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Please insert the LABORATORY REPORT SUBMISSION FORMas the front cover.
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2.
TABLE OF CONTENTS
The table of content and number of pages should be in following format.
Note: Each page should be numbered.
Content
Page Number
Summary
3.
1.0
2.0
3.0
Tutorial
4.0
References
5.0
Appendices
SUMMARY
Give the summary (not more than half page) on the overall experimental report. Give brief review on
the objectives of the experiment, main experimental results and discussions which are deemed
significant and finally conclusions obtained from the work.
4.
Example Table:
Table 1: X vs. Y
Samples
A
B
C
D
X (unit)
Y (unit)
Example Graph:
8.
TUTORIAL
Tutorial are the questions as given in the laboratory procedures. All questions must be answered as
required or else marks would not be rewarded for this section.
9.
REFERENCES
Details of published sources of material referred to or quoted in the text (including any lecture notes
and URL addresses of any websites used).
2.
Internet Website: Title of the information, year, source of data, [Online]. [Date Accessed].
Available from World Wide Web
Example:
BP Statistical Review of World Energy, 2007,BP (British Petroleum),[Online]. [Accessed
19th January, 2008]. Available from World Wide Web: http://bp.com/statisticalreview.
B.
The references should be arranged according to the author name in alphabetical order.
10.
APPENDICES
All the raw data and sample of calculations should be included here.
NOTE: STUDENTS ARE GIVEN OPTION TO HANDWRITE THE CALCULATIONS PART AS
TASKED IN THE REPORT. HOWEVER THE OTHER PART OF THE REPORT SHOULD BE
TYPED.
IMPORTANT NOTE:
1.
2.
Each member of the group is required to choose 1 part of each section to be executed individually.
Therefore any information copied from another group or taken directly from other sources such as
Internet without proper references will not be tolerated and the report will be marked as zero.
3.
Laboratory report should be submitted the following week (7 days) after the experimental is conducted.
4.
Any late submissions without agreement of the lecturer will result in 50% deductions of the overall
marks.
5.
Laboratory report should be submitted directly to the lecturer in charge for date verification.
APPENDIX
3
CHEMICAL PREPARATION
1. Ethyl acetate (CH3COOCH2CH3) (Liquid Phase)
Volume of ethyl acetate needed, V1 (L) from the original solution
mol
V2 (L)
L
V1 (L)
mol
10.10
L
M2
Where;
M2 = Desired molarity of Ethyl Acetate (mol/L) required in the experiment
V2 = Desired volume of Ethyl Acetate (mol/L) required in the experiment
2. Sodium Hydroxide (NaOH) (Solid Phase)
Weight of NaOH required for experiment, mNaoH
mol
g
MWNaOH
V2 (L)
L
mol
mNaOH (g) M 2
Where;
V1 (L)
mol
V2 (L)
L
mol
1.0
M2
Where;
M2 = Desired molarity of HCl (mol/L) required in the experiment
V2 = Desired volume of HCl (mol/L) required in the experiment
LABORATORY MANUAL
REACTION ENGINEERING
CKB 20104
JANUARY 2015
LIST OF EXPERIMENTS:
EXPERIMENT 1: BATCH REACTOR
Experiment A:The Batch Saponification of Ethyl Acetate
Experiment B:Effect of Temperature on the Batch Saponification Reaction
EXPERIMENT 2: CONTINUOUS STIRRED TANK REACTOR (CSTR)
Experiment A:Effect of RTD on the Reaction in a CSTR
Experiment B:The Effect of Temperature on the Reaction in a CSTR
EXPERIMENT 3: PLUG FLOW REACTOR (PFR)
Experiment A:Effect of Residence Time on the Reaction in a PFR
Experiment B: Effect of Temperature on the Reaction in a PFR
EXPERIMENT 4: REACTOR TEST RIG (RTR)
Experiment A: Reactor Comparison Test
EXPERIMENT 1
BATCH REACTOR
OBJECTIVES
To measure the rate constant of the reaction between ethyl acetate and sodium hydroxide under
batch condition.
To study the liquid phase reaction kinetics in a batch reactor.
To study the effect of temperature on the reaction in a batch reactor.
