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CONTINOUS STIRRED TANK REACTOR

(CSTR)

1.0 ABSTRACT/SUMMARY

Based on the title, this experiment had done in order to fulfil the
syllabus of Chemical Engineering Laboratory subject. Thus, the members
of the group should to know more detail about the Continuous Stirrer Tank
Reactor (CSTR) and to carry out the operation for the saponificaton of
Sodium Hydroxide, NaOH and ethyl acetate, Et(Ac). The objectives of the
experiment were to determine the reaction constant, k and to study the saponification
reaction between NaOH and ethyl acetate. The reaction rate, rA was measured throughout 5
minutes interval for 25 minutes. Then the samples that added with hydrochloric acid, HCL
and two drops of phenolpthalein indicator were titrated until the solution become light pink ..
The reaction constant, k was obtained from slope of graph of 1/Ca vs. time The results
obtained were according to the theory All the objectives were achieved. The values of the
reaction constant were obtained. The experiments were supposed to be conducted carefully so
that the results obtained for calculation are correct.

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CONTINOUS STIRRED TANK REACTOR
(CSTR)
2.0 INTRODUCTION

2.1 What Is The Continous Stirred Tank Reactor (CSTR) And How
Does Its Function?

The continuous stirred tank reactor (CSTR) is also known as vat- or backmix reactor, is
a common ideal reactor type in chemical engineering.[1] CSTR are open systems, operate at
steady state basis, where the conditions in the reactor do not change with time. Reactants are
continuously fed into the reactor and the products are continously removed.[2] A CSTR often
refer to a model to estimate the key unit operation variable when using a continuous agitated
tank reactor to reach a specified output. [1]
All calculation performed in CSTR are assume perfect mixing. In a perfect mixed
reactor, the output composition is identical to composition of the material inside the reactor,
which is a fuction of residence time and rate of reaction.[1]

2.2 Application Of Continous Stirred Tank Reactor (CSTR) In


Industries And Various Field.

Continous Stirred Tank Reactor are commonly used in industrial processing,


primarily homogenous liquid-phase flow reactions, where constant agitation is required. They
may be used by themselves, in series, or in battery. CSTR are also used in the pharmaceutical
industy as a loop reactor when heated, pressurized fluid enter it and etc.[3] A dimple jacketed
pressure vessel is shown in the diagram 2.2.1 and half jacket reactor in the diagram 2.2.2.

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CONTINOUS STIRRED TANK REACTOR
(CSTR)

Diagram 2.2.1 : Dimple Jacketed Pressure Vessel Diagram 2.2.2 : Half Jacket Reactor
CSTR like the diagram 2.2.3 below are always used in biological processes, such as
cell cultures. The CSTR shown below can be used for high density animal cell culture in
research or production. The vessels use are for single use.[3]

Diagram 2.2.3 : CSTR use in biological processes

Fermentors are CSTRs used in biological processes in many industries, such as


brewing, antibiotics, and waste treatment. In fermenters, large molecules are broken down
into smaller molecules, with alcohol produced as by- product. The industrial fermentor on the
figure 2.2.4 has a capacity 500 L and diagram 2.2.5 holds on 3.0 L.[3]

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CONTINOUS STIRRED TANK REACTOR
(CSTR)

Diagram 2.2.4 : 500 L capacity fermentor Diagram 2.2.5 : 3.0 L capacity fermentor

2.3 Advantages and Disadvantages of Continous Stirred Tank


Reactor (CSTR)

CSTR is easiy maintained because its works as good temperature controller.


Furthermore, CSTR is cheap to construct as well as has large heat capacity. In addition, the
interior reactor is easily accessed.[4]
The disadvantage of CSTR is the conversion of reactant to product per volume of the
reactor is small compared to the other flow reactors.[4]

3.0 OBJECTIVES

Firstly, th objective of this experiment are to determine the reaction rate constant, k for
batch reaction. Furthermore, to study saponification of ethyl acetate and sodium hydroxide.

