DISTILLATION

AN Hadebe and NNM Dladla

Department of Chemical Engineering
Durban University of Technology

November 2022
SUMMARY
Distillation is the most widely used method of separating fluid mixtures on a
commercial scale, it is thus an important part of many processes in the oil and
chemical industries. The mixtures are separated by heating a liquid until it boils,
then condensing and collecting the resultant hot vapors. Basically, we were tasked
with an isopropanol-methanol mixture. Our task is to operate the distillation
column on this alcohol at a reflux ratio of 2. We were then tasked to complete
mass and energy balances for the column. The material balance will help us
determine the distillate flow rate and composition. And the energy balance will
help us to check if it balances.

PAGE 1
PAGE 2
 1. INTRODUCTION

During the practical there will be an explanation of the operation conditions of the
distillation column. Distillation is a technique used widely throughout the
chemical process industries for separation, purification, and refining, so a
thorough understanding is of great importance.

PAGE 3
 2. THEORY
Material balance

The feed flowrate is calculated using the following formula:

𝐹 = 0.042𝑥 2 − 7.6 × 10−04 𝑥 3 equation 1

Where F = Flowrate (L/Hr)

x = Pump setting (%)
A pump configuration which is a set of curves expressing the pump performance
for a specific speed and impeller diameter (Applied Flow Technology 1996) in
appendix c was used to determine the flowrate of the feed and the exact flowrate
was calculated using equation 1 where a pump setting percentage is included.
Increasing the pump setting percentage results in an increase of the flowrate.
High feed rate may lead to increase in column bottom level or flooding in the
column. If the feed rate is too high, over-loading can occur.
The density of a stream containing A and B was calculated using the following
formula:
1 𝑥𝐴 𝑥𝐵 equation 2
= +
𝜌𝑚𝑖𝑥 𝜌𝐴 𝜌𝐵

𝑘𝑔
Where 𝜌𝑚𝑖𝑥 = 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝑎 𝑚𝑖𝑥𝑡𝑢𝑟𝑒 (𝑚3)
𝑥𝐴 = 𝑚𝑎𝑠𝑠 𝑓𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝐴
𝜌𝐴 = 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝐴
Density of a mixture was calculated for each stream to find the mass flowrates of
streams. Increasing the mass fractions results in a decrease of the density of a
mixture. This increase would not affect energy balance.

Mass flowrate of a stream was calculated using the following equation:

𝑚 ̇ = 𝜌𝑉̇ equation 3

Volumetric flowrate was used to determine the mass flowrate. For feed stream
the volumetric flowrate was given and for the bottom stream it had to be
measured. It was measured by timing the withdrawal of a 50 ml sample from the
stopcock valves located in the cooled product lines. The vapor flow rate is also a
factor in the effectiveness of the tray. Increasing the flow rate increases the
effective mass transfer rate, whilst simultaneously decreasing the contact time.
These counteracting effects lead to a roughly constant efficiency value for a tray in

PAGE 4
its normal operating range. Upon approaching its lower operating limit, a tray
starts weeping and loses efficiency.

The refractive index calibration curve in appendix D was used to find the mass
percentage of methanol in the bottom stream using the bottoms flowrate.
Refractive index of a solution depends on the concentration of solute.

Mass flowrate of overhead stream and its mass fractions was calculated using the
following formula:
F1 = F2 + F3 equation 4

Where F1 = Total flowrate of stream 1 (kg/s)

And the equation for finding mass fractions of each component was derived from
equation 4 since
𝐹1 = 𝑚𝑖,𝐹1 equation 5

Where 𝑚𝑖,𝐹1 = Mass flowrate of component i in stream F1 and

𝑚𝑖,𝐹1 = 𝐹1 𝑥𝑖,𝐹1 equation 6

Where 𝑥𝑖,𝐹1 = Mass fraction of component i in stream F1

The derived equation was:

𝐹1 𝑥𝑖,𝐹1 = 𝐹2 𝑋𝑖,𝐹2 + 𝐹3 𝑥𝑖,𝐹3 equation 7

Energy balance

The total energy balance for this distillation process was calculated using the
following equation:

𝐻𝐹1 + 𝑄𝑟𝑒𝑏𝑜𝑖𝑙𝑒𝑟 = 𝐻𝐹2 + 𝐻𝐹3 + 𝑄𝑐𝑜𝑛𝑑𝑒𝑛𝑠𝑜𝑟 equation 8

Where 𝐻𝐹𝑖 = 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝑒𝑛𝑡ℎ𝑎𝑙𝑝𝑦 𝑜𝑓 𝑠𝑡𝑟𝑒𝑎𝑚 𝑖 (𝑘𝑔/𝑠)

𝑄𝑟𝑒𝑏𝑜𝑖𝑙𝑒𝑟 = 𝑟𝑒𝑏𝑜𝑖𝑙𝑒𝑟 𝑑𝑢𝑡𝑦 (𝑘𝑔⁄𝑠)
𝑄𝑐𝑜𝑛𝑑𝑒𝑛𝑠𝑜𝑟 = 𝑐𝑜𝑛𝑑𝑒𝑛𝑠𝑜𝑟 𝑑𝑢𝑡𝑦(𝑘𝑔⁄𝑠)

The equation used is derived from the total energy balance stating that all energy
coming in = all energy going out.

The specific enthalpy of a stream was calculated using the following equation:

PAGE 5
 ̂𝐹𝑖 = 𝑚𝐹𝑖 𝐻𝐹𝑖
𝐻 equation 9

Where 𝐻𝐹𝑖 = 𝑒𝑛𝑡ℎ𝑎𝑙𝑝ℎ𝑦 𝑜𝑓 𝑠𝑡𝑟𝑒𝑎𝑚 𝑖

The difference between specific enthalpy and enthalpy is that specific enthalpy is
an intensive property, its value doesn’t depend upon the size or mass of the system
or matter but only in its type and its SI units are J/kg or KJ/kg and enthalpy is an
extensive property, its value depends upon the size of matter and its SI units are J
or KJ (Debarghya R 2020). Specific enthalpy is dependent on mass flowrate of
stream so an increase in mass flowrate will results in an increase in specific
enthalpy.

The enthalpy of stream was calculated using the following equation:

𝑇𝑖 equation 10
𝐻𝐹𝑖 = ∫ (𝐶𝑝,𝐹𝑖 ) 𝑑𝑇
𝑇𝑟𝑒𝑓

Where 𝐶𝑝,𝐹𝑖 = 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 ℎ𝑒𝑎𝑡 𝑐𝑎𝑝𝑎𝑐𝑖𝑡𝑦 𝑜𝑓 𝑠𝑡𝑟𝑒𝑎𝑚 𝑖

The specific enthalpy of a stream was calculated using the following equation:

𝐶𝑝,𝐹1 = 𝑥𝑚,𝐹1 𝐶𝑝,𝑚 + 𝑥𝑖,𝐹1 𝐶𝑝,𝑖 equation 11

Where 𝐶𝑝,𝑖 = 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 ℎ𝑒𝑎𝑡 𝑒𝑛𝑡ℎ𝑎𝑙𝑝𝑦 𝑜𝑓 𝑎 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡

The condenser duty was calculated using the following equation:

𝑄𝑐 = 𝑚𝑐/𝑤 𝐶𝑃𝐶/𝑊 (𝑇𝐶/𝑊𝑜𝑢𝑡 − 𝑇𝐶/𝑊𝑖𝑛 ) equation 12

Where 𝑚𝑐/𝑤 = 𝑚𝑎𝑠𝑠 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝑜𝑓 𝑐𝑜𝑜𝑙𝑖𝑛𝑔 𝑤𝑎𝑡𝑒𝑟 𝑠𝑡𝑟𝑒𝑎𝑚

