Академический Документы
Профессиональный Документы
Культура Документы
Each experimental report should contain the following items in accordance to the numbering as
listed:
1. COVER PAGE
Please insert the LABORATORY REPORT SUBMISSION FORM as the front cover.
DOWNLOAD FROM E-LEARNING.
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
1.0 Results and Discussion
2.0 Conclusions and Recommendations
3.0 Tutorial
4.0 References
5.0 Appendices
3. 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.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
Example Table:
Table 1: X vs. Y
Samples X (unit) Y (unit)
A
B
C
D
Example Graph:
2.0
1.8
1.6
1.4
Parameter Y (unit)
1.2
1.0
0.8
y = -0.7886x + 1.7986
0.6
0.4
0.2
0.0
0.0 0.5 1.0 1.5
Parameter X (unit)
d. Based on the experimental results, discuss on your findings and relate to your theory
and objective of experiment
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).
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
REFERENCES SHOULD BE IN COMPLETE FORM AS GIVEN BELOW OR ELSE MARKS
WILL BE DEDUCTED FOR EACH ERROR.
A. The references should be in following format:
1. Books/Journals: Authors (editor), title, publisher, year, chapter or page number
Example:
Smith J.M. and Van Hess H.C., Introduction to Chemical Engineering
Thermodynamics, McGraw-Hill, New York, 2001, p229
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. Laboratory reports are meant to be group tasks.
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 directly to the lecturer in charge for date verification.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
APPENDIX
CHEMICAL PREPARATION
æ mol ö æ g ö
mNaOH (g) = M 2 ç ÷ ´ MWNaOH ç ÷ ´V2 (L)
è L ø è mol ø
Where;
M2 = Desired molarity of NaOH (mol/L) required in the experiment
V2 = Desired volume of NaOH (mol/L) required in the experiment
Molecular weight of NaOH, MW NaOH = 40.0 g/mol
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
LABORATORY MANUAL
REACTION ENGINEERING
CKB 20104
SEPTEMBER 2015
LIST OF EXPERIMENTS:
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
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.
Before operating the unit and running experiments, you must familiarize yourself with
the unit’s components. Please refer to Figure 2 to understand the process. All glass
components of the QVF Batch Reactor unit are made of borosilicate glass with PTFE
gaskets.
1. Reactor (R1)
2. Agitator (A1)
4. Condenser (W1)
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
Coil heat exchanger, area 0.3 m2
5. Instrumentation
Chemical engineering processes can be broadly divided into two types: batch processes and
continuous processes. In a batch process, input materials are placed in a reactor and product is
withdrawn some time later. This is typical of what is normally done in chemistry laboratories. You
will be studying for batch conditions the reaction between an ester (ethyl acetate) and sodium
hydroxide:
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:
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
a) Integrated rate law method
Assuming the reaction to be a simple, irreversible, second order process, then the rate law
for a batch process may be written
d [ ester ]
= k [ ester ] [OH ]
-
Rate = -
dt
Suppose that the concentrations of the ester and hydroxide are equal at the start of the
experiment and equal to CA0 mol/dm3, and that at some time t later, both the ester and
hydroxide concentration have fallen to CA. Therefore, we obtain
dCA
- = k [ ester ] éëOH - ùû = kCA2
dt
Separating the variables and integrating with appropriate boundary conditions,
CA t
dC A
ò = k ò dt Þ
1 1
- = kt
C A0 C A2 0 C A C A0
A plot of 1/CA against t should give a straight line with the gradient, k.
b) Half-life method
1 1 1 æ CA0 - CA ö
From - = kt can be rearranged to give k = ç ÷
CA CA 0 t è CACA0 ø
Let t1/2 be the time taken for the concentration of ester to be halved, C A C A0 / 2 , then
1
k=
t1/2CA0
The time taken to halve the concentration of ester is inversely proportional to the initial
concentration. From plot of the ester concentration CA against t, it is possible to determine
t1 / 2 and hence the rate constant.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
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 tubing’s 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. Wipe off any spillage on the ground or working bench.
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.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
2. Pipette 200 mL of 0.1M ethyl acetate, Et(Ac) solution into a clean dry conical flask
4. Label 11 clean conical flasks from 1 to 11 and pipette 20 mL of 0.1M hydrochloric acid,
HCl into each of them (Flask 1 to 11).
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. After 5 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.
The number of moles of 0.1M NaOH used in the titration = Acid neutralized in titration
0.1(Y )
mol
= 1000
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
0.1(20)
We know the initial quantity of 0.1M acid = mol
1000
The amount of acid neutralized by sample = Moles of NaOH present in the sample
0.1(20 -Y )
mol
= 1000
0.1 ( 20 -Y )
´ mol / mL
= 1000 20
2. Determine the rate constant, k using both methods and compare both values as
explained previously:
1 1
- = kt
C A C A0
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 (CA0) 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 = 1/2
CA0).
1
k=
t1/2CA0
4.0 TUTORIAL
1. Discuss why it is vital to conduct certain chemical reactions in bench scale up and
subsequently discuss its disadvantages.