Keywords: Batch reactor; Kinetics; Saponification reaction; Activation energy
1.0
GENERAL DESCRIPTION
1.1
4. Condenser (W1)
Coil heat exchanger, area 0.3 m2
5. Instrumentation
Temperature measurement (TI-101)
Conductivity measurement (QI-401)
CH 3 COOC2 H 5 OH CH 3 COO C 2 H 5 OH
This type of reaction is called a saponification because of its importance in the manufacture of soap.
The reaction is relatively slow and the changing ester concentration can be followed quite easily by
analyzing samples from the reaction mixture every few minutes. The second order rate constant is
determined in two different ways:
a)
Rate
d ester
k ester OH
dt
Suppose that the concentrations of the ester and hydroxide are equal at the start of the experiment and
equal to CA0mol/dm3, and that at some time t later, both the ester and hydroxide concentration have
fallen to CA. Therefore we obtain
dCA
k ester OH kCA2
dt
t
dCA
1
1
C 2 k dt C C kt
C A0
0
A
A0
A
A plot of 1/CA against t should give a straight line with the gradient, k.
b)
Half-life method
1 C CA
1
1
k A0
kt
t
C
C
C
C
A A0
A0
From A
can be rearranged to give
Let t1/2 be the time taken for the concentration of ester to be halved,
C A C A0 / 2
, then
1
t1/2CA0
The time taken to halve the concentration of ester is inversely proportional to the initial concentration.
From plot of the ester concentration C Aagainst t, it is possible to determine t1 / 2 and hence the rate
constant.
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 tubings 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.
8.
Plastic gloves and eye shields must be worn when handling corrosive liquids, and heat resistant gloves when
adjusting steam valves.
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.
2.0
EXPERIMENTAL PROCEDURES
b)
c)
2. Pipette 200 mL of 0.1M ethyl acetate, Et(Ac) solution into a clean dry conical flask
3. Placed 200mL of 0.1M sodium hydroxide (NaOH) into 500 ml beaker.
4. Label 11 clean conical flasksfrom 1 to 11 and pipette 20 mLof 0.1M hydrochloric acid, HCl into
each of them (Flask 1 to 11).
5. Place the mechanical stirrer in the sodium hydroxide (NaOH) solution.
6. Turn on the stirrer and quickly pour all of the ethyl acetate, Et (Ac) from the conical flask into the
NaOH beaker, starting the stopwatch at roughly the mid-point of addition.
7. After5 minutes, withdraw by pipette 20 mL of the reacting mixture and pour into Flask 1, noting
the time at the mid-point of delivery.
8. Titrate the content of Flask 1 with 0.1M sodium hydroxide, NaOH using two or three drops of
phenolphthalein as indicator. The color of the indicator will change from colorless (acidic) to
pink (basic).
9. Stop the titration once the change of indicator color is observed. Determine the amount of NaOH
needed.
10. Withdraw further samples at 10 (Flask 2), 15 (Flask 3), 20 (Flask 4), 25 (Flask 5), 30 (Flask 6), 35
(Flask 7), 40 (Flask 8), 50 (Flask 9), 60 (Flask 10) and 70 (Flask 11) minutes. Repeat step 7 to 9.
11. Record the results in Appendix A.
3.0
Y mL
The number of moles of 0.1M NaOH used in the titration = Acid neutralized in titration
0.1(Y )
mol
1000
=
0.1(20)
mol
1000
We know the initial quantity of 0.1M acid=
The amount of acid neutralized by sample= Moles of NaOH present in the sample
10
0.1(20 Y )
mol
1000
=
Thus, NaOH concentration in 20 mL sample from the reactor=Ester concentration =
20 Y
0.1
mol / mL
1000
20
=
1. Plot a graph conversion, Xvs.reaction time and discuss it thoroughly.
2. Determine the rate constant, k using both methods and compare both values as explained
previously:
a. Integrated rate law method
1
1
kt
CA CA0
A plot of 1/CA against t should give a straight line with the gradient, k.
b. Half-life method
* In the half-life method, the initial concentrations (C A0 = 0.05 M) can be obtained
straight forward. From the graph (CA versus t) we can determined how long it takes for
that concentration to be halved (t1/2 = Reaction time when concentration = 0.025 M).
