FACULTY OF CHEMICAL ENGINEERING

NAME : JAY MAC MILLAN BIN AZMAN

STUDENT ID : 2019582099
GROUP : EH2205B GROUP 1
EXPERIMENT : CONTINUOUS STIRRED TANK REACTOR
DATE PERFORMED : 11HB MARCH 2020
SEMESTER :5
PROGRAMME / CODE : REACTION ENGINEERING LABORATORY (CHE506)
LECTURER : DR. SHARMEELA MATALI

No. Title Allocated Marks (%) Marks

1 Abstract
2 Introduction
3 Objective
4 Theory
5 Materials & Apparatus
6 Methodology
7 Result
8 Calculation
9 Discussion
10 Conclusion
11 Recommendation
12 References
13 Appendices
TOTAL MARKS 100

Remarks:

Checked by:
TABLE OF CONTENTS

1.0 Abstract 1
2.0 Introduction 2
3.0 Objectives 3
4.0 Theory 4-6
5.0 Materials & Apparatus 7-8
6.0 Methodology 9-10
7.0 Results 11-13
8.0 Calculation 14
9.0 Discussion 15-17
10.0 Conclusion 18
11.0 Recommendation 19
12.0 References 20
13.0 Appendices 21-22
1.0 ABSTRACT

Continuous stirred tank reactor (CSTR) is a common model for a chemical reactor in
chemical engineering. For this experiment, a laboratory scaled CSTR is used to
demonstrate its fundamental and working principle and to achieve the experiment
objectives. The objectives of this experiment are to carry out a saponification reaction
between NaOH and Et(Ac) in a CSTR, determine its reaction order via integral method
and identify the effect of temperature on the reaction of CSTR. A sample of 50 mL is
collected from the reactor for the reaction time of 1, 5, 10, 15, 20 and 25 minutes. These
samples are then taken to back titration process against 0.1 M NaOH where the volume
of NaOH titrated is then being used to calculate the concentration of NaOH at the outlet
stream. The graph of 1/CNaOH against time is then plotted to be compared with the
assumption that the reaction possesses a second reaction order. This experiment is
conducted at temperature 30°C ,40°C and 50°C .It is found that the graph is in a linearly
increasing manner with y-intercept of 1/CA and is consistent with second order reaction
graph found theoretically. The objectives are successfully obtained therefore the
experiment is successfully done.

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2.0 INTRODUCTION

A CSTR is a batch reactor equipped with an impeller or other mixing units to provide
efficient mixing. In chemical engineering, the CSTR is often used to refer to an idealised
agitated tank reactor used to model operation variables required to attain a specified output
before translating it into an industrial scale. CSTR applications is mainly on liquid-phase
reactions as in this experiment, and gas-liquid reactions. There some advantages of CSTR
which is reason why some industries prefer it. The general advantages from the use of CSTR
is low operating cost, consistent product quality due to reproducible process control and wide
range of throughput. However, this equipment does possess some disadvantages that
includes lower final conversion value. This is due to uncomplete mixing of liquid inside reactor
that causes unreacted starting material to get into the product stream. Besides, CSTR requires
higher investment or initial cost of operation compared to other reactor types to implement
the tedious continuous operation. For research or academic purposes, CSTR can be used to
study chemical kinetics studies, batch or continuous process, effect, or residence time on
reaction rate, and effect of temperature on reaction rate. To understand it, continuous stirred
tank reactor (CSTR) model BP100 has been designed to introduce students of Chemical
Engineering on reactor and reaction behaviour.

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3.0 OBJECTIVES

There were several objectives in conducting the experiment:

1) To carry out the continuous process of saponification reaction between NaOH
and Et(Ac).
2) To plot the graph of 1/CA against time.
3) To identify the effect of temperature on the reaction in a CSTR

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4.0 THEORY

There are several common continuous flow reactors such as continuous stirred tank
reactors (CSTR), the plug flow reactor (PFR) and the packed bed reactor (PBR). All of
them are almost operated at steady state. It. For this experiment, the working principle
and application of CSTR is studied and observed. CSTR is a type of reactor used
commonly in industrial processing primarily in the liquid phase reactions. It is normally
operated at steady state and is assumed to be perfectly mixed; consequently, there is no
time dependence or position dependence of the temperature, concentration, or the
reaction rate inside the CSTR. That is, every variable is the same at every point inside
the reactor. Because the temperature and concentration are identical everywhere within
the reaction vessel, they are the same at the exit point as they are elsewhere in the tank.
Thus, the temperature and concentration in the exit stream are modelled as being the
same as those inside the reactor. In systems where mixing is highly nonideal, the well-
mixed model is inadequate and we must resort to other modelling techniques such as
residence-time distributions, to obtain meaning full results. Figure 1 shows the cross-
section of a CSTR and CSTR mixing patterns.

