LABORATORY MANUAL (JAN 2017) REACTION ENGINEERING (CKB 20104)

EXPERIMENT 3

PLUG FLOW REACTOR (PFR)

OBJECTIVES
To determine the effect of residence time on the conversion in a PFR.
To determine the effect of temperature on the conversion in a PFR.

Keywords: PFR, pulse input, step input, residence time

1.0 GENERAL DESCRIPTION

1.1 Description and Assembly

Before operating the unit and running experiments, students must familiarize
themselves with the units components. Please refer to Figure 1 to understand the
process. All glass components of the QVF Plug Flow Reactor unit are made of
borosilicate 3.3 glass with PTFE gaskets.

1. Plug flow reactor (SR1)

Jacketed pipe with approximate capacity of 1.5 L

Pipe length 15 m

2. Feed vessels (B1/B2)

60 L PE rectangular vessels with all necessary connections

2. Dosing vessels (HB1/HB2)

1 L cylindrical vessels with overflow port and bottom port

3. Pumps (P1/P2)

Centrifugal pumps

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

4. Pre-heater (W1/W2)

Coil heat exchanger, area 0.06 m2

Max heating media pressure of 0.5 bar

5. Receiving vessel (B3)

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LABORATORY MANUAL (JAN 2017) REACTION ENGINEERING (CKB 20104)

100 L rectangular tank

6. Instrumentations

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

Temperature measurements (TI-101, TI-102)

Conductivity measurements (QI-401, QI-402)

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 vapors.

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 2017) REACTION ENGINEERING (CKB 20104)

Vent

QI TI
402 102
V10
HB1 HB2

SR1

V1 V2 T1

W1 W2 TI QI
101 401

Injection

B1 B2 FI
301
FI
302
FI
303
B3
V11

V3 V4 V7 V8 V9
P1 P2
M M
V5 V6
HS HS Process Water
1 2
V12

Figure 3: Plug Flow Reactor Unit

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LABORATORY MANUAL (JAN 2017) REACTION ENGINEERING (CKB 20104)

2.0 OPERATING PROCEDURES

2.1 General Start-Up Procedures for Experiments A & B

1. 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)

2. Ensure that all valves are initially closed.

3. Fill the feed vessel B1 with the NaOH and feed vessel B2 with the Et(Ac) solution.

4. Turn on the power for the control panel.

5. Open valves V1 and V2.

6. Switch on pumps P1 and P2. Observe the flow of NaOH and Et(Ac) solutions into
the dosing vessels HB1 and HB2 towards valves V8 and V7.

7. Make sure that the pipelines before valves V7 and V8 are filled with solutions.
Bleed any trapped air in the pipelines by using valves V7 and V8.

8. Allow both the solutions to overflow in the dosing vessels HB1 and HB2 into the
feed vessels B1 and B2.

9. The unit is now ready for experiment.

2.3 General Shut-Down Procedures

1. Switch off both pumps P1 and P2.

2. Switch off the thermostat T1.

3. Close the process water valve V12.

4. Open valves V3, V4, V5, V6, V7, V8 and V11 to drain all liquid from the unit.

5. Turn off the power for the control panel.

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LABORATORY MANUAL (JAN 2017) REACTION ENGINEERING (CKB 20104)

EXPERIMENT A: Effect of Residence Time on the Reaction in a PFR

3.0 EXPERIMENTAL PROCEDURES

3.1 OBJECTIVE

To carry out a saponification reaction between NaOH and Et(Ac) in a PFR.

To determine the reaction rate constant.
To determine the effect of residence time on the conversion in a PFR.

3.2 PROCEDURES:
1. Perform the general start-up procedures
2. Open valves V7 and V8 and adjust valves V7 (Monitor at FI-301) and V8 (Monitor
at FI-302) to give a flow rate of about 400 mL/min. Make sure that both flow rates
are the same.
3. Allow both the NaOH and Et(Ac) solutions to enter the plug flow reactor SR1 and
empty into the receiving vessel B3.
4. Adjust valves V7 and V8 to give the desired flow rate. Make sure that both flow
rates are the same.
5. Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-402).
6. Start the timer and record both conductivity values (QI-401 and QI-402) and flow
rates (FI-301 and FI-302) when it has reached steady state (Conductivity value
begin to steadily decline with time).
7. Record the inlet and outlet conductivity values and both flow rates for every 5
minutes until the conductivity do not change over time. This is to ensure that the
reactor has reached steady state.
8. Repeat the experiment (steps 4 to 5) for different residence times by adjusting the
flow rates to the desired values. Make sure that both flow rates are the same.

4.0 ANALYSIS AND DISCUSSION:

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

2. Find the concentration of NaOH in 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, t for the different flow rate. Discuss the
graph.

4. The reactors residence time is defined as the reactor volume divided by the average total
feed flow rates.
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LABORATORY MANUAL (JAN 2017) REACTION ENGINEERING (CKB 20104)

VPFR
Residence Time, t =
F0

Subsequently calculate the average residence time, avg (NOTE: 1 FLOW RATE
PARAMETER GIVES 1 AVERAGE RESIDENCE TIME).

5. Compare the highest conversion, X for the different average residence time, avg (NOTE:
1 FLOW RATE PARAMETER GIVES 1 AVERAGE RESIDENCE TIME). Compare
the highest conversion, X at the different average residence time, avg. Discuss
thoroughly and explain how residence time can influence the rate of reaction.

6. For the different average reactor residence times, avg (NOTE: 1 FLOW RATE GIVES 1
AVERAGE RESIDENCE TIME), calculate the value of the reaction rate constant, k and
the rate of reaction, rA.