4.0
1
t1/2CA0
TUTORIAL
Discuss why vital to conduct certain chemical reactions in bench scale up and subsequently discuss
its disadvantages.
5.0
EXPERIMENTAL PROCEDURES
2.
3.
4.
Check that there is sufficient water in the thermostat T1 tank. Refill as necessary.
5.
Open cooling water valve V5 and let the cooling water flow through the condenser W1.
6.
Switch on the thermostat T1 and set the water temperature to the desired temperature.
7.
8.
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.
9.
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.
10.
11.
12.
At every 5-minute interval, open sampling valve V1 (at the bottom) and collect a 10 mL
sample. Carry out a conductivity measuring by using conductivity meter.
13.
Record your conductivity value and temperature value from TI-101 in the Appendix C.
14.
End the experiment when the conductivity values do not change significantly over time.
Switch off the stirrer M1. Drain the reactor R1 by opening valve V1.
15.
Refilled the reactor with fresh solutions of 3 L of 0.1 M ethyl acetate and 3 L of 0.1 M
sodium hydroxide.
16.
Repeat the experiment (steps 1-8) for different reactor temperature by setting the
thermostat temperature tothe desired temperature.
17.
12
3. Plot a graph Conversion, X vs time, t forthe different temperature and subsequently compare the
conversions for the different temperature. Discuss it thoroughly and include explanations on the
effect of temperature onto the reaction.
4. For a second order reaction, the rate law is shown to be:
rA
dCA
kCA2 AND
dt
Therefore
CA
dCA
CA0
CA2
k dt
t
1
1
kt
CA
CA0
where CA0 is the initial concentration of reactant NaOH in the reactor(0.05 M).
5. For each temperature value, plot the graph of 1/C A vs time, t and evaluate the slope and y-axis
intercept.
6. Determine the rate constant, k from the slope value for different temperature values. Examine
the change in the rate constant.
7. Plot a graph of ln k vs 1/T and evaluate the slope and y-axis intercept.
Ea
RT
Ea 1
ln A
R T
(R = 8.314 J/mol.K)
8. 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. Describe an example of industrial applications other than saponification that utilized batch
reactors in its process.
2. Discuss the advantages and disadvantages of using batch reactors in chemical reaction.
9.0
REFERENCES
1. Atkins, P.W. Physical Chemistry (various ed.)
2. Smith, J.M. Chemical Engineering Kinetics (3rd ed.), McGraw-Hill, 1981
3. Frost, A.A. & Pearson, R.G. Kinetics and Mechanics (2nd ed.), Wiley, 1961
4. Fogler, H.S., Elements of Chemical Reaction Engineering, 3rd edition, Prentice Hall Int. Series,
N.J. (USA), 1997.
13
5. Levenspiel, O., Chemical Reaction Engineering, 3rd edition, John Wiley and Sons, 1999
6. Astarita G., Mass Transfer with Chemical Reaction, Elsevier, 1967.
7. Model SOLTEC BP 141 Operating Manual, Solution Engineering Bhd, KL.
APPENDIX A
Table forExperiment A: The Batch Saponification of Ethyl Acetate
Time
(min)
Flask
Number
5
10
15
20
25
30
35
40
50
60
70
Concentration of
NaOH,
CNaOH (M)
Amount of
NaOH titred
(mL)
Conversion,
X (%)
(Self calculate)
1
2
3
4
5
6
7
8
9
10
11
NOTE:
1. Formula to calculate conversion, X
APPENDIX B
Experiment B: Effect of Temperature on the Batch Saponification Reaction
TABLE OF CALIBRATION CURVE
14
Solution Mixtures
Conversion
Concentration
of NaOH (M)
Conductivity
(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
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.
APPENDIX C
Table for Experiment B: Effect of Temperature on the Batch Saponification Reaction
Volume of NaOH
3L
Volume of Et(Ac)
3L
15
0.05 M
0.05 M
Temperature
_____C
Time
(min)
Temperature
(C)
Conductivity
(mS/cm)
Concentration of NaOH,
CNaOH (M)
(From calibration curve)
Conversion,
X (%)
(Self calculation)
0
5
10
15
20
25
30
35
40
45
50
55
60
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).
