LABORATORY MANUAL (JAN 2018) REACTION ENGINEERING (CKB 20104)

EXPERIMENT 4
REACTOR TEST RIG
OBJECTIVES
To compare the performance of single reactor, 3 CSTRs AND PFR.

Keywords: CSTR, PFR, Reactors in series; Conversion; Residence time distribution (RTD) studies

1.0 GENERAL DESCRIPTION

1.1 Description and 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 Reactor Test Rig unit are made of
borosilicate 3.3 glass with PTFE gaskets.

1. Reactor (R1)

 Jacketed cylindrical vessel, 4 L nominal capacity

2. Cascaded reactors (R2/R3/R4)

 Jacketed cylindrical vessel, 1 L nominal capacity each

3. Plug flow reactor (SR1)

 Jacketed pipe with approximate capacity of 3.0 L

4. Feed vessels (B1/B2)

 100 L PE rectangular vessels with all necessary connections

5. Dosing vessels (HB1/HB2)

 1 L cylindrical vessels with overflow port and bottom port

6. Pumps (P1/P2)

 Centrifugal pumps

 max delivery rate of 60 L/h and max delivery height of 8 m

7. Pre-heater (W1/W2)

 Coil heat exchanger, area 0.06 m2

 max heating media pressure of 0.5 bar

8. Receiving vessel (B3)

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LABORATORY MANUAL (JAN 2018) REACTION ENGINEERING (CKB 20104)

 100 L rectangular tank

9. Instrumentations

 Flow measurements (FI-301, FI-302, FI-303)

 Temperature measurements (TI-101, TI-102, TI-103, TI-104)

 Conductivity measurements (QI-401, QI-402, QI-403, QI-404)

1.2 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 leak.

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 shall be allowed to carry out any servicing.
Manufacturer's manual must always be observed.

12. Before any servicing, shut down the whole operation and let the system to
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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LABORATORY MANUAL (JAN 2018) REACTION ENGINEERING (CKB 20104)

Vent

V22 V23 V24 M2 V25

HS
4
QI
404
M M3
HS
TI
5
104

M M4
HB1 HB2 HS T1
6
TI
103
M
QI
403
R2
M1 V16
HS
3 R3
TI

V1 V2
102 V17
M
QI
402 R4
SR1
W1 W2 V18

V11 V12 V13

QI TI
401 101 R1
V14
Injection
V15
FI FI FI
B1 B2 301 302 303

V19 V20 V21

V8 V9 V10

P1 P2 V27
V3 V4
M M V5 V6 Process Water
HS HS
V7
1 2 B3 V26

Figure 4: Reactor Test Rig

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LABORATORY MANUAL (JAN 2018) REACTION ENGINEERING (CKB 20104)

2.0 OPERATING PROCEDURES

2.1 General Start-Up Procedures for Experiment
1. Ensure that all valves are initially closed.
2. Prepare the following solutions:
a) 50 L of sodium hydroxide, NaOH (0.1 M)
b) 50 L of ethyl acetate, Et(Ac) (0.1 M)
3. Fill the feed vessel B1 with the NaOH solution and feed vessel B2 with the Et(Ac)
solution.
4. Turn on the power for the control panel.
5. Open the process water valve V27.
6. Open valves V1 and V2.
7. Switch on both pumps P1 and P2. Observe the flow of NaOH and Et(Ac) solutions
into the dosing vessels HB1 and HB2, towards valves V10 and V9 respectively.
8. Make sure that the pipelines before valves V9 and V10 are filled with liquid. Bleed
any trapped air in the pipelines by using valves V9 and V10.
9. Allow both solutions to overflow in the dosing vessels HB1 and HB2 into the feed
vessels B1 and B2 respectively.
10. The unit is now ready for experiment.
2.2 Selection of Reactors
Any one of the three reactors provided in the reactor test rig can be used for each of
the experiments. The following procedures will explain the steps needed to select a
particular reactor to run an experiment.
1. Ensure that all valves from V3 to V21 are closed.
2. For the plug flow reactor SR1:
a) Open valves V11 and V19.
b) Read the outlet conductivity value from QI-404 and temperature value from
TI-104.
3. For the single stage continuous stirred tank reactor R1:
a) Open valves V13 and V14.
b) Switch on the stirrer M1.
c) Read the outlet conductivity value from QI-402 and temperature value from
TI-102.
4. For the 3-stage continuous stirred tank reactors R2, R3 and R4:
a) Open valves V12 and V21.
b) Switch on the stirrers M2, M3 & M4.