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

VPFRC A0 1- X

F0, avg = Average total inlet flow rate of solutions (mL/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)
X = Conversion (NOTE: Choose Highest Conversion X)

5.0 TUTORIAL

1. Discuss the advantages and disadvantages of using PFR reactors in chemical reaction.
Describe an example of industrial applications that utilized PFR reactors in its process.

2. Write a one-paragraph summary of any journal article that studies chemical reaction in a
PFR. The article must have been published within the last 5 years. Explain on the PFR
reactor used in the study and its significance to the study done.

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LABORATORY MANUAL (JAN 2017) REACTION ENGINEERING (CKB 20104)

EXPERIMENT B Effect of Temperature on the Reaction in a PFR

6.1 OBJECTIVE:

To determine the effect of temperature on the conversion in a PFR.

6.2 PROCEDURES:

1. Perform the general start-up procedures.

2. Check that there is sufficient water in the thermostat T1 tank. Refill as necessary.

3. Open the process water valve V12.

4. Switch on the thermostat T1 and set the water to the desired temperature.

5. Open valves V7 and V8 and adjust valves V7 (Monitor at FI-301) and V8

(Monitor at FI-302) to give a flow rate of about 400 mL/min. Make sure that both
flow rates are the same.

6. Allow both the NaOH and Et(Ac) solutions to enter the plug flow reactor SR1 and
empty into the receiving vessel B3.

7. Adjust valves V7 and V8 to give a flow rate of about 100 mL/min. Make sure that
both flow rates are the same.

8. Start monitoring the conductivity value at inlet (QI-401) and outlet (QI-402).

9. Start the timer and record both conductivity values (QI-401 and QI-402) flow rates
(FI-301 and FI-302), and temperatures ((TI-101 and TI-102) when it has reached
steady state (Conductivity value begin to steadily decline with time).

10. Record the conductivity, flow rates, and temperatures for every 5 minutes until they
do not change over time. This is to ensure that the reactor has reached steady state.

11. Repeat the experiment (steps 5 onwards) for different reactor temperatures by
increasing the thermostat temperature to the desired temperature. Make sure that the
flow rates of both solutions are maintained at 100 mL/min.

7.0 ANALYSIS AND DISCUSSION

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

2. Find the concentration of NaOH in 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, t for the 2 different temperatures.

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LABORATORY MANUAL (JAN 2017) REACTION ENGINEERING (CKB 20104)

4. Compare the highest conversion, X at the different temperature. Discuss it thoroughly and
explain how temperature can influence the rate of reaction, rA.

5. For different reactor temperature, calculate the value of the reaction rate constant, k.

F0,avg X
Reaction rate constant, k =
VPFRC A0 1- X

F0 = Average total inlet flow rate of solutions (mL/min)

CA0 = Inlet concentration of reactant NaOH (M) (Concentration at t=0)
X = Conversion (NOTE: Choose Highest Conversion X)

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

-Ea
From Arrhenius equation, k(T ) = Aexp
RT
(R = 8.314 J/mol.K)
-Ea 1
In linear form ln k = + ln A
R T

7. Calculate the saponification reactions activation energy, Ea and frequency factor, A from
the slope and intercept values using the Arrhenius equation.

8.0 TUTORIAL

1. Discuss the advantages and disadvantages of using PFR reactors in chemical reaction.
Describe an example of industrial applications that utilized PFR reactors in its process.

2. Write a one-paragraph summary of any journal article that studies chemical reaction in a
PFR. The article must have been published within the last 5 years. Explain on the PFR
reactor used in the study and its significance to the study done.

9.0 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

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LABORATORY MANUAL (JAN 2017) REACTION ENGINEERING (CKB 20104)

APPENDIX A
RESULTS FOR PREPARATION OF CALIBRATION CURVE

Concentration Conductivity
of NaOH (M) (mS/cm)

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 2017) REACTION ENGINEERING (CKB 20104)

RESULTS FOR EXPERIMENTS

Reactor volume = 1.5 L Flowrate = _____ mL/min

Temperature = _____ oC

Total flow Inlet Outlet

Flow rate Flow rate rate of Residence concentration concentration Conversion,
Inlet Outlet
Temperature of NaOH, of Et(Ac), solutions, time, (min) conductivity of NaOH, Conductivity of NaOH, X (%)
Time (C) FNAOH FET F0 (mL/min) (Self- (Self-
(mS/cm) CNaOH (M) (mS/cm) CNaOH (M)
(min) (mL/min) (mL/min) = FNAOH + FET calculate) (from calibration calculate)
(from calibration
(Self-calculate) curve) curve)
Inlet Outlet
0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg = avg =

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 2017) REACTION ENGINEERING (CKB 20104)

RESULTS FOR EXPERIMENTS

Reactor volume = 1.5 L Flowrate = _____ mL/min

Temperature = _____ oC

Total flow Inlet Outlet

Flow rate Flow rate rate of Residence concentration concentration Conversion,
Inlet Outlet
Temperature of NaOH, of Et(Ac), solutions, time, (min) conductivity of NaOH, Conductivity of NaOH, X (%)
Time (C) FNAOH FET F0 (mL/min) (Self- (Self-
(mS/cm) CNaOH (M) (mS/cm) CNaOH (M)
(min) (mL/min) (mL/min) = FNAOH + FET calculate) (from calibration calculate)
(from calibration
(Self-calculate) curve) curve)
Inlet Outlet
0
5
10
15
20
25
30
35
40
45
50
55
60
F0,avg = avg =

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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