Figure 4.1: Continuous Stirred Tank Reactor (CSTR)

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A mole balance on species j at any instant in time t, yields the following equation:

𝑅𝑎𝑡𝑒 𝑜𝑓 𝑔𝑒𝑛𝑒𝑟𝑎𝑡𝑖𝑜𝑛 𝑅𝑎𝑡𝑒 𝑜𝑓

𝑅𝑎𝑡𝑒 𝑜𝑓 𝑓𝑙𝑜𝑤 𝑅𝑎𝑡𝑒 𝑜𝑓 𝑓𝑙𝑜𝑤
𝑜𝑓 𝑗 𝑏𝑦 𝑐ℎ𝑒𝑚𝑖𝑐𝑎𝑙 𝑎𝑐𝑐𝑢𝑚𝑢𝑙𝑎𝑡𝑖𝑜𝑛
𝑜𝑓 𝑗 𝑖𝑛𝑡𝑜 𝑜𝑓 𝑗 𝑜𝑢𝑡 𝑜𝑓
𝑟𝑒𝑎𝑐𝑡𝑖𝑜𝑛 𝑤𝑖𝑡ℎ𝑖𝑛 𝑜𝑓 𝑗 𝑤𝑖𝑡ℎ𝑖𝑛
𝑡ℎ𝑒 𝑠𝑦𝑠𝑡𝑒𝑚 − 𝑡ℎ𝑒 𝑠𝑦𝑠𝑡𝑒𝑚 + =
𝑡ℎ𝑒 𝑠𝑦𝑠𝑡𝑒𝑚 𝑡ℎ𝑒 𝑠𝑦𝑠𝑡𝑒𝑚
𝑚𝑜𝑙𝑒 𝑚𝑜𝑙𝑒
( ) ( ) 𝑚𝑜𝑙𝑒 𝑚𝑜𝑙𝑒
[ 𝑡𝑖𝑚𝑒 ] [ 𝑡𝑖𝑚𝑒 ] ( ) ( )
[ 𝑡𝑖𝑚𝑒 ] [ 𝑡𝑖𝑚𝑒 ]

Where the simplified general mole balance equation gives about to:
𝑣
𝑑𝑁𝑗
𝐹𝑗,𝑜 − 𝐹𝑗 + ∫ 𝑟𝑗 𝑑𝑉 = 𝐸𝑞𝑢𝑎𝑡𝑖𝑜𝑛 4.0
𝑑𝑡
0

And is applied to a CSTR operated at steady state (i.e., conditions do not change with
time),
𝑑𝑛𝑗
= 0 𝐸𝑞𝑢𝑎𝑡𝑖𝑜𝑛 4.1
𝑑𝑡

In which there are no spatial variations in the rate of reaction (i.e., perfect mixing),
𝑣

∫ 𝑟𝑗 𝑑𝑉 = 𝑉𝑟𝑗 𝐸𝑞𝑢𝑎𝑡𝑖𝑜𝑛 4.2

0

It takes the familiar form known as the design equation for a CSTR:

𝐹𝑗,𝑜 − 𝐹𝑗
𝑉= 𝐸𝑞𝑢𝑎𝑡𝑖𝑜𝑛 4.3
−𝑟𝑗
The CSTR design equation gives the volume V necessary to reduce the entering flow
rate of species j, from Fjo to the exit flow rate Fj, when species j is disappearing at a
rate of -rj.

The mole balance, Equation 4.3, when applied to species A in the reaction,
𝑏 𝑐 𝑑
𝐴+ 𝐵 → 𝐶 + 𝐷 𝐸𝑞𝑢𝑎𝑡𝑖𝑜𝑛 4.4
𝑎 𝑎 𝑎

Can be arranged to
𝐹𝐴,𝑜 − 𝐹𝐴
𝑉= 𝐸𝑞𝑢𝑎𝑡𝑖𝑜𝑛 4.5
−𝑟𝐴

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We now substitute for FA in terms of F A0 and X
𝐹𝐴 = 𝐹𝐴,𝑜 − 𝐹𝐴,𝑜 𝑋 𝐸𝑞𝑢𝑎𝑡𝑖𝑜𝑛 4.6
Then substitute into Equation 4.5 and further simplify to see the CSTR volume
necessary to achieve a specified conversion X is,

𝐹𝐴,𝑜 𝑋
𝑉= 𝐸𝑞𝑢𝑎𝑡𝑖𝑜𝑛 4.6
(−𝑟𝑗 )𝑛𝑒𝑤

Collection and analysis of rate data via homogenous reactions are made through the
method of integral where several plots of graphs are made on different axes
parameters and then compared to the theoretical plot for the determination of reaction
order and rate constant of a particular reaction.