𝐶𝑃𝐶/𝑊 = 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 ℎ𝑒𝑎𝑡 𝑒𝑛𝑡ℎ𝑎𝑙𝑝𝑦 𝑜𝑓 𝑐𝑜𝑜𝑙𝑖𝑛𝑔 𝑤𝑎𝑡𝑒𝑟 𝑠𝑡𝑟𝑒𝑎𝑚
𝑇𝐶/𝑤 = 𝑡𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒 𝑜𝑓 𝑐𝑜𝑜𝑙𝑜𝑛𝑔 𝑤𝑎𝑡𝑒𝑟 𝑠𝑡𝑟𝑒𝑎𝑚

PAGE 6
 3. EXPERIMENTAL METHOD AND APPARATUS

(DVI/3000 2019)

Procedure

✓ Turn on the Exhaust fan system to the left of the distillation column.
✓ Fill the feeding storage tank with 50L of the mixture to distill.

PAGE 7
✓ Adjust the feeding flow rate using the inlet globe valve to approximately 130
L/hr.
✓ Fill in the kettle with the mixture up to the overflow level.
✓ Set the reflux conditions turning the three-way switch to the TOTAL REFLUX
position and adjust power level to 2 KW.
✓ Feed the condenser with water circulation of 150 L/h.
✓ Feed with cold water to all the distillate and residue coolers.
✓ Start heating the kettle until you note some vapors near the column reflux
head.
✓ Wait until the temperature profile along the column is stable.
✓ Select the level of introduction of the mixture into the distillation column.
✓ Start the dosing pump, the feeding flow rate should have already been adjusted
( not exceeding 30% setting) before starting the distillation process.
✓ Adjust the preheating temperature to approximately 0.25 KW.
✓ Power up the preheater when its level is enough.
✓ Wait for all temperatures to stabilize.
✓ Write down all process values and set points.
✓ Set the reflux ratio to 2.
✓ Wait for all temperatures to stabilize.
✓ Write down all process values and set points.
✓ Take samples of the bottoms to determine mass fraction using a refractometer.
✓ Measure bottom flowrate by timing withdrawal of 50 ml sample from relevant
stock valves.

PAGE 8
 4. RESULTS DISCUSSION AND CONCLUSION
CALCULATIONS

Material balance

From appendix c
𝑓𝑒𝑒𝑑 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 = 0.042(32)2 − 7.6 × 10−04 (32)3
= 18,10432 𝐿/𝐻𝑟

Feed
1 𝑥𝑚,𝐹1 𝑥𝑖,𝐹1
= +
𝜌𝑚𝑖𝑥 𝜌𝑚 𝜌𝑖
0.347731713 0.652268287
= +
792 786
∴ 𝜌𝑚𝑖𝑥 = 788.0760533 𝑘𝑔/𝑚3

𝑚 ̇ = 𝜌𝑉̇
788.0760533 𝑘𝑔 18.10432 𝐿 1𝑚3 1ℎ𝑟
| | |
𝑚3 ℎ𝑟 1000𝐿 3600𝑠
𝑚̇ = 0.00396322 𝑘𝑔/𝑠

From appendix D
Mass % of methanol on Bottoms stream = 30%
∴ Mass % of isopropanol = 70%

Bottoms
Measured flowrate = 50,25921661 ml/ 11 s
50,25921661 𝑚𝑙 1𝐿 3600 𝑠
| |
11𝑠 1000 𝑚𝑙 1 ℎ𝑟
∴ 𝑏𝑜𝑡𝑡𝑜𝑚𝑠 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 = 16,44847089 𝐿/ℎ𝑟

1 𝑥𝑚,𝐹3 𝑥𝑖,𝐹3
= +
𝜌𝑚𝑖𝑥 𝜌𝑚 𝜌𝑖
0.30 0.70
= 792 + 786
∴ 𝜌𝑚𝑖𝑥 = 787,7904328 𝑘𝑔/𝑚3
𝑚 ̇ = 𝜌𝑉̇
787,7904328 𝑘𝑔 16,44847089 𝐿 1𝑚3 1ℎ𝑟
| | |
𝑚3 ℎ𝑟 1000𝐿 3600𝑠
𝑚̇ = 0,00359943 𝑘𝑔/𝑠