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CONTINOUS STIRRED TANK REACTOR
(CSTR)

4.0 THEORY

4.1 IDEAL STIRRED-TANK REACTOR

A stirred-tank reactor (STR) may be operated either as a batch reactor or as a steady-


state flow reactor (better known as Continuous Stirred-Tank Reactor (CSTR)). The key or
main feature of this reactor is that mixing is complete so that properties such as temperature
and concentration of the reaction mixture are uniform in all parts of the vessel. Material
balance of a general chemical reaction is described below.[5]

The conservation principle required that the mass of species A in an element of reactor
volume ∆V obeys the following statement:

Rate of Rate of
A A Rate of A Rate of A
Accumulate
into - out of + produced = d
within within
volume volume volume volume
elemen elemen
t t element Element

4.2 BATCH STIRRED-TANK REACTOR (BSTR)

In batch reactions, there are no feed or exit streams and therefore equation (1) can be
simplified into:
Rate of A Rate of A
accumulate
produced = d
within within

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CONTINOUS STIRRED TANK REACTOR
(CSTR)
volume volume
element element

The rate of reaction of component A is defined as:

-rA = 1/V (dNA/dt) by reaction = [moles of A which appear by reaction]


[unit volume] [unit time]

By this definition, if A is a reaction product, the rate is positive; whereas if it is a reactant


which is consumed, the rate is negative.

Rearranging equation,
(-rA) V = NAO dXA
dt

Integrating equation gives,


t = NAO ∫ dXA__
(-rA)V

where t is the time required to achieve a conversion XA for either isothermal or non-
isothermal operation.[5]
1/-rA

Area = t

Ca

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CONTINOUS STIRRED TANK REACTOR
(CSTR)

4.3 EFFECT OF TEMPERATURE ON RATE OF REACTION

As we increase the temperature the rate of reaction increases. This is because, if we


heat a substance, the particles move faster and so collide more frequently. That will speed up
the rate of reaction. Collisions between molecules will be more violent at higher
temperatures. The higher temperatures mean higher velocities. This means there will be less
time between collisions. The frequency of collisions will increase. The increased number of
collisions and the greater violence of collisions result in more effective collisions. The rate
for the reaction increases. Reaction rates are roughly doubled when the temperature increases
by 10 degrees Kelvin.[5]

In any single homogenous reaction, temperature, composition and reaction rate are
uniquely related. They can be represented graphically in one of three ways as shown in figure
4.3 below:

C r3
r2
r1

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CONTINOUS STIRRED TANK REACTOR
(CSTR)

T
Figure 4.3 : the graphically related between homogenous reaction, temperature and reaction
rate

5.0 APPARATUS

1) Continuous Stirred Tank Reactor (MODEL BP 100)

Controller such as
reactor switch of pump

Tube in taking
the sample

2) 0.1 M ethyl acetate – for reaction

3) 0.1 M and 0.25 M NaOH. – for reactor and titration respectively

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CONTINOUS STIRRED TANK REACTOR
(CSTR)
4) 0.25 M HCL – for titration

5) Conical flask – used in titration

6) Burette – put of NaOH during titration and being put on the retort stand

7) Phenolphthalein – as the indicator in titration( the solution will turn light pink)

8) measuring cylinder – to measure the sample or used of solution to get correct calibration.

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CONTINOUS STIRRED TANK REACTOR
(CSTR)

6.0 PROCEDURE

6.1 In the reactor

Firstly, before starting the experiment, the tank that contains of ethyl acetate and
NaOH must be checked. Then, the experiment is started to fill the reactor with NaOH and
ethyl acetate. The pump 1 is switched on to pump the ethyl acetate until reaches 1.25 liters or
reaches the line that being marked on the reactor. Finished to fill with ethyl acetate then fill
the reactor with NaOH by switch on the pump 2. This pump 2 is being switched on for the
NaOH solution being pump until the solution reaches mark of 2.5 liters. The stirrer will be
switched on and the speed be set at 180 rpm. The timing will be immediately started. At time
t=1 minutes, the samples being taken about 50 mL by opened the valve 7 and the titration will
be done. Then, the timing is reset for 5, 10, 15, 20 and 25 minutes. An example will be taken
for the time taken. All of the sample will be titrated.

6.2 During titration

Firstly, 10 mL of HCL is put inside the conical flask and added 3 drops of
phenolphthalein. After that, the sample that being taken will be mixed with this solution.
Then, it is being titrated with NaOH until reaches light pink. The data for used of NaOH
during titration was recorded.

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7.0 RESULT

7.1 The feed concentration, standard solution concentration with


volume and volume of sample used.

Feed Concentration Conc. of NaOH = 0.05


moles/liter
Conc. of Ethyl Acetate = 0.1
moles/liter
Standard Solution Conc. of HCl = 0.25
moles/liter
Volume of HCl = 10
moles/liter
Conc. of NaOH = 0.1
moles/liter
Sample Volume of sample = 50 ml

Table 7.1 : The feed concentration, standard solution concentration with


volume and volume of sample used.

