FACULTY: ENGINEERING EDITION:

TECHNOLOGY
LABORATORY: PROCESS
REVISION NO:
TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: BATCH
DISTILLATION AMENDMENT
DATE:
FACULTY OF ENGINEERING TECHNOLOGY
DEPARTMENT OF MECHANICAL ENGINEERING TECHNOLOGY

PROCESS TECHNOLOGY LABORATORY

LABORATORY INSTRUCTION SHEETS

COURSE CODE BNL 40203

EXPERIMENT NO. EXPERIMENT 2

EXPERIMENT TITLE BATCH DISTILLATION

GROUP NO.
1)
2)
3)
GROUP MEMBERS
4)
5)
6)
LECTURER/INSTRUCTOR/ 1)
TUTOR 2)
DATE OF REPORT
SUBMISSION
ATTENDANCE/PARTICIPATION/DISCIPLINE: /5%
INTRODUCTION: /5%
PROCEDURE: /5%
RESULTS& CALCULATIONS /15%
ANALYSIS /15%
DISTRIBUTION OF MARKS
FOR LABORATORY DISCUSSIONS: /20%
REPORT: ADDITIONAL QUESTIONS /15%
CONCLUSION /10%
SUGGESTIONS& RECOMENDATIONS /5%
REFERENCES: /5%
TOTAL: /100%
EXAMINER COMMENTS: RECEIVED DATE AND STAMP:
 FACULTY: ENGINEERING EDITION:
TECHNOLOGY
LABORATORY: PROCESS
REVISION NO:
TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: BATCH
DISTILLATION AMENDMENT

KOD ETIKA PELAJAR DATE:

(KEP)
JABATAN TEKNOLOGI KEJURUTERAAN KIMIA

FAKULTI TEKNOLOGI KEJURUTERAAN

Saya dengan ini mengaku bahawa saya telah menyediakan laporan ini dengan daya usaha

saya sendiri. Saya juga mengaku tidak menerima atau memberi sebarang bantuan dalam

menyediakan laporan ini dan membuat ikrar ini dengan kepercayaan bahawa apa-apa yang

tersebut di dalamnya adalah benar.

Ketua Nama:

Kumpulan No. Matriks: (Tandatangan)

Ahli 1 Nama:

No. Matriks: (Tandatangan)

Ahli 2 Nama:

No. Matriks: (Tandatangan)

Ahli 3 Nama:

No. Matriks: (Tandatangan)

Ahli 4 Nama:

No. Matriks: (Tandatangan)

Ahli 5 Nama:

No. Matriks: (Tandatangan)

_______________

Tarikh :________________________________
 FACULTY: ENGINEERING EDITION:
TECHNOLOGY
LABORATORY: PROCESS
REVISION NO:
TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: BATCH
DISTILLATION AMENDMENT
DATE:

1.0 OBJECTIVES

1. To perform batch distillation on a binary mixture using a sieve plate column.

2. To investigate the effects of a constant reflux ratio and regulating reflux ratio on product composition at top and bottom.

2.0 LEARNING OUTCOMES

Conduct the separation engineering principles involved in pilot plant effectively.

3.0 INTRODUCTION / THEORY

CHEMICAL PREPARATION

Mixing distilled water/ethanol

The sieve plate distillation column can be used for distilling a binary mixture consisting of either of the two components listed
above, e.g. distilled water-ethanol, distilled water-propanol or ethanol-propanol. To prepare 1L ethanol-water mixture of
composition 50 V/V% of ethanol, observe the following steps.

1. Fill a 1 L measuring cylinder with 500 ml of component ethanol.

2. Pour 500ml water into the same beaker which is contain 500ml of ethanol.
3. Stir the mixture using a glass rod.
4. The product is now a 1 L batch of binary mixture with 50 V/V% of ethanol.

In order to prepare an X V/V% component of A mixture with B, please refer the table below (this is for 1L binary mixture, please
follow the ratio for preparation of larger volume. E.g. for 20L binary mixture of 50V/V% of ethanol-water mixture, mix 10L ethanol
with 10L distilled water ):

TABLE 1: BINARY MIXTURE PREPARATION TABLE

X, V/V% Component A (ml) Component B (ml)
10 100 900
20 200 800
30 300 700
40 400 600
50 500 500
60 600 400
70 700 300
80 800 200
90 900 100

NOTE
1. Ethanol is volatile and will evaporate quickly. Avoid exposing these chemicals to the atmosphere for extended periods of time.
2. Dispose of all unused chemicals in an appropriate manner after the experiment. Under no circumstances should the
chemicals be allowed to flow into the main drains.
 FACULTY: ENGINEERING EDITION:
TECHNOLOGY
LABORATORY: PROCESS
REVISION NO:
TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: BATCH
DISTILLATION AMENDMENT
DATE:

4.0 EQUIPMENTS & MATERIALS

E F G

K
D

LEGEND

A - Reboiler / Evaporator
B - Distillation column
C - Sampling ports
D - Differential Pressure Gauge
E - Condenser
F - Reflux Divider
G - Reflux Valve
J - Water jet vacuum
K - Top product tank
L - Control Panel
 FACULTY: ENGINEERING EDITION:
TECHNOLOGY
LABORATORY: PROCESS
REVISION NO:
TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: BATCH
DISTILLATION AMENDMENT
DATE:

(L) Control Panel

Pour the feed to

evaporator
through this

Evaporator / Reboiler

Heater
HeaterPower
Power
Warning : Never open this Regulator
Regulator
inlet cap while in operation
under pressure as vapors
built up may cause injury !! Mains Power Switch
 FACULTY: ENGINEERING EDITION:
TECHNOLOGY
LABORATORY: PROCESS
REVISION NO:
TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: BATCH
DISTILLATION AMENDMENT
DATE:

5.0 PROCEDURES

5.1 General Start-up Procedures

1. Attach the inlet hose from the condenser unit to a cold water supply and the outlet hose to a drain.
2. Ensure that all valves on the unit are closed.
3. Connect the unit to a 415 VAC 3 phase 50 Hz power supply and switch on the power supply.
4. Switch ON the main power switch in front of both of the control panels on the unit.
5. Open valves V105 and V107 for initial vacuum suction application if desired. Keep an eye on the pressure gauge,
close V105 and V107 when the vacuum pressure reaches 0.2 bar.
6. The unit is now ready for experiments.
7. After the experiment, leave the sieve plate column for 20 minutes to cool down. Turn off the water supply and
disconnect the hoses if not required. Do not open the reboiler cap while the contents are at high temperatures as
vapors might rush out of the tank.
8. For storage purposes during a long break, drain off the contents in the reboiler with valves (DV01), reflux tank
(DV02) and top product tank (DV106). All alcohol samples can be re-used after the experiment, as long as they are
uncontaminated. Else, maintain the tank with alcohol to conduct further experiments.
9. Switch off the main power unit and power supply.

SAFETY AND PRECAUTION

1. Read the safety instructions thoroughly before conducting the experiment.

2. Wear protective gloves, glasses, laboratory protective clothing, long pants and covered shoes when conducting the
experiment.
3. Dispose of all unused chemicals in an appropriate manner after the experiment. Under no circumstances should
the chemicals be allowed to flow into the main drains.
4. Should any of the chemicals come into contact with the body, rinse off immediately with cold water and inform the
lab attendant. Seek medical treatment if symptoms persist.
5. Report any breakages or consumables which need replenishing.
6. Wash your hands thoroughly with soap after the experiment.
7. Be alert and careful at all times when conducting the experiment.
 FACULTY: ENGINEERING EDITION:
TECHNOLOGY
LABORATORY: PROCESS
REVISION NO:
TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: BATCH
DISTILLATION AMENDMENT
DATE:

5.3 EXPERIMENT

EQUIPMENT AND ACCESSORIES

1. LS-32202 Batch Distillation Unit

2. Refractometer & refractive index data
3. 8 L of binary mixture (ethanol-distilled water)
4. Beakers

SAFETY AND PRECAUTION

1. Read the safety instructions thoroughly before conducting the experiment.

2. Wear protective gloves, glasses, laboratory protective clothing, long pants and covered shoes when conducting the
experiment.
3. Dispose of all unused chemicals in an appropriate manner after the experiment. Under no circumstances should
the chemicals be allowed to flow into the main drains.
4. Should any of the chemicals come into contact with the body, rinse off immediately with cold water and inform the
lab attendant. Seek medical treatment if symptoms persist.
5. Report any breakages or consumables which need replenishing
6. Wash your hands thoroughly with soap after the experiment.
7. Be alert and careful at all times when conducting the experiment.
8. Do not operating the water jet vacuum pump when the vapour formed reach at the condenser. You are only
recommended to operate the water jet vacuum pump before the feed start to boil.