2. Write a one-paragraph summary of any journal article that studies chemical reaction in
a batch reactor. The article must have been published within the last 5 years. Explain
on the batch reactor used in the study and its significance to the study done.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
Experiment B: Effect of Temperature on the Batch Saponification Reaction
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 Conversion, X vs time, t for the 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.
dC A dC A
ò = -k ò dt
CA t
-rA = - = kC A2 AND
dt C A0
C A2 0
1 1
Therefore = 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/CA’ 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.
æ -Ea ö
From Arrhenius equation, k(T ) = A exp ç ÷
è RT ø
(R = 8.314 J/mol.K)
-Ea æ 1 ö
In linear form ln k = ç ÷ + ln A
R èT ø
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
8.0 TUTORIAL
1. Describe an example of industrial applications other than saponification that utilized
batch reactors in its process. Discuss the advantages and disadvantages of using batch
reactors in chemical reaction.
2. Write a one-paragraph summary of any journal article that studies chemical reaction in
a batch reactor. The article must have been published within the last 5 years. Explain
on the batch reactor used in the study and its significance to the study done.
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.
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 for Experiment A: The Batch Saponification of Ethyl Acetate
Concentration of
Amount of NaOH, Conversion,
Time Flask
NaOH titred CNaOH (M) X (%)
(min) Number
(mL) (From equation (Self calculate)
above)
5 1
10 2
15 3
20 4
25 5
30 6
35 7
40 8
50 9
60 10
70 11
NOTE:
1. Formula to calculate conversion, X
𝐶𝑁𝑎𝑂𝐻(𝑡=0)− 𝐶𝑁𝑎𝑂𝐻(𝑡)
𝑋= × 100%
𝐶𝑁𝑎𝑂𝐻(𝑡=0)
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
APPENDIX B
Experiment B: Effect of Temperature on the Batch Saponification Reaction
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 2019) REACTION ENGINEERING (CKB 20104)
APPENDIX C
Table for Experiment B: Effect of Temperature on the Batch Saponification
Reaction
Volume of NaOH = 3L
Volume of Et(Ac) = 3L
Temperature = _____ C
Concentration of Conversion,
Time Temperature Conductivity NaOH, CNaOH (M) X (%)
(min) (°C) (mS/cm) (From calibration (Self
curve) 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
𝐶𝑁𝑎𝑂𝐻(𝑡=0)− 𝐶𝑁𝑎𝑂𝐻(𝑡)
𝑋= × 100%
𝐶𝑁𝑎𝑂𝐻(𝑡=0)
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
Continue:
Volume of NaOH = 3L
Volume of Et(Ac) = 3L
Temperature = _____ C
Concentration of Conversion,
Temperatur
Time Conductivity NaOH, CNaOH (M) X (%)
e
(min) (mS/cm) (From calibration (Self
(°C)
curve) 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
𝐶𝑁𝑎𝑂𝐻(𝑡=0)− 𝐶𝑁𝑎𝑂𝐻(𝑡)
𝑋= × 100%
𝐶𝑁𝑎𝑂𝐻(𝑡=0)
END EXPERIMENT 1
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
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.
To study the effect of temperature on the reaction in CSTR.
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
5. Condenser (W1)
Coil heat exchanger, area 0.2 m2
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
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)
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
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
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
b) Carefully pour the NaOH solution into vessel B1 and the Et(Ac) solution
into vessel B2.
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.
5. Open valves V4, V9 and V12 to drain any liquid from the unit.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
3.1 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.
To determine the reaction rate constant.
3.2 PROCEDURES:
1. Perform the general start-up procedures.
2. Switch ON both pumps P1 and P2 simultaneously.
3. 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.
4. Let the reactor fill up with both solutions until it is just about to 1/2 full.
5. Switch ON the stirrer M1.
6. Adjust the valves V5 and V10 to give the desired flow rate. Make sure that
both flow rates are maintained the same.
7. Start monitoring the conductivity value at QI-401.
8. Start the timer and record the conductivity value (QI-401) and both flow
rates (FI-301 and FI-302) when it has reached steady state (Conductivity
value begin to steadily decline with time).
9. Record the conductivity values and both flows rate for every 5 minutes until
the conductivity 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.
11. Repeat the experiment (steps 6 to 10) for different residence times by
adjusting the feed flow rates of NaOH and Et(Ac).
12. Make sure that both flow rates are maintained the same.
13. Perform the general shut-down procedures.
4.0 ANALYSIS AND DISCUSSION:
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.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
3. Plot a graph of conversion, X vs. reaction time, t for the different flow rate.
Discuss the graph.
4. The reactor’s residence time is defined as the reactor volume divided by the
average total feed flow rates.
VCSTR
Residence Time, t =
F0
Subsequently calculate the average residence time, τavg (NOTE: 1 FLOW RATE
PARAMETER GIVES 1 AVERAGE RESIDENCE TIME).
5. Compare the highest conversion, X for the different average residence time, τavg
(NOTE: 1 FLOW RATE PARAMETER GIVES 1 AVERAGE RESIDENCE TIME).
Compare the highest conversion, X at the different average residence time, τavg.
Discuss thoroughly and explain how residence time can influence the rate of
reaction.