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LABORATORY MANUAL (JAN 2018) REACTION ENGINEERING (CKB 20104)

c) Read the outlet conductivity value from QI-403 and temperature value from
TI-103.
2.3 General Shut-Down Procedure
1. Switch off both pumps P1 and P2.
2. Close the process water valve V27.
3. Open valves V3 to V21 and valve V26 to drain all liquid from the unit.
4. Turn off the power for the control panel.

3.0 EXPERIMENTAL PROCEDURES

3.1 OBJECTIVE:

 To carry out a saponification reaction between NaOH and Et(Ac) using

different types of reactors.
 To compare the reaction conversion between different types of reactors.
 To determine the reaction rate constant.

3.2 PROCEDURES:
1. Perform the general start-up procedures

Plug Flow Reactor, PFR

2. Open valves V11 and V19.
3. Open valves V9 (Monitor at FI-302) and V10 (Monitor at FI-303) and adjust
valves V9 and V10 to give a flow rate of about 200 mL/min. Make sure that
both flow rates are the same.
4. Allow both the NaOH and Et(Ac) solutions to enter the selected reactor and
empty into the receiving vessel B3.
5. Adjust valves V9 (FI-302) and V10 (FI-303) to give the desired flow rate.
Make sure that both flow rates are the same.
6. Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-404).
7. Start the timer and record both conductivity values (QI-401 and QI-404) and
flow rates (FI-302 and FI-303) when it has reached steady state
(Conductivity value begin to steadily decline with time).
8. Record the inlet and outlet conductivity and flow rate of the reactor for every
5 minutes until they do not change over time. This is to ensure that the
reactor has reached steady state.
9. Repeat the experiment (steps 2 to 6) by selecting a different reactor.
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LABORATORY MANUAL (JAN 2018) REACTION ENGINEERING (CKB 20104)

Single stage continuous stirred tank reactor

1. Open valves V13 and V14.
2. Open valves V9 (Monitor at FI-302) and V10 (Monitor at FI-303) and adjust
valves V9 and V10 to give a flow rate of about 200 mL/min. Make sure that
both flow rates are the same.
3. Allow both the NaOH and Et(Ac) solutions to enter the selected reactor and
empty into the receiving vessel B3.
4. Switch on the stirrer M1.
5. Adjust valves V9 (FI-302) and V10 (FI-303) to give the desired flow rate.
Make sure that both flow rates are the same.
6. Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-402).
7. Start the timer and record both conductivity values (QI-401 and QI-402) and
flow rates (FI-302 and FI-303) when it has reached steady state
(Conductivity value begin to steadily decline with time).
8. Record the inlet and outlet conductivity and flow rate of the reactor for every
5 minutes until they do not change over time. This is to ensure that the
reactor has reached steady state.
9. Repeat the experiment (steps 2 to 6) by selecting a different reactor.

3-stage continuous stirred tank reactors

1. Open valves V12 and V21.
2. Open valves V9 (Monitor at FI-302) and V10 (Monitor at FI-303) and adjust
valves V9 and V10 to give a flow rate of about 200 mL/min. Make sure that
both flow rates are the same.
3. Allow both the NaOH and Et(Ac) solutions to enter the selected reactor and
empty into the receiving vessel B3.
4. Switch on the stirrer M2, M3 and M4.
5. Adjust valves V9 (FI-302) and V10 (FI-303) to give the desired flow rate.
Make sure that both flow rates are the same.
6. Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-403).
7. Start the timer and record both conductivity values (QI-401 and QI-403) and
flow rates (FI-302 and FI-303) when it has reached steady state
(Conductivity value begin to steadily decline with time).
8. Record the inlet and outlet conductivity and flow rate of the reactor for every
5 minutes until they do not change over time. This is to ensure that the
reactor has reached steady state.