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5.0 MATERIAL & APPARATUS

Figure 5.1: Solteq CSTR Model BP 100

Figure 5.2: Materials used in experiment

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Figure 5.3: An acid-base titration indicator Figure 5.4: 0.1 M of NaOH used for
titration

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6.0 METHODOLOGY

General Start-up Procedures.

1. The following solutions are prepared:
a. 20 L of sodium hydroxide, NaOH (0.1M)
b. 20 L of ethyl acetate, Et (Ac) (0.1M)
c. 1 L of hydrochloric acid, HCL (0.25M), for quenching.
2. Valves are initially closed.
3. The feed tanks are charged as follows:
a. The charge ports for tanks T1 and T2 are opened.
b. NaOH solution is carefully poured into vessel T2 and the Et (Ac)
solution into vessel T1.
c. The charge port caps are closed for both tanks.
4. The power for the control panel is turned on.
5. The heater is only switched on if it is fully submerged in the liquid. The liquid
level is always maintained at the level above the height of the heater to avoid
damage to the heater.
6. Assembly of the stirrer is made sure properly secured to avoid damages to the
mechanical seal.
7. All of the tubing is periodically inspected for leakage and worm out. Leakage
might cause damage to equipment by corrosive reactants.
8. The unit is now ready for experiment.

Experimental Procedures.
1. Pump P1 is switched on to allow 1.25 L of 0.1 M ethyl acetate, Et (Ac), from the
feed tank into reactor. The pump is then switched off upon reaching the desired
volume.
2. Pump P2 is then switched on to allow 1.25 L of 0.1 M sodium hydroxide, NaOH,
into the reactor. The pump is then switched off as the total volume of 2.5 L of liquid
in the reactor has been reached.
3. The stirrer is then switched on and the timer is started.
4. 1 minute into the experiment, 50 mL of sample is collected through the opening
of valve V4.
5. The sample is then quenched with 10 mL of hydrochloric acid, HCL, to
immediately stopped any further reaction from occurring.
6. Addition of 3 drops of phenolphthalein are added prior to back titration against
0.1M of NaOH solution.

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7. The volume of NaOH needed to titrate the sample until equilibrium is achieved,
that is the solution in the conical flask turns to light pink are recorded.
8. Steps 4-7 are repeated for the experiment time of 5, 10, 15, 20, and 25 minutes.
9. Step 8 is repeated in which temperature is set at 30°C, 40°C and 50°C.
10. The experiment is then prepared to be shut down.

General Shut-down Procedures.

1. The cooling water valve from main pipe is kept open to allow the cooling water
to continue flowing.
2. Both pumps P1 and P2 are switched off. The stirrer is switched off and the heater
is allowed to cool down to room temperature.
3. The power for the control panel is turned off.
4. The reactor and the tubings are cleaned after each experiment as NaOH and Et
(Ac) are corrosive and can damage the tubings and reactor after sometime.
5. All liquids are disposed immediately after each experiment and the reactants or
products in the tank must be disposed as well.

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7.0 RESULTS

Table 7.1: Results obtained from the experiment at 30°C

Time(min) Volume of Volume of Concentration 1/ CA (L/mol)

sample (mL) NaOH titrated of NaOH, CA
(mL) (mol/L)
1 50 12.5 0.0250 40.00
5 50 14.1 0.0218 45.87
10 50 13.2 0.0236 42.37
15 50 14.4 0.0212 47.17
20 50 13.7 0.0226 44.25
25 50 13.0 0.0240 41.67

1/CA vs times
48

47

46
1/CA (L/mol)

45
y = 0.0415x + 43.029
44
R² = 0.0195
43

42

41

40
0 5 10 15 20 25 30
Time (mins)

Figure 7.1: Graph of 1/CA against time for a second order reaction at 30°C

Hence from the graph, it is found that the rate constant of this reaction,
k=0.0415 L/mol-1 min-1.

