices such as fan should be turned off in the lab to avoid disturbances or fluctuation
in surrounding environment which could affect result of experiment.

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6.0 REFERENCES

Distillation Columns. (n.d.). Retrieved on February 24, 2020 from

http://encyclopedia.che.engin.umich.edu/
Geankopolis, C.J. (2014). Transport Processes & Separation Process Principles (Includes
Unit Operations). London: Pearson Education Limited

Maxfield, M. (2018). Practical Uses of Distillation. Retrieved on February 24, 2020 from
https://sciencing.com/

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 APPENDIX A
PHYSICAL PROPERTIES OF METHANOL

15
 APPENDIX B
SAMPLE CALCULATIONS PART 1

iv) Calculation of number of moles of methanol:

𝑣𝑜𝑙𝑢𝑚𝑒 × 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝑔𝑟𝑎𝑣𝑖𝑡𝑦 𝑜𝑓 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 2𝑚𝐿 × 0.792
=
𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 32.04 gmol − 1
=0.049 mole

v) Calculation of number of moles of water:

𝑣𝑜𝑙𝑢𝑚𝑒 × 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝑔𝑟𝑎𝑣𝑖𝑡𝑦 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 18𝑚𝐿 × 1.000
=
𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 18.015 gmol − 1
= 0.999

vi) Calculation of mole percentage of methanol:

𝑚𝑜𝑙 𝑜𝑓 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 0.049

× 100% = × 100%
𝑡𝑜𝑡𝑎𝑙 𝑚𝑜𝑙 𝑜𝑓 𝑚𝑖𝑥𝑒𝑑 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 0.049 + 0.999
= 4.676%

16
 APPENDIX C
SAMPLE CALCULATIONS PART 2

y = −4 × 10−6 𝑥 2 + 0.0004x + 1.3274

Where, x = mole fraction of methanol,
y = refractive index
0 = −4 × 10−6 𝑥 2 + 0.0004x + (1.3274 − 𝑦)
a = −4 × 10−6 b = 0.0004c = (1.3274 − 𝑦)
−𝑏 ± √𝑏 2 − 4𝑎𝑐
x=
2𝑎
At time = 5 minutes, refractive index = y = 1.335,
−(0.0004) ± √(0.0004)2 − 4(−4 × 10−6 )(1.3274 − 1.335) 1
x= ×
2(−4 × 10−6 ) 100
x =  0.7449

17