January 2010

EXPERIMENT NO: 1

BATCH REACTION PROCESS

OBJECTIVES

1) To study the liquid phase reaction kinetics in a batch reactor.

2) To study the operation of a batch reactor at different operating conditions in terms of
conversion.
3) To study the effect of temperature on the reaction in CSTR

Keywords: Batch reactor; Kinetics; Saponification reaction; Activation energy

2.0

GENERAL DESCRIPTION
2.1

Description and Assembly

Before operating the unit and running experiments, you must familiarize
yourself with the units components. Please refer to Figure 2 to understand
the process. All glass components of the QVF Batch Reactor unit are made
of borosilicate glass with PTFE gaskets.
1. Reactor (R1)

Fused jacketed vessel with graduation, nominal capacity 10 L

Bottom port for dead space reduced bottom outlet valve
Jacket connections for heating agent
Cover DN300 with connections for: Agitator
Charge port with screw cap for feeding by hand
Inlet for dosing vessel B1
Vapour pipe with connection for distillate and vapour trap
Conductivity and temperature sensor

2. Agitator (A1)

Laboratory drive 230V / 50,60Hz

0.25 kW, 0-550 rpm, steplessly adjustable by hand

3. Dosing vessel (B1)

2,000 mL graduated cylindrical vessel with overflow pipe

4. Condenser (W1)

Coil heat exchanger, area 0.3 m

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CKD 20002 (REACTOR TECHNOLOGY), Experiment 1: Batch Reactor

January 2010

Max coolant pressure of 3 bars with allowable temperature difference of

130C

5. Instrumentation

2.2

Temperature measurement (TI-101)

Conductivity measurement (QI-401)

Safety Considerations
1. Students must not carry out laboratory work without the supervision of a
lecturer.
2. Read operating instructions carefully, and make sure that you fully
understand all aspects of operation of the batch reactor unit.
3. Safety glasses must be worn at all times during these experiments
remember you are in charge of all safety aspects.
4. For each experimental setting, allow 10 minutes for equilibrium conditions
to be established.
5. After each experiment, make sure that the reactor and tubing are cleaned
properly. Sodium hydroxide and ethyl acetate both are corrosive and can
damage the tubings and the reaction rig.
6. Dispose all liquids immediately after each experiment. Do not leave any
reactants or product in the feed or product vessels.
7. Wipe off any spillage on the ground or working bench.
8. Plastic gloves and eye shields must be worn when handling corrosive
liquids, and heat resistant gloves when adjusting steam valves.

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CKD 20002 (REACTOR TECHNOLOGY), Experiment 1: Batch Reactor

January 2010

9. All experiments involving a potential explosive hazard must be conducted

behind special shields.
10. When working with solvents etc., ensure that the apparatus is adequately
vented.
11. All used solvent should be handed to the technician and not disposed
into drains or laboratory sinks.
12. Smoking is forbidden in all laboratories.
13. Safety helmets must be worn.
14. Services equipment (vacuum generators) must in no circumstances be
started up by students.
15. Gas cylinders, when in use, should be adequately strapped to bench and
supported in the upright position, away from sunlight or flames. Ensure
that cylinders are shut-off after use.
16. Before using any chemical, ensure that you are familiar with its hazards
and with emergency procedures.
17. If in doubt, ask the lecturer in charge.
18. If chemical spillage occurs, evacuate the laboratory in an orderly fashion.
19. Plug in all cables into appropriate sockets before switching on the main
switch. Inspect all cables for any damage to avoid electric shock.
Replace if necessary.
20. Do not switch on the heater unless it is fully submerged in the liquid.
Always maintain liquid level above the height of the heater to avoid
damage to the heater.