2. Formula to calculate conversion, X
Continue:
Table for Experiment B: Effect of Temperature on the Batch Saponification Reaction
Volume of NaOH
3L
Volume of Et(Ac)
3L
16
0.05 M
0.05 M
Temperature
_____ C
Time
(min)
Temperature
(C)
Conductivity
(mS/cm)
Concentration of NaOH,
CNaOH (M)
(From calibration curve)
Conversion,
X (%)
(Self calculation)
0
5
10
15
20
25
30
35
40
45
50
55
60
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).
2. Formula to calculate conversion, X
END EXPERIMENT 1
EXPERIMENT 2
CONTINUOUS STIRRED TANK REACTOR (CSTR)
OBJECTIVES
To study liquid phase reaction kinetics in a CSTR
To determine the conversion at different residence time.
17
GENERAL DESCRIPTION
1.1
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
5.Condenser (W1)
Safety Considerations
1. The unit must be operated under the supervision of an authorized staff who 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.
19
V1
V6
B1
Cooling
Water
B2
W1
Cooling
Water
V13
HS
1
Q1
401
TI
101
V2
V7
FI
301
FI
302
V5
V10
V3
R1
V8
V3
V11
V4
P1
V9
P2
M
HS
2
HS
3
V12
B3
Figure 2: Continuous Stirred Tank Reactor Unit
12
T1
2.0
OPERATING PROCEDURES
2.1
b)
Carefully pour the NaOH solution into vessel B1 and the Et(Ac) solution
into vessel B2.
c)
2.2
13
3.2
3.0
EXPERIMENTAL PROCEDURES
OBJECTIVES:
PROCEDURES:
1.
14
4.0
1.
Residence Time,
VCSTR
F0
A0
CA
avgC
2
A
avg
CA
CA0
5.0
TUTORIAL
1. Discuss the advantages and disadvantages of using CSTR reactors in chemical reaction.
2. Describe an example of industrial applications that utilized CSTR reactors in its process.
15
OBJECTIVES:
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 cooling water valve V13 and let the cooling water flow through the condenser W1.
4. Switch on the thermostat T1 and set the water temperature to the desired temperature.
5. Switch ON both pumps P1 and P2 simultaneously.
6. Open and adjust the valves V5(Monitor at FI-301)and V10 (Monitor at FI-302)to give a
flow rate of about 200 mL/min. Both must be adjusted to equal flow rate.
7. Let the reactor fill up with both solutions until it is just about to 1/2 full.
8. Switch ON the stirrer M1.
9. Start monitoring the conductivity value at QI-401.
10. Start the timer and record the conductivity value at QI-401, temperature value at TI-101
and both flow rates (FI-301 and FI-302) when it has reached steady state (Conductivity
value begin to steadily decline with time).
11. Record the conductivity, temperature, both flow rate values for every 5 minutes until the
conductivity does not change over time. This is to ensure that the reactor has reached
steady state.
12. End the experiment when the conductivity values do not change significantly over time.
13. Repeat the experiment (steps 6 to 11) for different reactor temperatures by setting the
thermostat temperature to the desired temperature. Make sure that the flow rates of both
solutions are maintained at the original flow rate.
14. Perform the general shut-down procedures.
16
A0
CA
avgC
2
A
CA
CA0
6. Plot a graph of ln k vs 1/T and evaluate the slope and y-axis intercept.
Ea
RT
Ea 1
ln A
R T
(R = 8.314 J/mol.K)
6. Calculate the saponification reactions activation energy, E a and frequency factor, A from
the slope and intercept values using the Arrhenius equation.
8.0
TUTORIAL
1.
2.
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.
17
Solution Mixtures
Conversion
Concentration
of NaOH (M)
Conductivity
(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
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.
18
APPENDIX B
RESULTS FOR EXPERIMENTS
Reactor volume
Concentration of NaOH in feed vessel
Concentration of Et(Ac) in feed vessel
Time
Flow rate of
Temperature
NaOH, FNAOH
(C)
(mL/min)
=
=
=
10 L
_____ M
_____ M
Flow rate of
Et(Ac), FEt
(mL/min)
Flowrate
=
Temperature =
Total flow rate
of solutions,
F0 (mL/min),
= FNAOH + FEt
(Selfcalculation)
Residence
time, (min)
(Self
calculation)
_____ mL/min
_____ oC
Conductivity
(mS/cm)
Concentration of
NaOH,
CNaOH (M)
(From calibration
curve)
Conversion,
X (%)
(Self
calculation)
0
5
10
15
20
25
30
35
40
45
50
55
60
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).