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LABORATORY MANUAL (JAN 2018) REACTION ENGINEERING (CKB 20104)

4.0 ANALYSIS AND DISCUSSION:

1. Use the sample table in Appendix B for data collection.

2. Find the concentration of NaOH exiting the reactor from the calibration curve.
Subsequently calculate the conversion, X based on the formula given in Appendix.

3. Plot a graph of conversion, X vs. reaction time for each of the reactor.

4. Compare the graphs between the different types of reactors and observe the
relationship. Based on the experimental results, discuss which configurations are
the best for this reaction and state the reasons accordingly.

5. Determine the following parameters:

a) Single stage CSTR

1. The reactor’s residence time is defined as the reactor volume divided by

the average total feed flow rates.

VCSTR
Residence Time, t =
F
0

Subsequently calculate the average residence time, τavg

2. Calculate the value of the reaction rate constant, k and the rate of
reaction, –rA.

Reaction rate constant, k =

(C A0
- CA ) AND Rate of reaction, - r = kC A2
t avg C 2
A
A

τavg = Average residence time (min)

CA = Exit concentration of reactant NaOH (M)
(Note: Concentration of NaOH at the highest conversion, X)
CA0 = Inlet concentration of reactant NaOH (M) (Concentration at
t=0)

b) 3-stage CSTR’s in series

1. The reactor’s residence time is defined as the reactor volume divided by

the average total feed flow rates.

VCSTR
Residence Time, t =
F
0

Subsequently calculate the average residence time, τavg

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LABORATORY MANUAL (JAN 2018) REACTION ENGINEERING (CKB 20104)

2. Calculate the value of the reaction rate constant, k and the rate of
reaction, –rA.

Reaction rate constant, k =

(C A0
- CA ) AND Rate of reaction, - r = kC A2
t avg C 2
A
A

τavg = Average residence time (min)

CA = Exit concentration of reactant NaOH (M)
(Note: Concentration of NaOH at the highest conversion, X)
CA0 = Inlet concentration of reactant NaOH (M) (Concentration at
t=0)

3. In the 3-stage CSTR in series, all of equal volume and same operating
temperature, the Damnköhler (Da) number for a second order reaction in
a CSTR is defined as, Da = τavgkCA0. Calculate the the Damnköhler (Da)
number and discuss its correlation to the highest conversion achieved in
this experiment.

c) Plug flow reactor (PFR)

1. Calculate the value of the reaction rate constant, k and the rate of
reaction, –rA.

F0,avg æ X ö
Reaction rate constant, k = ç ÷ AND Rate of reaction, - rA = kC A
2

VPFRC A0 è 1- X ø

CA = Exit concentration of reactant NaOH (M)

(Note: Concentration of NaOH at the highest conversion, X)
CA0 = Inlet concentration of reactant NaOH (M) (Concentration at
t=0)
X = Extent of conversion (NOTE: Choose Highest Conversion X)
F0,avg = Average total inlet flow rate of solutions (mL/min)

5.0 TUTORIAL
1. Write the differences between 3 reactors: Single CSTR, 3-stages CSTR and
Tubular (PFR) reactor. Discuss the advantages and disadvantages for each
configuration.
2. Write a one-paragraph summary of any journal article that studies chemical
reaction in a multiple stages CSTR. The article must have been published within

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LABORATORY MANUAL (JAN 2018) REACTION ENGINEERING (CKB 20104)

the last 5 years. Explain on the PFR reactor used in the study and its significance
to the study done.