3.0

OPERATING PROCEDURES
3.1

General Start-Up Procedures

1. Prepare the following solutions:
a) 9 L of sodium hydroxide, NaOH (0.1 M)
b) 9 L of ethyl acetate, Et (Ac) (0.1 M)
2. Ensure that all valves are initially closed.
3. Turn on the power for the control panel.
4. Open cooling water valve and let the cooling water flow through the
condenser.
5. The unit is now ready for experiment.

3.2

General Shut-Down Procedures

1. Keep the cooling water valve open to allow the cooling water to
continue flowing.

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CKD 20002 (REACTOR TECHNOLOGY), Experiment 1: Batch Reactor

January 2010

2. Switch off the pump and heating. Let the liquid in the reaction vessel
cool down to room temperature.
3. Switch off the stirrer.
4. Close cooling water valve.
5. Open bottom valve to drain any liquid from the unit.
6. Turn off the power for the control panel.

4.0

EXPERIMENTAL PROCEDURES

4.1

EXPERIMENT 1: Batch Saponification Reaction

OBJECTIVE:

To carry out a batch saponification reaction between Et(Ac) and

NaOH.

PROCEDURES:
1. Perform the general start-up procedures.
2. Measure and carefully pour 3 L of 0.1 M ethyl acetate solution into the
reactor R1 through the charge port on the vessel cover.
3. Then, measure and carefully pour 3 L of 0.1 M sodium hydroxide solution
into the reactor R1 through the charge port on the vessel cover.
4. Switch on the stirrer and set the speed to 300 rpm. Set the heating
temperature T1 and T2 at 40C.
5. Start the timer simultaneously.
6

At every 5-minute intervals, open sampling valve (at the bottom) and
collect a 2 mL sample. Carry out a conductivity measuring by using
conductivity meter.

8. Record your conductivity value in the table Appendix B.

7. End the experiment when the conductivity values do not change
significantly over time.
8. Perform the general shut-down procedures.
ANALYSIS AND DISCUSSION:
1. Use the sample table in Appendix B for data collection.
2. By using the data in the sample table in Appendix A,
i)

Plot the calibration curve of Concentration of NaOH (M) vs

Conductivity. Determine the slope and y-axis intercept.

ii)

Plot the calibration curve of Conversion vs Conductivity.

Determine the slope and y-axis intercept.

4. For an equimolar reaction with the same initial reactants concentration

(CA0 = CB0), the rate law is shown to be:
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CKD 20002 (REACTOR TECHNOLOGY), Experiment 1: Batch Reactor

January 2010

-rA = - dCA/dt = kCA

ln [- dCA/dt] = ln k + ln CA
where CA is the concentration of NaOH in the reactor at time t.

4.2

i)

Plot a graph of ln [- dCA/dt] vs ln CA and evaluate the slope

and y-axis intercept

ii)

Determine the order of the reaction, and the rate constant

from the slope and intercept values.

EXPERIMENT 2: Effect of Temperature on the Batch Saponification

Reaction
OBJECTIVE:

To determine the effect of temperature on the extent of conversion.

PROCEDURES:
1. Perform the general start-up procedures.
2. Measure and carefully pour 3 L of 0.1 M ethyl acetate solution into the
reactor R1 through the charge port on the vessel cover.
3. Then, measure and carefully pour 3 L of 0.1 M sodium hydroxide solution
into the reactor R1 through the charge port on the vessel cover.
4. Switch on the stirrer and set the speed to 300 rpm. Set the heating
temperature T1 and T2 at 50C.
5. Start the timer simultaneously.
6. At every 5-minute intervals, open sampling valve (at the bottom) and
collect a 2 mL sample. Carry out a conductivity measuring by using
conductivity meter.
7. Record your conductivity value in the Appendix B.
8. End the experiment when the conductivity values do not change
significantly over time.
9. Repeat the procedure 1-8 with the temperature at 60C.
10. Perform the general shut-down procedures.
ANALYSIS AND DISCUSSION:
1. Use the sample table in Appendix B for data collection.
2. Plot a graph conversion vs time at different temperature and
subsequently compare the conversions for the different temperature.
Discuss it thoroughly and include explanations on the effect of
temperature onto the reaction.
3. For a second order reaction, the rate law is shown to be:
-rA = - dCA/dt = kCA
CA