2. Formula to calculate conversion, X
=
=
=
10 L
_____ M
_____ M
Flow rate of
Et(Ac), FEt
(mL/min)
Flowrate
=
Temperature =
Total flow rate
of solutions,
F0 (mL/min),
= FNAOH + FEt
(Selfcalculation)
Residence
time, (min)
(Self
calculation)
_____ mL/min
_____ oC
Conductivity
(mS/cm)
Concentration of
NaOH,
CNaOH (M)
(From calibration
curve)
Conversion,
X (%)
(Self
calculation)
0
5
10
15
20
25
30
35
40
45
50
55
60
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).
2. Formula to calculate conversion, X
20
GENERAL DESCRIPTION
1.1
Pipe length 15 m
Centrifugal pumps
EXPERIMENT 3
4. Pre-heater (W1/W2)
Coil heat exchanger, area 0.06 m2
20
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.
21
22
V1
B1
P1
M
HS
1
2.0
OPERATING PROCEDURES
2.1
2.3
13
3.0
EXPERIMENTAL PROCEDURES
OBJECTIVE
PROCEDURES:
14
4.0
1.
Residence Time,
VPFR
F0
F0,avg
X
2
AND Rate of reaction, - rA kCA
VPFRCA0 1 X
F0, avg =
CA
5.0
CA0
TUTORIAL
1.
2.
OBJECTIVE:
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 temperaturesfor 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.
16
7.1
F0,avg
VPFRCA0 1 X
F0
CA0
6. Plot a graph of ln k vs 1/T and evaluate the slope and y-axis intercept.
Ea
RT
Ea 1
ln A
R T
(R = 8.314 J/mol.K)
7. Calculate the saponification reactions activation energy, E a and frequency factor, A from
the slope and intercept values using the Arrhenius equation.
8.0
TUTORIAL
1.
2.
9.0
REFERENCES
1. Levenspiel O., Chemical Reaction Engineering, John Wiley (USA), 1972.
17
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
Solution Mixtures
Conversion
Concentration
of NaOH (M)
Conductivity
(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
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.
18
Time
(min)
Temperature
(C)
=
=
=
1.5 L
_____ M
_____ M
Total flow
rate of
solutions,
F0 (mL/min)
= FNAOH + FET
Flowrate
=
Temperature =
Residence
time, (min)
(Selfcalculate)
(Self-calculate)
Inlet
Inlet
conductivity
(mS/cm)
_____ mL/min
_____ oC
Inlet
concentration
of NaOH,
CNaOH (M)
(from calibration
curve)
Outlet
Conversion,
concentration
Outlet
X (%)
of
NaOH,
Conductivity
(SelfCNaOH (M)
(mS/cm)
calculate)
(from calibration
curve)
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).
2. Formula to calculate conversion, X
Time
(min)
Temperature
(C)
=
=
=
1.5 L
_____ M
_____ M
Total flow
rate of
solutions,
F0 (mL/min)
= FNAOH + FET
Flowrate
=
Temperature =
Residence
time, (min)
(Selfcalculate)
(Self-calculate)
Inlet
Inlet
conductivity
(mS/cm)
_____ mL/min
_____ oC
Inlet
concentration
of NaOH,
CNaOH (M)
(from calibration
curve)
Outlet
Conversion,
concentration
Outlet
X (%)
of
NaOH,
Conductivity
(SelfCNaOH (M)
(mS/cm)
calculate)
(from calibration
curve)
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).
X
2. Formula to calculate conversion, X
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
6. Pumps (P1/P2)
Centrifugal pumps
7. Pre-heater (W1/W2)
20
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.