Heads
Total balance
F1 = F2 + F3

PAGE 9
0.00396322 = 0,00359943 + 𝐹2
∴ 𝐹2 = 0,00036379 𝑘𝑔/𝑠
Methanol balance
𝐹1 𝑥𝑚,𝐹1 = 𝐹2 𝑋𝑚,𝐹2 + 𝐹3 𝑥𝑚,𝐹3
0.00396322 (0.347731713) = 0,00359943(0.30) + 0,00036379 𝑥𝑚,𝐹2
0,00137813728 − 0,001079829 = 0,00036379𝑥𝑚,𝐹2
∴ 𝑥𝑚,𝐹2 = 0.8199990643

Isopropanol balance
𝐹1 𝑥𝑖,𝐹1 = 𝐹2 𝑋𝑖,𝐹2 + 𝐹3 𝑥𝑖,𝐹3
0.00396322 (0.652268287) = 0,00359943(0.70) + 0,000363791𝑥𝑖,𝐹2
0,00258508272 − 0,002519601 = 0,000363791𝑥𝑖,𝐹2
∴ 𝑥𝑖,𝐹2 = 0. 1799981869

𝑚𝑚,𝐹2 = 𝐹2 𝑋𝑚,𝐹2
= 0,00036379(0.8199990643)
= 0,00029830745 𝑘𝑔/𝑠

𝑚𝑖,𝐹2 = 𝐹2 𝑋𝑖,𝐹2
= 0,00036379(0. 1799981869)
= 0,00006548213 𝑘𝑔/𝑠

Energy balance

Reflux = 2
𝐹6 = 2𝐹2
𝐹6 = 2(0,00036379 )
= 0.00072758 𝑘𝑔/𝑠

F4 = F6 + F2
= 0.00072758 + 0,00036379
= 0,00109137 𝑘𝑔/𝑠

𝐹5 = 𝐹4
= 0,00109137 𝑘𝑔/𝑠

Total energy balance

𝐻𝐹1 + 𝑄𝑟𝑒𝑏𝑜𝑖𝑙𝑒𝑟 = 𝐻𝐹2 + 𝐻𝐹3 + 𝑄𝑐𝑜𝑛𝑑𝑒𝑛𝑠𝑜𝑟

Tref = 0oC

𝐶𝑝,𝐹1 = 𝑥𝑚,𝐹1 𝐶𝑝,𝑚 + 𝑥𝑖,𝐹1 𝐶𝑝,𝑖

= 0.347731713(2510) + 0.652268287(1540)

PAGE 10
 = 1877,299762 KJ/kg0C

21℃
𝐻𝐹1 = ∫ (1877,299762) 𝑑𝑇
0℃
= 1877,299762(21)
= 39423,29499 𝐾𝐽/𝑘𝑔

̂𝐹1 = 𝑚𝐹1 𝐻𝐹1

𝐻
= 0.00396322 (39423,29499)
= 156,243071𝐾𝐽/𝑠

𝐶𝑝,𝐹2 = 𝑥𝑚,𝐹2 𝐶𝑝,𝑚 + 𝑥𝑖,𝐹2 𝐶𝑝,𝑖

= 0.8199990643(2510) + 0. 1799981869(1540)
= 2335,394859 KJ/kg0C

64,5℃
𝐻𝐹2 = ∫ (1831) 𝑑𝑇
0℃
= 2335,394859(64,5)
= 150632,9684 𝐾𝐽/𝑘𝑔

̂𝐹2 = 𝑚𝐹2 𝐻𝐹2

𝐻
= 0,00036379(150632,9684)
= 54,79876758 𝐾𝐽/𝑠

𝐶𝑝,𝐹3 = 𝑥𝑚,𝐹3 𝐶𝑝,𝑚 + 𝑥𝑖,𝐹3 𝐶𝑝,𝑖

= 0.3(2510) + 0.7(1540)
= 1831 KJ/kg0C

73℃
𝐻𝐹3 = ∫ (1831) 𝑑𝑇
0℃
= 1831(73)
= 133663 𝐾𝐽/𝑘𝑔

̂𝐹3 = 𝑚𝐹3 𝐻𝐹3

𝐻
= 0,00359943 (133663)
= 481,1106121 𝐾𝐽/𝑠

𝑚 ̇ = 𝜌𝑉̇

PAGE 11
1000 𝑘𝑔 150 𝐿 1𝑚3 1ℎ𝑟
| | |
𝑚3 ℎ𝑟 1000𝐿 3600𝑠

= 0,04166666667 𝑘𝑔/𝑠

𝑄𝑐 = 𝑚𝑐/𝑤 𝐶𝑃𝐶/𝑊 (𝑇𝐶/𝑊𝑜𝑢𝑡 − 𝑇𝐶/𝑊𝑖𝑛 )

