July 2018

EXPERIMENT NO: 1

BATCH REACTOR

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 batch reactor.

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 unit’s 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

2

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 Max coolant pressure of 3 bars with allowable temperature difference of

130°C

5. Instrumentation

 Temperature measurement (TI-101)

 Conductivity measurement (QI-401)

2.2 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 tubing’s 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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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 (V5) and let the cooling water flow through the
condenser.

5. Switch on the heater and set the heating temperature T1 at 40C.

6. The unit is now ready for experiment.

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3.2 General Shut-Down Procedures

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

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 1A: 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.
5. Start the timer simultaneously.
6 At every 5-minute intervals, open sampling valve (at the bottom) and
collect a 10 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 (30 minutes).
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.
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# Use the linear equation (i) and (ii) to determine the value of
concentration of NaOH (M) and conversion (%) in sample table in
Appendix B.
4. For an equimolar reaction with the same initial reactants’ concentration
(CA0 = CB0), the rate law is shown to be:
α
-rA = - dCA/dt = kCA
ln [- dCA/dt] = ln k + α ln CA
where CA is the concentration of NaOH in the reactor at time t.
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 (α) and the rate constant (k)
from the slope and intercept values.

4.2 EXPERIMENT 1B: 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. Set the heating temperature T1 at 50C. Switch on the stirrer.
5. Start the timer simultaneously.
6. At every 5-minute intervals, open sampling valve (at the bottom) and
collect a 10 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 (30 minutes).
9. Repeat the procedure 2 – 8 with the temperature at 60C.
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 of Conversion (%) vs Time (min) at different temperature
(40, 50 & 60 C) and subsequently compare the conversions for the
different temperature. Discuss the trend 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:
2
–rA = - dCA/dt = kCA
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CA t

  dt
2
dCA/ CA = -k
CA0 0

1/CA = kt + 1/CA0
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 (min) 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.
4. Calculate the saponification reaction’s activation energy, Ea and
frequency factor, A using the Arrhenius equation.

k T   Ae  Ea / RT , (R = 8.3014 J/mol.K)
Ea  1
lnk  lnA   
R T
i) Plot a graph of ‘ln k’ vs ‘1/T’ (T in Kelvin unit).
ii) Determine activation energy (Ea) and frequency factor (A) from
the slope and intercept values.

5.0 TUTORIAL

1. Discuss the advantages and disadvantages of using batch reactors in chemical

reaction.
2. Determine the effect of temperature on chemical reaction.
3. Write down the function of each following component in a batch reactor used in
this experiment.
 Stirrer
 Thermocouple
 Temperature controller

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APPENDIX A

TABLE OF CALIBRATION CURVE

Solution Mixtures
Concentration Conductivity
Conversion
of NaOH (M) (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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APPENDIX B

TABLE FOR EXPERIMENT A

Volume of NaOH = _____ L

Volume of Et(Ac) = _____ L
Initial concentration of NaOH = _____ M
Initial concentration of Et(Ac) = _____ M

Concentration of Conversion,
Temperature
Time Conductivity NaOH, CNaOH (M) X (%)
(°C)
(min) (mS/cm) (from calibration (from calibration
TI-101
curve) curve)

0
5
10
15
20
25
30

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TABLE FOR EXPERIMENT B

Volume of NaOH = _____ L

Volume of Et(Ac) = _____ L
Initial concentration of NaOH = _____ M
Initial concentration of Et(Ac) = _____ M

Temperature: 50C

Concentration of Conversion,
Temperature
Time Conductivity NaOH, CNaOH (M) X (%)
(°C)
(min) (mS/cm) (from calibration (from calibration
TI-101
curve) curve)

0
5
10
15
20
25
30

Temperature: 60C

Concentration of Conversion,
Temperature
Time Conductivity NaOH, CNaOH (M) X (%)
(°C)
(min) (mS/cm) (from calibration (from calibration
TI-101
curve) curve)

0
5
10
15
20
25
30

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CKD 20003 (REACTOR TECHNOLOGY), Experiment 1: Batch Reactor