EXPERIMENT 2: TUBULAR FLOW REACTOR

5.0 MATERIALS AND APPRATUS

5.1 MATERIAL
1) Ethyl Acetate
2) Sodium Hydroxide
3) Water
5.2 APPARATUS
1) Tubular reactor (R1)
i. Stainless steel coil
ii. Volume: approx. 0.4-L
2) Water jacket (B4)
i. Cylindrical vessel made of borosilicate glass
ii. Capacity: approx. 10-L
iii. 2x1.0 kW cartridge heater
iv. Cooling tubes
v. Stirrer: 50 2000 rpm with LCD display
a. Max. Torque 30 Ncm
b. 230VAC / 50-60 Hz / 75 W
c. Circulation pump (P3)
3) Feed tanks (B1, B2)
i. 20-L cylindrical vessels made of stainless steel
ii. Water de-ionizer fitted to tank B1

EXPERIMENT 2: TUBULAR FLOW REACTOR

4) Waste tank (B3)

i. 60-L rectangular tank made of stainless steel
5) Pre-heater (B5)
i. 3-L cylindrical vessel made of stainless steel
ii. Internal coils for each reactants
6) Feed pumps (P1, P2)
i. Centrifugal pumps
ii. Max delivery rate: 1 usgpm (3.78 LPM)
iii. Max delivery height: 25 psi IV. Power: 12V

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR Page 8

7) Instrumentations
Flow measurements (FI-01, FI-02)
Temperature measurements (TIC-01, TI-02)
Conductivity measurements (QI-01, QI-02)

EXPERIMENT 2: TUBULAR FLOW REACTOR

Valves and Instruments List

Valves list:
Tag
V1
V2
V3
V4
V5
V6
V7
V8
V9
V10
V11
V12
V13
V14
V15
V16
V17

Location
Drain valve for feed tank B1
Inlet valve for pump P1
De-ionized water supply to feed tank B1
Drain valve for feed tank B2
Inlet valve for pump P2
Valve for feed inlet to reactor from F1 01
Drain valve for F1 01
Valve for feed inlet to reactor from F1 02
Drain valve for F1 02
Drain valve for water jacket B4
Drain valve
By-pass valve for pump P3
Inlet flow for pre-heater B5
Sampling valve
Sampling valve
Drain valve
Cooling water outlet

Initial position
Close
Close
Close
Close
Close
Close
Close
Close
Close
Close
Close
Close
Close
Close
Close
Close
Close

Instruments list:
Tag
F1 01
F2 02
Q1 01
Q2 02
TIC 01
TI 02

Description
Liquid flow meter
Liquid flow meter
Conductivity
Conductivity
Temperature controller
Pre-heater temperature

Units
L/min
L/min
mS/cm
mS/cm
C
C

Range
0.0-3
0.0-3
0.0-200.0
0.0-200.0
0.0-100.0
0.0-100.0

Accuracy
2%
2%
1% FS
1% FS
0.5 C
0.5 C

EXPERIMENT 2: TUBULAR FLOW REACTOR

EXPERIMENT 2: TUBULAR FLOW REACTOR

6.0 METHODOLOGY

6.1 General Start-Up Procedures

1) All valves were initially closed except valves V16.
2) The following solution were prepared:
i) 20 liter of sodium hydroxide, NaOH (0.1 M)
ii) 20 liter of ethyl acetate, Et (Ac) (0.1 M)
3) The feed tank B1 was filled with the NaOH solution and feed tank B2 with the Et (Ac)
solution.
4) Valve, V17 was opened. V10 and V11 were opened until water jacket, B4 is fill on with 4 L of
water. V11 was closed and valve V10, V12 and V13 were opened.
5) Pump, P3 was opened and was allowed clean water to flow through Pre-heater B5 with clean
water by opening valve V10, V11, V12 and V13. The vent valve must be open.
6) The power for the control panel was turned on. Valves V2, V5, V6 and V8 were opened.
7) Both pumps P1 and P2 were switched on. P1 and P2 were adjusted to obtain flow of
approximately 0.30 L/min at both flow meters FI 01 and FI 02. Both flow rates must be the
same.
8) Both solutions were allowed to flow through the reactor R1 and overflow into the waste tank
B3.
9) Pump P3 was switched on to circulate the water through pre-heater B5. The stirrer motor was
switched on and the speed was set to about 200 rpm to ensure homogeneous water jacket
temperature. (Note: Pre-caution, the water level must be higher than the heater)
10) For experiment, the following additional steps were performed:
i) The heater was switched on.
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EXPERIMENT 2: TUBULAR FLOW REACTOR

ii) Valve V17 was opened to let the cooling water to flow through the cooling tubes. The
water supply valve was adjusted to obtain reasonable cooling water flow in order to minimize the
temperature overshoot at the TI 01 during heater cut-off.
iii) The temperature set point on TI 01 was set to the desired temperature.
11) The unit was ready for experiment.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR Page 11