21
22
V22
V23
M2
V24
V25
HS
4
QI
404
M3
M
HS
5
TI
104
M4
HB1
HS
6
HB2
QI
403
R2
M1
HS
3
V1
V2
W1
V17
R4
V18
V11
QI
401
R3
QI
402
SR1
W2
V16
TI
102
T1
TI
103
V12
V13
R1
TI
101
V14
Injection
V15
B1
FI
301
B2
FI
302
FI
303
V19
V8
P1
V3
P2
V4
HS
1
HS
2
V9
V20
V21
V10
V27
V5
V6
V7
B3
V26
Process Water
2.0
OPERATING PROCEDURES
2.1
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)
b)
Read the outlet conductivity value from QI-404 and temperature value from TI-104.
b)
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)
b)
c)
Read the outlet conductivity value from QI-403 and temperature value from TI-103.
37
2.3
3.0
3.
Open valves V3 to V21 and valve V26 to drain all liquid from the unit.
4.
EXPERIMENTAL PROCEDURES
OBJECTIVE:
To carry out a saponification reaction between NaOH and Et(Ac) using different
types of reactors.
3.2
1.
PROCEDURES:
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.
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.
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.
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.
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.
39
4.0
1.
The reactors residence time is defined as the reactor volume divided by the average total feed
flow rates.
Residence Time,
VCSTR
F
0
Calculate the value of the reaction rate constant, k and the rate of reaction, rA.
A0
CA
avgC
2
A
avg
CA
CA0
The reactors residence time is defined as the reactor volume divided by the average total feed
flow rates.
Residence Time,
VCSTR
F
0
2.
Calculate the value of the reaction rate constant, k and the rate of reaction, rA.
A0
CA
avgC
2
A
avg
CA
CA0
3. In the 3-stage CSTR in series, all of equal volume and same operating
temperature, the Damnkhler (Da) number for a second order reaction in a
CSTR is defined as, Da = avgkCA0.Calculate the the Damnkhler (Da) number
and discuss its correlation to the highest conversion achieved in this experiment.
F0,avg
X
2
AND Rate of reaction, - rA kCA
VPFRCA0 1 X
5.0
CA0
F0,avg
TUTORIAL
1.
Write the differences between 3 reactors: Single CSTR, 3-stages CSTR and
Tubular(PFR) reactor.
2.
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.
41
APPENDIX A
RESULTS FOR PREPARATION OF CALIBRATION CURVE
Solution Mixtures
Conversion
Concentration
of NaOH (M)
Conductivity
(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
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.
42
Time
(min)
Temperature
(C)
PFR
Reactor volume
3L
_____ M
_____ M
Total flow
rate of
solutions,
F0 (mL/min)
= FNAOH + FET
Residence
time, (min)
(Selfcalculate)
(Self-calculate)
Inlet
Inlet
conductivity
(mS/cm)
Inlet
concentration
of NaOH,
CNaOH (M)
(from calibration
curve)
Outlet
Conversion,
concentration
Outlet
X (%)
of
NaOH,
Conductivity
(SelfCNaOH (M)
(mS/cm)
calculate)
(from calibration
curve)
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).
X
2. Formula to calculate conversion, X
Time
(min)
Temperature
(C)
Single-stage CSTR
Reactor volume
4L
_____ M
_____ M
Total flow
rate of
solutions,
F0 (mL/min)
= FNAOH + FET
Residence
time, (min)
(Selfcalculate)
(Self-calculate)
Inlet
Inlet
conductivity
(mS/cm)
Inlet
concentration
of NaOH,
CNaOH (M)
(from calibration
curve)
Outlet
concentration Conversion,
Outlet
X (%)
of NaOH,
Conductivity
(SelfCNaOH (M)
(mS/cm)
calculate)
(from calibration
curve)
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).
X
2. Formula to calculate conversion, X
Time
(min)
Temperature
(C)
3-stage CSTRs
Reactor volume
1L
_____ M
_____ M
Total flow
rate of
solutions,
F0 (mL/min)
= FNAOH + FET
Residence
time, (min)
(Selfcalculate)
(Self-calculate)
Inlet
Inlet
conductivity
(mS/cm)
Inlet
concentration
of NaOH,
CNaOH (M)
(from calibration
curve)
Outlet
Conversion,
concentration
Outlet
X (%)
of
NaOH,
Conductivity
(SelfC
(M)
NaOH
(mS/cm)
calculate)
(from calibration
curve)
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).
X
2. Formula to calculate conversion, X