CA0

dCA/ CA2 = -k

dt
0

1/CA = kt + 1/CA0
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CKD 20002 (REACTOR TECHNOLOGY), Experiment 1: Batch Reactor

January 2010

Where CA0 is the initial concentration of reactant NaOH in the reactor.

i)

For each temperature value (40, 50 & 60 C), plot the graph of
1/CA vs time, t and evaluate the slope and y-axis intercept.

ii)

Determine the rate constant, k from the slope value for different
temperature values. Examine the change in the rate constant.

iii)

Plot a graph of ln k vs 1/T and evaluate the slope and y-axis

intercept.

iv)

Calculate the saponification reactions activation energy, E and

Arrhenius constant, A from the slope and intercept values using
the Arrhenius equation.

k (T ) = Ae E / RT , (R = 8.3014 J/mol.K).
4. Discuss the advantages and disadvantages of using batch reactors in
chemical reaction.
5. List down the problems encountered when running the experiment and
suggest methods of improvement.

5.0

TUTORIAL
1. Describe an example of industrial applications other than saponification that
utilized batch reactors in its process.
2. Write down the function of each following component in a batch reactor used in
this experiment.
Stirrer
Thermocouple
Temperature controller

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CKD 20002 (REACTOR TECHNOLOGY), Experiment 1: Batch Reactor

January 2010

APPENDIX A

TABLE OF CALIBRATION CURVE

Solution Mixtures
Conversion

Concentration
of NaOH (M)

Conductivity
(mS/cm)

0.1 M NaOH

0.1 M Na(Ac)

H2O

0%

100 mL

100 mL

0.0500

10.7

25%

75 mL

25 mL

100 mL

0.0375

9.7

50%

50 mL

50 mL

100 mL

0.0250

7.5

75%

25 mL

75 mL

100 mL

0.0125

5.6

100%

100 mL

100 mL

0.0000

4.0

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CKD 20002 (REACTOR TECHNOLOGY), Experiment 1: Batch Reactor

January 2010

APPENDIX B
TABLE FOR EXPERIMENTS 1

Volume of NaOH

= _____ L

Volume of Et(Ac)

= _____ L

Initial concentration of NaOH

= _____ M

Initial concentration of Et(Ac)

= _____ M

Time
(min)

Temperature
(C)

Conductivity
(mS/cm)

Concentration of
NaOH, CNaOH (M)

Conversion,
X (%)

0
5
10
15
20
25
30
35
40
45
50
55
60

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CKD 20002 (REACTOR TECHNOLOGY), Experiment 1: Batch Reactor

January 2010

TABLE FOR EXPERIMENTS 2

Volume of NaOH

= _____ L

Volume of Et(Ac)

= _____ L

Initial concentration of NaOH

= _____ M

Initial concentration of Et(Ac)

= _____ M

Time
(min)

Temperature
(C)

Conductivity
(mS/cm)

Concentration of
NaOH, CNaOH (M)

Conversion,
X (%)

0
5
10
15
20
25
30
35
40
45
50
55
60

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CKD 20002 (REACTOR TECHNOLOGY), Experiment 1: Batch Reactor

January 2010

TABLE FOR EXPERIMENTS 2

Volume of NaOH

= _____ L

Volume of Et(Ac)

= _____ L

Initial concentration of NaOH

= _____ M

Initial concentration of Et(Ac)

= _____ M

Time
(min)

Temperature
(C)

Conductivity
(mS/cm)

Concentration of
NaOH, CNaOH (M)

Conversion,
X (%)

0
5
10
15
20
25
30
35
40
45
50
55
60

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CKD 20002 (REACTOR TECHNOLOGY), Experiment 1: Batch Reactor

10