6.2 General Shut-Down Procedures
1) Pumps P1, P2 and P3 were switched off. Valves V2 and V5 were closed.
2) The heater was switched off.
3) The cooling water kept circulating through the reactor while the stirrer motor was running to
allow the water jacket to cool down to room temperature.
4) The stirrer and the cooling water were off.
5) If the equipment is not going to be used for long period of time, all liquid were drained from
the unit by opening valves V1 to V17. The feed tanks were rinsed with clean water.
6) The power for the control panel was turned off.

6.3 Experiment Procedures

1) The general start-up procedures were performed.
2) Valves V6 and V8 were opened.
3) Both the NaOH and Et (Ac) solutions were allowed to enter the plug reactor R1 and empty
into the waste tank B3.
4) P1 and P2 were adjusted to give a constant flow rate of about 0.30 L/min at flow meters FI 01
and FI 02. Both flow rates must be the same. The flow rates were recorded.

EXPERIMENT 2: TUBULAR FLOW REACTOR

5) Start monitoring the inlet (QI 01) and outlet (QI 02) were started to monitor the conductivity
values until they do not change over time. This is to ensure that the reactor has reached steady
state.
6) Both inlet and outlet steady state conductivity values were recorded. The concentration of
NaOH exiting the reactor and extent of conversion were found out from the calibration curve.
7) Optional: Sampling valve V15 was opened and a 50 ml sample was collected. A back titration
procedure was carried out to manually determine the concentration of NaOH in the reactor and
extent of conversion.
8) The experiment (steps 4 to 7) was repeated for different residence times by reducing the feed
flow rates of NaOH and Et (Ac) to about 0.25, 0.20, 0.15, 0.10 and 0.05 l/min. Both flow rates
must be the same.
9) The general shutdown procedures were performed.

EXPERIMENT 2: TUBULAR FLOW REACTOR

7.0 DATA AND RESULTS

TABLE 1: Data obtain from the experiment
No

Volume ,
V TFR
(L)

1
2
3
4
5
6

4
4
4
4
4
4

Flow rate of
NaOH
(L/min)

Flow rate of
Et(Ac)
(L/min)

Total Flow Rate

of solutions ,
v

Residence
Time ,
(min)

0.30
0.25
0.20
0.15
0.10
0.05

(L/min)
0.60
0.50
0.40
0.30
0.20
0.10

6.6667
8.0000
10.0000
13.3333
20.0000
40.0000

0.30
0.25
0.2
0.15
0.1
0.05

TABLE 2: Data obtain from the experiment

No

Inlet

Outlet

Conversion,

Reaction Rate

Rate of

Conductivity

Conductivity

Constant, k

Reaction

(mS/cm)
10.7

(mS/cm)
8.2

(%)
21.74

(L/mol.min)
0.4167

(mol/L.min)
2.5521 x
103

10.3

7.8

26.09

0.4412

2.4101 x
103

10.2

7.7

27.17

0.3731

1.9990 x
103

10.0

7.3

31.52

0.3452

1.6188 x
3

10
5

9.9

7.3

31.52

0.2301

1.0791 x
103

9.4

6.6

39.13
8

0.1607

5.9542 x

EXPERIMENT 2: TUBULAR FLOW REACTOR

104

GRAPH 1: CONVERSION X VS RESIDENCE TIME

EXPERIMENT 2: TUBULAR FLOW REACTOR

12.0 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
5. Plug Flow Reactor. University of Michigan statement. Retrieved from
https://en.wikipedia.org/wiki/Plug_flow_reactor_model

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EXPERIMENT 2: TUBULAR FLOW REACTOR

13.0 APPENDIX

Tubular Flow Reactor (TFR)

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EXPERIMENT 2: TUBULAR FLOW REACTOR

Tubular Flow Diagram

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