= 0,04166666667 (4180)(30,2 − 25)
= 905,6666667 𝐾𝐽/𝑘𝑔

Reboiler Duty (Qr) = 1450 𝐾𝐽/𝑘𝑔

Energy in = 𝐻𝐹1 + 𝑄𝑟𝑒𝑏𝑜𝑖𝑙𝑒𝑟

= 156,243071 + 1450
= 1606,243071

Energy out = 𝐻𝐹2 + 𝐻𝐹3 + 𝑄𝑐𝑜𝑛𝑑𝑒𝑛𝑠𝑜𝑟

= 54,79876758 + 481,1106121 + 905,6666667

= 1441,576045

Difference = 1606,243071 − 1441,576045

= 159,667026

1441,576045
% Loss = × 100% − 100
1606,24307
= 10,25168787 %

RESULTS

F1 F2 F3 F4 F5
Total 0,00396322 0,00036379 0,00359943 0,04167 0,04167
flowrate(kg/s)
Mass fractions
Methanol 0.347 0.819 0,30 0.819 0.819
Isopropanol 0.652 0. 179 0,70 0. 179 0. 179
Water - - - 1 1
Stream 21 64,5 73 25 30,2
temperature
(0c)
Enthalpy 156,24 54,79 481,11 905,67 -
(kj/s)

PAGE 12
 Heat duty , Q (KJ/s)
Feed preheater 156,243071
Reboiler 1450
Condenser 905,67
DISCUSSION

CONCLUSION

5. Nomenclature
Name Symbol Unit
Volumetric flowrate 𝑉̇ L/hr
Time t s or hr
O
Temperature T C
Mass flowrate of streams mi -
Composition of component xi -
Heat duty Q KJ/s
Density 𝜌 Kg/m3
Pressure P Kw
Total flowrate of stream F Kg/s
Mass flowrate 𝑚̇ Kg/s
Mass m ml

6. References

PAGE 13
 7. Appendices

Sera Diaphragm Pump

30
y = 207,55x - 83,443
25 R² = 0,1056
Flowrate (L/hr)

20

15

10

0
0 5 10 15 20 25 30 35
Pump setting (%)

Appendix 1

PAGE 14
Appendix 2

Pump setting % for feed diaphragm pump: %

Reflux ratio :
Refractive index of feed stream
Mass fraction of methanol %
Mass fraction of isopropanol
Refractive index of bottoms stream
Mass fraction of methanol %
Mass fraction of isopropanol
Density of methanol g/cm3
Density of isopropanol g/cm3
Column Reflux temp °C
Tray #1 Temp °C
Tray #6 Temp °C

PAGE 15
 Tray #11 Temp °C

Reboiler Temp °c
Overheads Temp (after cooler) °c
Bottoms Temp (after cooler) °C
Feed Temp (before heater) °C

Feed Temp (after heater) °c

Cond Cooling Water Temp (in) °C
Cond Cooling Water Temp (out) °C

Reboiler Duty kW
Feed Preheater Duty

Feed Flowrate L/hr

Bottom Product Flow (measure) L/hr

Condenser cooling water flowrate L/hr

Appendix 3

Feed Temp oC 21
Bottom Temp oC 73
Distillate Temp oC 64,5
Bottom Refractive
1,365
Index
Distillate Refractive
1,34
Index
Pump Setting % 32
Reboiler Duty kW 1450
CW Flow (l/hr) 150
CW In oC 25
CW Out oC 30,2

PAGE 16