6.0 REFERENCES
1. Levenspiel O., “Chemical Reaction Engineering”, John Wiley (USA), 1972.
2. Fogler H.S., “Elements of Chemical Reaction Engineering, 3rd Ed.”, Prentice Hall
(USA), 1999.
3. Smith J.M., “Chemical Engineering Kinetics”, McGraw Hill (Singapore), 1981.
4. Astarita G., “Mass Transfer with Chemical Reaction”, Elsevier, 1967.
APPENDIX A
RESULTS FOR PREPARATION OF CALIBRATION CURVE

Concentratio
Conductivity
n of NaOH
(mS/cm)
(M)

0.0500 10.7
0.0375 9.7
0.0250 7.5
0.0125 5.6
0.0000 4.0

NOTE
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis).
2. Determine the slope of the curve.
3. Use the calibration curve to determine the concentration of the experimental product (M)
from the pre-determined conductivity found during the experiment.

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LABORATORY MANUAL (JAN 2018) REACTION ENGINEERING (CKB 20104)

TABLE FOR EXPERIMENT

Reactor type = PFR Reactor volume = 3L

Total flow Inlet Outlet

Flow rate rate of concentratio concentratio Conversio
Flow rate Residence Outlet
of solutions, Inlet n of NaOH, Conductivit n of NaOH, n,
Temperature of NaOH,
Et(Ac), time, τ (min) conductivit
Time (°C) FNAOH F 0 (mL/min)
(Self- CNaOH (M) y CNaOH (M) X (%)
(min) FET = FNAOH + FET calculate)
y (mS/cm) (from (from (Self-
(mL/min) (mS/cm) calculate)
(mL/min) (Self- calibration calibration
calculate) curve) curve)
Inlet Outlet
0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg = τavg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve
(Appendix B).
Inlet concentration of NaOH - Outlet concentration of NaOH
2. Formula to calculate conversion, X X= ´100%
Inlet concentration of NaOH
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LABORATORY MANUAL (JAN 2018) REACTION ENGINEERING (CKB 20104)

TABLE FOR EXPERIMENT

Reactor type = Single-stage CSTR Reactor volume = 4L

Total flow Inlet Outlet
Flow rate rate of concentratio concentratio Conversio
Flow rate Residence Outlet
of solutions, Inlet n of NaOH, Conductivit n of NaOH, n,
Temperature of NaOH,
Et(Ac), time, τ (min) conductivit
Time (°C) FNAOH F 0 (mL/min) (Self- CNaOH (M) y CNaOH (M) X (%)
(min) FET = FNAOH + FET calculate)
y (mS/cm) (from (from (Self-
(mL/min) (mS/cm) calculate)
(mL/min) (Self- calibration calibration
calculate) curve) curve)
Inlet Outlet
0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg = τavg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve
(Appendix B).
Inlet concentration of NaOH - Outlet concentration of NaOH
2. Formula to calculate conversion, X X= ´100%
Inlet concentration of NaOH

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LABORATORY MANUAL (JAN 2018) REACTION ENGINEERING (CKB 20104)

TABLE FOR EXPERIMENT

Reactor type = 3-stage CSTRs Reactor volume = 1L

Total flow Inlet Outlet

Flow rate rate of concentratio concentratio Conversio
Flow rate Residence Outlet
of solutions, Inlet n of NaOH, Conductivit n of NaOH, n,
Temperature of NaOH,
Et(Ac), time, τ (min) conductivit
Time (°C) FNAOH F0 (mL/min) (Self- CNaOH (M) y CNaOH (M) X (%)
(min) FET = FNAOH + FET calculate)
y (mS/cm) (from (from (Self-
(mL/min) (mS/cm) calculate)
(mL/min) (Self- calibration calibration
calculate) curve) curve)
Inlet Outlet
0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg = τavg =

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured conductivity value based on the calibration curve
(Appendix B).
Inlet concentration of NaOH - Outlet concentration of NaOH
2. Formula to calculate conversion, X X= ´100%
Inlet concentration of NaOH
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