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7.2 The volume of Sodium Hydroxide needed to neutralize the


sample solution

Time Volume Volume of Volume of Mole of HCl Mole of


(min) of Quenching HCl Reacted with NaOH
titrating HCl Reacted NaOH in Unreacted in
NaOH Unreacted with NaOH Sample Sample
(ml) with NaOH in in Sample
Sample (ml) (ml)
1 15.7 6.28 3.72 0.00093 0.00093
5 21.2 8.48 1.52 0.00038 0.00038
10 23.0 9.20 0.80 0.00020 0.00020
15 23.7 9.48 0.52 0.00013 0.00013
20 24.0 9.60 0.40 0.00010 0.00010
25 25.0 10.00 0.00 0.00000 0.00000
Table 7.2: The volume of Sodium Hydroxide needed to neutralize the
sample solution

7.3 The concentration and mole fraction af reacted and unreacted


sodium hydroxide,NaoH with Ethyl Acetate
Concentrati Steady Concentratio Mole of Concentratio Concentratio
on of NaOH state n of NaOH NaOH n of Ethyl n of Ethyl
Unreacted Fraction Reacted with Reacted Acetate Acetate
with Ethyl Conversi Ethyl with Ethyl Reacted with unreacted
Acetate on of Acetate Acetate in NaOH (moles/litre)
(moles/litre) NaOH, XA (moles/litre) Sample (moles/litre)
,CA
0.0186 0.628 0.0064 0.00032 0.0064 0.0436
0.0076 0.848 0.0174 0.00087 0.0174 0.0326
0.0040 0.920 0.0210 0.00105 0.0210 0.0290

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0.0026 0.948 0.0224 0.00112 0.0224 0.0276
0.0020 0.960 0.0230 0.00115 0.0230 0.0270
0.0000 1.000 0.0250 0.00125 0.0250 0.0250

Table 7.3: The concentration and mole fraction af reacted and unreacted
sodium hydroxide,NaoH with Ethyl Acetate

1/CA vs time (min)


700

600
f(x) = 95.66x
500 R² = 0.99

400
1/CA
300

200

100

0
1 5 10 15 20 25

time (min)

Figure 7.3.1: Graph of 1/CA vs time (min)

Rate constant, k (Lmol-1min-1) = 25.304

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8.0 SAMPLE CALCULATION

Volume of Quenching HCl Unreacted with NaOH in Sample (ml) :

C NaOH , std
¿ × Volume of titrating NaOH (ml)
C HCl ,std

0.1
¿ ×15.7
0.25

¿ 6.28 ml

Volume of HCl Reacted with NaOH in Sample (ml) :

¿ V HCl −Volume of Quenching HCl Unreacted with NaOH ∈ Sample(ml)

¿ 10−6.28

¿ 3.72ml

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Mole of HCl Reacted with NaOH in Sample :

¿ C HCl , std × Volume of HCl Reacted with NaOH ∈Sample( ml)

¿ ( 0.25 ×3.72 ) ÷ 1000

¿ 0.00093 moles

Mole of NaOH Unreacted in Sample = Mole of HCl Reacted with NaOH


in Sample

Concentration of NaOH Unreacted with Ethyl Acetate


(moles/litre) :

Mole of HCl Reacted with NaOH ∈Sample


¿ ×1000
Vs

0.00093
¿ ×1000
50

¿ 0.0186 moles /litre

Steady state Fraction Conversion of NaOH, XA :

Concentration of NaOH Unreacted with Ethyl Acetate (moles /litre)


¿ 1−
C AO

0.0186
¿ 1−
0.05

¿ 0.628

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Concentration of NaOH Reacted with Ethyl Acetate (moles/litre) :

¿ C NaOH ,o −Concentration of NaOH Unreacted with Ethyl Acetate ( moles


litre )

¿ 0.025−0.0186

moles
¿ 0.0064
litre

Mole of NaOH Reacted with Ethyl Acetate in Sample :

¿ Concentration of NaOH Reacted with Ethyl Acetate ( moles


litre )
×V s

¿ 0.0064 ×0.05

¿ 0.00032 moles

Concentration of Ethyl Acetate Reacted with NaOH (moles/litre) :

Mole of NaOH Reacted with Ethyl Acetate∈Sample


¿
Vs

0.00032
¿
0.05

moles
¿ 0.0064
litre

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CONTINOUS STIRRED TANK REACTOR
(CSTR)
Concentration of Ethyl Acetate unreacted (moles/litre) :

¿ C EA , o−Concentration of Ethyl Acetate Reacted with NaOH ( moles


litre )

