January 2016

EXPERIMENT NO: 2

CONTINUOUS STIRRED TANK REACTOR

OBJECTIVES

1). To study liquid phase reaction kinetics in a CSTR

2). To determine the conversion at different residence time.

3). To study the effect of temperature on the reaction in CSTR.

Keywords: CSTR; residence time; Mixing; Saponification kinetics; Activation energy

2.0 GENERAL DESCRIPTION

2.1 Description & Assembly

Before operating the unit and running experiments, you must familiarize
yourself with the unit’s components. Please refer to Figure 1 to understand
the process. All glass components of the QVF Continuous Stirred Tank
Reactor unit are made of borosilicate 3.3 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 feed vessels B1 and B2
Vapour pipe
Integrated conductivity and temperature sensor

2. Agitator (A1)
Laboratory drive 230V / 50,60Hz
0.11 kW, 50-700 rpm, steplessly adjustable by hand, max torque 60 Ncm

3. Feed vessels (B1/B2)

50 L graduated cylindrical vessels

4. Pumps (P1/P2)
Centrifugal pumps
Max suction height of 3 m

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CKD 20002 (REACTOR TECHNOLOGY), Experiment 2: Continuous Stirred Tank Reactor
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5. Condenser (W1)
2
Coil heat exchanger, area 0.2 m
Max coolant pressure of 2 bar with allowable temperature difference of
150°C

6. Receiving vessel (B3)

100 L rectangular tank

7. Instrumentation
Flow measurement (FI-301, FI-302)
Temperature measurement (TI-101)
Conductivity measurement (QI-401)

2.2 Safety Considerations

1. The unit must be operated under the supervision of an authorized staff

that has been properly trained to handle the unit.
2. All operating instructions supplied with the unit must be carefully read
and understood before attempting to operate the unit.
3. Feed stock which severely affects PTFE, PFA and borosilicate glass are
not to be used.
4. The system should not be subjected to shock, sudden impact, vibration,
additional load, or permanent external action of aggressive vapours.
5. Always check and rectify any leakages.
6. Do not touch the hot components of the unit.
7. Be extremely careful when handling hazardous, flammable or polluting
materials.
8. Restore the system to operating conditions after any repair job.
9. Make sure the system is sufficiently ventilated when working at
atmospheric pressure.
10. Do not exceed the maximum cooling pressure of 2 bar (g) for the top
condenser (W3) and product cooler (W4).
11. Only a properly trained staff should be allowed to carry out any servicing.
Manufacturer's manual must always be observed.
12. Before any servicing, shut down the whole operation, let the system cool
down and be properly ventilated.
13. Do not use any coarse or abrasive cleaners on glass components.
14. Leaking couplings should be carefully retightened. Replace any gaskets
or seals if necessary.

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CKD 20002 (REACTOR TECHNOLOGY), Experiment 2: Continuous Stirred Tank Reactor
 January 2016

Vent

V1 V6

Cooling
Water
B1 B2 W1 Cooling
Water
V13
HS
1

Q1
M 401

TI
101
V2 V7
FI FI
301 302

V5 V10 R1
V3 V8
V3

V11
V4 V9
P1 P2
M M V12
HS HS
2 3 B3 T1
Figure 1: Continuous Stirred Tank Reactor (CSTR)

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3.0 OPERATING PROCEDURES

3.1 General Start-up Procedures

1. Prepare the following solutions:

a) 25 L of sodium hydroxide, NaOH (0.1 M)
b) 25 L of ethyl acetate, Et(Ac) (0.1 M)
2. Ensure that all valves are initially closed.
3. Charge the feed vessels as follows:
a) Open the charge port caps for vessels B1 and B2.
b) Carefully pour the NaOH solution into vessel B1 and the Et(Ac) solution
into vessel B2.
c) Close the charge port caps for both vessels.
4. Turn on the power for the control panel.
5. Check that there is sufficient water in the thermostat T1 tank. Refill as
necessary.
6. Open cooling water valve V13 and let the cooling water flow through the
condenser W1 (*Exp B only).
7. Switch on the thermostat T1 and set the water temperature to desired
temperature (*Exp B only).
8. Open valve V2, V7 and V11.
9. The unit is now ready to be used for an experiment.