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Table 7.2: Results obtained from the experiment at 40°C

Time(min) Volume of Volume of Concentration 1/ CA (L/mol)

sample (mL) NaOH titrated of NaOH, CA
(mL) (mol/L)
1 50 12.9 0.0242 41.32
5 50 13.7 0.0226 44.25
10 50 13.8 0.0224 44.64
15 50 14.0 0.0220 45.45
20 50 13.8 0.0224 44.64
25 50 13.6 0.0228 43.86

1/CA vs times (40C)

46
45.5
y = 0.0822x + 42.985
45
R² = 0.2746
44.5
1/CA (L/mol)

44
43.5
43
42.5
42
41.5
41
0 5 10 15 20 25 30
Times (min)

Figure 7.2: Graph of 1/CA against time for a second order reaction at 40°C

Hence from the graph, it is found that the rate constant of this reaction,
k=0.0822L/mol−1 min−1.

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Table 7.3: Results obtained from the experiment at 50°C

Time(min) Volume of Volume of Concentration 1/ CA (L/mol)

sample (mL) NaOH titrated of NaOH, CA
(mL) (mol/L)
1 50 12.7 0.0246 40.65
5 50 13.7 0.0226 44.25
10 50 14.3 0.0214 46.73
15 50 13.8 0.0224 44.64
20 50 14.9 0.0202 49.50
25 50 14.2 0.0216 46.30

1/CA vs times (50C)

50
49
y = 0.2421x + 42.278
48 R² = 0.5528
47
1/CA (L/mol)

46
45
44
43
42
41
40
0 5 10 15 20 25 30
Times (min)

Figure 7.3: Graph of 1/CA against time for a second order reaction at 50°C

Hence from the graph, it is found that the rate constant of this reaction,
k=0.2421L/mol−1 min−1

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8.0 CALCULATION
Back Titration Sample Calculation for Identification of Concentration of NaOH
a) Concentration of NaOH entering the reactor, CNaOH,o
𝐶𝑁𝑎𝑂𝐻,𝑓 1𝑚𝑜𝑙/𝐿
= = 0.5𝑚𝑜𝑙/𝐿
2 2

b) Volume of unreacted quenching HCL, V2

𝐶𝑁𝑎𝑂𝐻,𝑠 0.1𝑚𝑜𝑙/𝐿
𝑥𝑉1 = 0.25𝑚𝑜𝑙/𝐿 𝑥12.5𝑚𝐿 = 5𝑚𝐿
𝐶𝐻𝐶𝐿,𝑠

c) Volume of HCL reacted with NaOH in sample, V3

𝑉𝐻𝐶𝐿,𝑠 − 𝑉2 = 10 − 5 = 5𝑚𝐿 = 0.005𝐿
d) Moles of HCL reacted with NaOH in sample, n1
0.25𝑚𝑜𝑙
𝐶𝐻𝐶𝐿,𝑠 𝑥 𝑉3 = 𝑥 0.005𝐿 = 0.00125mol
𝐿

e) Moles of unreacted NaOH in sample, n2

𝑛2 = 𝑛1
f) Concentration of unreacted NaOH in the reactor, CNaOH
1000 1000
𝑛𝑠 𝑥 = 0.00125 𝑥 = 0.025𝑚𝑜𝑙/𝐿
𝑉𝑠 50

*Calculation is made for the 1st minute into reaction time, with the volume of NaOH
titrated of 12.9mL to obtain the concentration of NaOH of 0.025mo/L
*The above calculation is repeated for reaction times of 5, 10, 15, 20 and 25 minutes
for respective volume of NaOH titrated
*The calculation is repeated for temperature 40°C and 50°C

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9.0 DISCUSSION

The main objective of the experiment is to carry out the continuous process of
saponification reaction between NaOH and Et(Ac), to plot the graph of 1/CA against
time and to identify the effect of temperature on the reaction in a CSTR.For this
particular experiment, saponification reaction of NaOH and Et(Ac) under continuous
stirred tank reactor (CSTR)is assumed occurred under steady state condition as well as
perfect mixing between the reactants. Collection and analysis of rate data is usually
achieved by measuring concentration as a function of time and then using either the
differential, integral or nonlinear regression method of data analysis to determine the
reactions order and specific reaction rate constant, k. To determine the reaction order
by integral method, initial reaction order are made and integrate the differential
equation used to model the batch system. If the assumed order is correct, the appropriate
plot of the concentration-time data should be linear with its intercepts intact. In this
method of analysis of rate data, the appropriate function of concentration corresponding
to a particular rate law that is linear with time is as follows:

Figure 9.1: Zero-order reaction Figure Figure 9.2: First-order reaction

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Figure 9.3: Second-order reaction Figure 9.4: Reaction-order >2

In this experiment, it is assumed that the reaction possessed a second order reaction
with the reaction rate equation:

−rA=kC2A Equation 9.0

Since the concentration of both reactants at the feed is the same, the concentration of B
at any time in the reactor is assumed the same a concentration of A at any time in the
reactor and hence the equation above is postulated.

Graph of 1/CNaOH against time is then plotted as shown in Figure 7.1, 7.2 and 7.3
based on the data obtained in the experiment for respective temperature. The initial
reading of concentration deviates as suppose to the linearly increasing pattern of the
expected graph in relative with time of reaction. This suggest that there is error
occurrence in conducting the experiment that leads to the inaccurate reading of
concentration in the 1st minute. From the equation of the graph, the slope and therefore
the rate constant is defined as k=0.0415 L/mol·min, k=0.0822 L/mol·min and k=0.2421
L/mol·min at temperature 30°C , 40°C and 50°C respectively.

It can be identified that there are several parameters that leads to error in results
obtained. The first being is the accumulation of unreacted reacted in the sample
collection stream. Mishandling of the equipment at some point of time as been used by
many different students that lack of knowledge on the equipment, may damage the
piping and fittings of CSTR that hinder its ability to work at its full efficiency. Next,
the tedious process of back titration can alter that volume of NaOH titrated needed for

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the sample to reach its end-point. As can be seen in Figure 13.2, the end point reached
differ for every reaction. This will leads to unnecessary amount of NaOH being titrated
into the sample and affect the whole calculation process as the increment of volume
from 1st minute to 25 minutes of reaction only takes places in less than 1 mL
theoretically. Last but not least, quenching of the sample proves to be important in this
experiment as to stop further reaction from occurring. Late quenching actions allows
the sample to react for a little longer that it should be and hence affect the volume of
NaOH titrated.

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10.0 CONCLUSION

The saponification reaction in CSTR has been observed with experimental data is
being used to determine the order of reaction for 3 temperature. The graph of 1/CNaOH
against time is then plotted to give a linear relationship that confirms a second order
reaction for this reaction. Slope of the graph, which is the rate constant, k, at
temperature 30°C, 40°C and 50°C are found to be 0.0415 L/mol·min, 0.0822
L/mol·min. and 0.2421 L/mol·min. respectively. Since the experiment is successfully
done. Hence, objectives are successfully obtained.

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11.0 RECOMMENDATION

In order to achieve a better result of experiment, some recommendations are

suggested. A better condition of CSTR equipment ensure the higher accuracy of data.
For example, well maintained part of CSTR such as the stirrer will ensure the mixing
process of the chemicals, hence increase the conversion of chemicals to products.
Besides, well condition heating coil of CSTR will ensure the uniform temperature of
chemicals, hence increase the consistency and accuracy of data. For back titration
process, some improvement can be made is to directly quench the sample with HCL.
This allow the reaction in the sample to a complete halt prior to titration against NaOH.
It is important to dispose some of the sample in the stream prior to sample collection to
be used in the titration. Lastly, the students should study the lab manual and prepare a
necessary table before conducting the experiment to ensure the experiment run
smoothly.

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12.0 REFERENCES

1) E. Education, H. E. Continuous, S. Tank, and C. Engineering, “Model: bp

100.”
2) H. S. Fogler, Elements of Chemical Engineering, 4th Edition. Pearson
Education
Limited, 2014
3) Robert H. Perry (1997). Perry’s Chemical Engineers Handbook (7th ed)
McGraw-Hill Co.
4) Schmidt, Lanny D. (1998). The Engineering of Chemical Reactions. New
York: Oxford University Press
5) https://www.labequip.co.za/docs/Continuous%20Stirred%20Tank%20Reactor
%20%20BP100.pdf
6) https://www.cs.montana.edu/webworks/projects/stevesbook/contents/chapters/
chapter008/section002/blue/page003.html

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1.3 APPENDICES

Figure 13.1: Value of NaOH titrated obtained experimentally.

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Figure 13.2: The end-point achieved through back titration of sample against 0.1 M NaOH

Figure 13.3: Back titration process

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