6. For the different average reactor residence times, τavg (NOTE: 1 FLOW RATE
GIVES 1 AVERAGE RESIDENCE TIME), calculate the value of the reaction rate
constant, k and the rate of reaction, –rA.
5.0 TUTORIAL
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
6.1 OBJECTIVES:
To determine the effect of temperature on the extent of conversion.
To determine the value of the reaction’s activation energy.
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 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.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
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.
5. For different reactor temperatures, calculate the value of the reaction rate
constant, k.
6. Plot a graph of ‘ln k’ vs ‘1/T’ and evaluate the slope and y-axis intercept.
æ -Ea ö
From Arrhenius equation, k(T ) = A exp ç ÷
è RT ø
(R = 8.314 J/mol.K)
-Ea æ 1 ö
In linear form ln k = ç ÷ + ln A
R èT ø
8.0 TUTORIAL
1. Discuss the advantages and disadvantages of using CSTR reactors in chemical
reaction. Describe an example of industrial applications that utilized CSTR
reactors in its process.
2. Write a one-paragraph summary of any journal article that studies chemical
reaction in a CSTR. The article must have been published within the last 5 years.
Explain on the CSTR reactor used in the study and its significance to the study
done.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
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.
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 2019) REACTION ENGINEERING (CKB 20104)
APPENDIX B
RESULTS FOR EXPERIMENTS
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
𝐶𝑁𝑎𝑂𝐻(𝑡=0)− 𝐶𝑁𝑎𝑂𝐻(𝑡)
𝑋= × 100%
𝐶𝑁𝑎𝑂𝐻(𝑡=0)
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
EXPERIMENT
Pipe length 15 m
3. Pumps (P1/P2)
Centrifugal pumps
4. Pre-heater (W1/W2)
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
6. Instrumentations
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.
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.
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LABORATORY MANUAL (JAN 2019) 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
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
3. Fill the feed vessel B1 with the NaOH and feed vessel B2 with the Et(Ac)
solution.
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.
4. Open valves V3, V4, V5, V6, V7, V8 and V11 to drain all liquid from the unit.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
3.1 OBJECTIVE
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.
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.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
4. The reactor’s residence time is defined as the reactor volume divided by the
average total feed flow rates.
VPFR
Residence Time, t =
F0
Subsequently calculate the average residence time, τavg (NOTE: 1 FLOW RATE
PARAMETER GIVES 1 AVERAGE RESIDENCE TIME).
5. Compare the highest conversion, X for the different average residence time, τavg
(NOTE: 1 FLOW RATE PARAMETER GIVES 1 AVERAGE RESIDENCE TIME).
Compare the highest conversion, X at the different average residence time, τavg.
Discuss thoroughly and explain how residence time can influence the rate of
reaction.
6. For the different average reactor residence times, τavg (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 æ X ö
Reaction rate constant, k = ç ÷ AND Rate of reaction, - rA = kC A
2
VPFRC A0 è 1- X ø
5.0 TUTORIAL
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
6.1 OBJECTIVE:
6.2 PROCEDURES:
4. Switch on the thermostat T1 and set the water to the desired temperature.
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.
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
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.
5. For different reactor temperature, calculate the value of the reaction rate constant,
k.
F0,avg æ X ö
Reaction rate constant, k = ç ÷
VPFRC A0 è 1- X ø
6. Plot a graph of ‘ln k’ vs ‘1/T’ and evaluate the slope and y-axis intercept.
æ -Ea ö
From Arrhenius equation, k(T ) = A exp ç ÷
è RT ø
(R = 8.314
-Ea æ 1 ö
In linear form ln k = ç ÷ + ln A
R èT ø
J/mol.K)
8.0 TUTORIAL
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
9.0 REFERENCES
2. Fogler H.S., “Elements of Chemical Reaction Engineering, 3rd Ed.”, Prentice Hall
(USA), 1999.
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 2019) REACTION ENGINEERING (CKB 20104)
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 2019) REACTION ENGINEERING (CKB 20104)
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 2019) 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
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)
6. Pumps (P1/P2)
Centrifugal pumps
7. Pre-heater (W1/W2)
9. Instrumentations
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.
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.
Vent
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
QI TI
401 101 R1
V14
Injection
V15
FI FI FI
B1 B2 301 302 303
P1 P2 V27
V3 V4
M M V5 V6 Process Water
HS HS
V7
1 2 B3 V26
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LABORATORY MANUAL (JAN 2019) 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.
3.1 OBJECTIVE:
3.2 PROCEDURES:
1. Perform the general start-up procedures
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LABORATORY MANUAL (JAN 2019) REACTION ENGINEERING (CKB 20104)
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.
VCSTR
Residence Time, t =
F
0
2. Calculate the value of the reaction rate constant, k and the rate of
reaction, –rA.
VCSTR
Residence Time, t =
F
0
2. Calculate the value of the reaction rate constant, k and the rate of
reaction, –rA.
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.
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
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 2019) 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 2019) REACTION ENGINEERING (CKB 20104)
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 2019) REACTION ENGINEERING (CKB 20104)
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 2019) REACTION ENGINEERING (CKB 20104)
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
39