3.2 General Shut-Down Procedures

1. Keep the cooling water valve V13 open to allow the cooling water to continue
flowing.
2. Switch off both pumps P1 and P2. Switch off the stirrer M1.
3. Switch off the thermostat T1. Let the liquid in the reaction vessel R1 cool
down to room temperature.
4. Close cooling water valve V13.
5. Open valves V4, V9 and V12 to drain any liquid from the unit.
6. Turn off the power for the control panel.

4.0 EXPERIMENTAL PROCEDURES

4.1 EXPERIMENT A: Effect of RTD on the Reaction in a CSTR

OBJECTIVES:
 To carry out a saponification reaction between NaOH and Et(Ac) in a CSTR.
 To determine the effect of residence time on the extent of conversion.

PROCEDURES:

1. Perform the general start-up procedures.

2. Open valves V5 and V10.
3. Switch ON both pumps P1 and P2 simultaneously.
4. Let the reactor fill up with both solutions until it is just about to 1/2 full.

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CKD 20002 (REACTOR TECHNOLOGY), Experiment 2: Continuous Stirred Tank Reactor 4
 January 2016

5. Readjust the valves V5 and V10 to give a flow rate of about 100 mL/min.
Make sure that both flow rates are the same.
6. Switch ON the stirrer M1.
7. Start the timer simultaneously.
8. Record the conductivity value at Q1-401 for every 5 minutes until it does not
change over time. This is to ensure that the reactor has reached steady state.
9. End the experiment when the conductivity values do not change significantly
over time (30 minutes).
10. Repeat the experiment (steps 3 to 9) for different residence times by
adjusting the feed flow rates of NaOH and Et(Ac) to about 200 mL/min and
300 mL/min. Make sure that both flow rates are maintained the same.
11. Perform the general shut-down procedures.

ANALYSIS AND DISCUSSION:

1. Use the table for data collection at Appendix B.

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.
# Use the equation (i) and (ii) to determine the value of concentration of
NaOH (M) and conversion (%) in sample table in Appendix B.
3. Plot a graph of conversion vs. time for the different residence time (flow
rates) (100, 200 and 300 mL/min). The reactor’s residence time is defined as
the reactor volume divided by the total feed flow rates.
VCSTR
Residence time,  
F0
Compare the conversion at the different residence time. Discuss the graph
thoroughly and explain how it can influence the rate of reaction.
4. For a second order equimolar reaction with the same initial reactants’
concentration (CA0 = CB0), the rate law is shown to be:

 rA  kC A CB  kC 2A

FA 0 X
VCSTR 
 rA

FA 0 X F0 C A 0  C A 
VCSTR  
kC 2A kC 2A
where X is extent of conversion, CA is exit concentration of reactant NaOH
(M), F0 is total inlet flow rate of solutions (mL/min) and C A0 is inlet
concentration of reactant NaOH in the reactor (M).
5. For different reactor residence times, calculate the value of the reaction rate
constant, k and the rate of reaction, -rA.

Reaction rate constant, k 

C A0  C A 
C 2A

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CKD 20002 (REACTOR TECHNOLOGY), Experiment 2: Continuous Stirred Tank Reactor 5
 January 2016

Rate of reaction,  rA  kC 2A

4.2 EXPERIMENT B: The Effect of Temperature on the Reaction in a CSTR

OBJECTIVES:
 To determine the effect of temperature on the extent of conversion.