EXPERIMENT PRE-PROCEDURE

1. Attach the inlet hose from the condenser unit to a cold water supply and the outlet hose to a drain.
2. Ensure that all hand valves on the unit are closed except the one on the water inlet valve V104.
3. Connect the unit to a 415 VAC 3 phase 50 Hz power supply and switch on the power supply.
 FACULTY: ENGINEERING EDITION:
TECHNOLOGY
LABORATORY: PROCESS
REVISION NO:
TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: BATCH
DISTILLATION AMENDMENT
DATE:

PROCEDURE (CONSTANT & REGULATING FLUX)

1. Prepare a 8 L batch of binary mixture (refer to CHEMICAL PREPARATION) of known composition.

2. Collect a 10 mL of the prepared sample using a syringe and test the refractive index.
3. Pour the mixture into the reboiler as shown in picture 1 in page 23.
4. Switch ON the main power switches on the unit.
5. Close all the valves on this unit.
6. Open valves V105 and V107 if initial vacuum suction is required. Keep an eye on the pressure gauge, close V105
and V107 when the vacuum pressure reaches 0.2 bar.
7. Open valve V104. Start the cooling water supply. NOTE: Do not open valves V105 and V107 when the
experiment is running.
8. Turn on the Reboiler heater ON/OFF switch located on the Control Panel.
9. Set the power of the boiler to maximum using the power regulator.
10. Set the temperature of reboiler, T15 to 88ºC by pressing UP or DOWN button. Note: high power setting is
required in order to supply sufficient energy to warm the system up in the initial startup.
11. Turn on the reflux switch and set the reflux to 100%. The reflux controller indicates percentage of condensate
returning to the column. Open valve V106 on the Top product tank.
12. Wait for the vapor to condense in the glass condenser. Note: please take note of the temperature change on
T11, when T11 reaches about 80ºC, it will begin to show condensate collection.
13. Once the top product appears in the divider vessel, leave the column at total reflux (100%) for another 5 minutes to
allow the system to stabilize.
14. After that, record down all the temperatures as the initial experiment point.
15. Change the reflux ratio to the 80% initially, then 70% after 5 minutes, 60%, 50%, 40% and 30% for every 5 minutes
interval.
16. During the intervals prior to change of reflux control, draw a small sample (approximately 10ml) from the top
product tank (DV03) and reboiler tank (DV01) and m4ceasure and note down the refractive index of each sample
at constant room temperatures. To quickly cool down the reboiler’s sample, place the sample tube in a beaker filled
with cold water. Note: you are recommended to wear protective gloves, glasses, laboratory cloth, long pants
and covered shoes when taking samples from top product (DV03) and reboiler tank (DV01).
17. Take 6 set of readings. Then, empty the top product vessel and measure its volume. This will give us the product
output rate of the system.
18. Tabulate the data obtained in as shown in table 4.
19. All alcohol samples can be re-used after the experiment, as long as they are uncontaminated.

Note: If the system still not working (there are still no flow in the distillation) after 80 oC, open valve DV02 for a while to release the
pressure. After reached 2 bar, close the valve again.
 FACULTY: ENGINEERING EDITION:
TECHNOLOGY
LABORATORY: PROCESS
REVISION NO:
TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: BATCH
DISTILLATION AMENDMENT
DATE:

6.0 RESULTS & CALCULATION

Table 3: batch distillation result tabulate table

Reflux (%) 100% 80% 70% 60% 50% 40% 30%

Top product
Refractive index
Composition (mol%)
Bottom product
Refractive index
Composition (mol%)
 FACULTY: ENGINEERING EDITION:
TECHNOLOGY
LABORATORY: PROCESS
REVISION NO:
TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: BATCH
DISTILLATION AMENDMENT
DATE:

7.0 DATA ANALYSIS

Equilibrium Data for Ethanol-Water Mixtures

Mole fraction of ethanol in liquid, x Mole fraction of ethanol in vapour, y

0.00 0.00
0.02 0.192
0.05 0.377
0.1 0.527
0.2 0.656
0.3 0.713
0.4 0.746
0.5 0.771
0.6 0.794
0.7 0.822
0.8 0.858
0.9 0.912
0.94 0.942
0.96 0.959
0.98 0.978
1.0 1.0

Steps for drawing Mc-Cabe Thiele graph

1) Use 3 different reflux ratio (70%, 50% and 30%). So it will have 3 graphs.

2) Draw equilibrium curve.

3) Draw 45o line.

4) Feed: xF= 0.5.

5) Draw the q line (q= 1).

6) Find the distillate, xD,and bottom, xW ,composition.

7) Draw the rectifying and stripping line.

8) Determine the distillation column theoretical stages.

 FACULTY: ENGINEERING EDITION:
TECHNOLOGY
LABORATORY: PROCESS
REVISION NO:
TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: BATCH
DISTILLATION AMENDMENT
DATE:

8.0 DISCUSSION & CONCLUSION

1. Discuss the advantages of a bubble cap distillation column compared to sieve plate and valve plate columns.
2. As a process design engineer, given a set of product output quality and flow requirements, describe how you would
proceed in designing the distillation system and calculate the cost of operations.

Approved by / Disahkan oleh :

Prepared by / Disahkan oleh:

Signature / Tandatangan :
Signature/Tandatangan:
Name / Nama : EN. BACHIK BIN ABU BAKAR
Name/Nama: DR. NURASYIKIN BINTI MISDAN

Date/Tarikh :
Date / Tarikh :