PROCEDURES:

1. Perform the general start-up procedures.

2. Set the thermostat T1 temperature to 40°C.
4. Open valves V5 and V10.
5. Switch on both pumps P1 and P2 simultaneously.
6. Let the reactor fill up with both solutions until it is just about to 1/2 full.
7. Readjust the valves V5 and V10 to give a flow rate of 100 mL/min. Make sure
that both flow rates are the same.
8. Switch ON the stirrer M1.
9. Start the timer simultaneously.
10. Record the conductivity value at Q1-401 for every 5 minutes until it does not
change over time. This is to ensure that the reactor has reached steady state.
10. End the experiment when the conductivity values do not change significantly
over time (30 minutes).
11. Repeat the experiment (steps 2 to 10) for different reactor temperatures by
setting the thermostat temperature to 50 °C and 60 °C. Make sure that the
flow rates of both solutions are maintained at 100 mL/min.
12. 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.
# Use the equation (i) and (ii) to determine the value of concentration of
NaOH (M) and conversion (%) in sample table in Appendix B.
3. Plot a graph of conversion (X) vs. time (t) for different reactor temperature
(40, 50 & 60 C). Compare the conversion at the different temperature.
Discuss the graph thoroughly and explain how it can influence the rate of
reaction.
4. For different reactor temperatures, calculate the value of the reaction rate
constant (k) and rate of reaction (-rA).

Reaction rate constant, k 

C A0  C A 
C 2A

Rate of reaction,  rA  kC 2A

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5. Calculate the Saponification reaction’s activation energy, E and frequency

factor (A) from the slope and intercept values using the Arrhenius equation.

kT  AeE / 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. What will be the effect of flow rates and temperature on the reaction rate and rate
constant?
2. Why the CSTR is so special compared to Batch & Tubular (PFR) reactor?
3. Discuss the advantages and disadvantages of using CSTR reactors in chemical
reaction.

APPENDIX A

RESULTS FOR PREPARATION OF CALIBRATION CURVE

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CKD 20002 (REACTOR TECHNOLOGY), Experiment 2: Continuous Stirred Tank Reactor 7
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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

RESULTS FOR EXPERIMENTS A & B

Reactor volume = _____ L Flowrate = _____ mL/min

o
Concentration of NaOH in feed vessel = _____ M Temperature = _____ C
Concentration of Et(Ac) in feed vessel = _____ M

Flow rate of Flow rate of

Temperature Total flow rate Conductivity Concentration of
NaOH Et(Ac) Residence Conversion,
Time (°C) of solutions, (mS/cm) NaOH,
(mL/min) (mL/min) time,  (min) X (%)
TI-101 F0 (mL/min) QI-401 CNaOH (M)
FI-301 FI-302

0
5
10
15
20
25
30

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CKD 20002: Reactor Technology, Experiment 2: Continuous Stirred Tank Reactor
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RESULTS FOR EXPERIMENTS A & B

Reactor volume = _____ L Flowrate = _____ mL/min

o
Concentration of NaOH in feed vessel = _____ M Temperature = _____ C
Concentration of Et(Ac) in feed vessel = _____ M

Flow rate of Flow rate of

Temperature Total flow rate Conductivity Concentration of
NaOH Et(Ac) Residence time, Conversion,
Time (°C) of solutions, (mS/cm) NaOH,
(mL/min) (mL/min)  (min) X (%)
TI-101 F0 (mL/min) QI-401 CNaOH (M)
FI-301 FI-302

0
5
10
15
20
25
30

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CKD 20002: Reactor Technology, Experiment 2: Continuous Stirred Tank Reactor
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RESULTS FOR EXPERIMENTS A & B

Reactor volume = _____ L Flowrate = _____ mL/min

o
Concentration of NaOH in feed vessel = _____ M Temperature = _____ C
Concentration of Et(Ac) in feed vessel = _____ M

Flow rate of Flow rate of

Temperature Total flow rate Conductivity Concentration of
NaOH Et(Ac) Residence time, Conversion,
Time (°C) of solutions, (mS/cm) NaOH,
(mL/min) (mL/min) (min) X (%)
TI-101 F0 (mL/min) QI-401 CNaOH (M)
FI-301 FI-302

0
5
10
15
20
25
30

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CKD 20002: Reactor Technology, Experiment 2: Continuous Stirred Tank Reactor