¿ 0.05−0.0064

moles
¿ 0.0436
litre

9.0 DISCUSSION

NaOH + Et(Ac) → Na(Ac) + EtOH

The experiment was carried out by using special hydroxide and ethyl acetate. Inside
the reactor, the saponification of sodium hydroxide and ethyl acetate producing sodium
acetate and ethanol. Order of the reaction is based on the powers of the concentration which
are raised in the kinetic law. Based on result and the sample of calculation, the value of data
was fitted to second order reaction.[5]

From Arrhenius’s equation, k = Ae-E/RT it show that the temperature has an effect to
the reaction rate constant. It states that when the rate constant doubles, so wills the rate of
reaction. The higher the temperature the faster the molecules move producing much more
kinetic energy than normal. More collision is happen in order for a reaction to occur and thus
larger fraction of molecules to provide the activation energy needed for the reaction.
Activation energy, Ea is the minimum energy needed for the reaction to occur.[5]
Therefore, the rate law for this experiment is:

-dCa/dt = kCa2

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The time taken for each sample taken is from the first minute the time started and
followed by the next 5th minute, 10th minute, 15th minute, 20th minute, and 25th minute. The
volume of titrating sodium hydroxide to calculate the amount of quenching hydrochloric acid,
phenolphthalein is used to be indicator of the mixture to be in neutral condition. Volume of
quenching hydrochloric acid unreacted with sodium hydroxide in sample is calculated using
the amount of sodium hydroxide titrated with the mixture.

The slopes of the graph are representing the specific reaction rate constant, K. K
constant can be obtained by considering all the data obtained throughout the experiment.
Based on the calculation, K can be calculated.

Since the reaction is second order, the reaction rate by the rate law is in the form of
-ra =kCACB. Then for this experiment, the volume of quenching HCL unreacted with NaOH
ins sample (ml) is 6.28 ml, 8.48 ml, 9.20 ml, 9.48 ml, 9.60 ml and 10.00 ml. Next, the
volume of HCL reacted with NaOH in sample (ml) is 3.72 ml, 1.52 ml, 0.80 ml, 0.52 ml,
0.40 ml and 0.00 ml respectively.

The volume of titrating NaOH for experiment A was increased from 15.7 ml, 21.2 ml,
23.0 ml, 23.7 ml, 24.0 ml and 25.0 ml. That means the higher the concentration of HCL, the
more volume of NaOH is needed to neutralize the mixture.

After calculating all the data obtained, values of constant k can be known. From the graph,
the value k is 25.304 Lmol-1min-1.

10.0 CONCLUSION

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After the experiment has been done and the parameters needed is found, a conclusion for
this experiment had been made. The objective of this experiment obtained successfully. First
and foremost, this reaction is a 2 nd order. Therefore, the reaction rate by the rate law is in the
form of -ra=kCACB. The second conclusion is that from the graph, the value k is 25.304 Lmol -
1
min-1.

11.0 RECOMMENDATION

In this experiment there have certain things that need to be considered on to get most
accurate data and some suggestion to increase the accuracy. Firstly, the solution in reactor
need to be sure completely mixed before the sample is taken. This is to prevent the error
while doing the titration.

Secondly, while handling this chemical, student should use the gloves and googles if
need. Then, when titration, make sure the 10 mL of HCL must be put into the conical flask
and added with 3 drops of phenolphthalein then put the sample from the reactor. The titration
need to be done carefully until it reaches the light pink.

Before taking the sample from the reactor, when opened the valve 7 the sample need to
be throw a little bit then it can be taken for 50 mL. This is to prevent if the sample that
contain in tube is not the best sample in the reactor.

Make sure all the flask, apparatus that involved in titration process is cleaned from
chemicals because it will affect the titration results. Then, wait until the system stable before
taking the reading, because sometimes, the system is not well reacted, but students already
take the readings.

Furthermore, make sure all valves are in their right positions before starting the
experiments to prevent any damages into the equipment. Before taking the sample, make sure
flush the products a little bit, just to ensure there are no previous product in the outlet stream

Last but not least, do not let the temperature shoot higher or lower than the
temperature needed. Make sure the temperatures are well controlled.

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12.0 REFERENCES

[1] Schmidt, Lanny D. (1998). The Engineering of Chemical Reactions. New York : Oxford
University Press.

[2] Fogler, Scott H. Elements of Chemical Reaction Engineering, 3rd Edition, Englewood
Cliffs,NJ : Prentice- Hall, 1998 , pp.180-191

[3] Wales, Stanley M. Chemical Process Equipment: Selection and Design. Boston :
Butterworth- Heinemann, 1990, pp 578-595

[4] Perry, Robert H, and Don W. Green. Perry’s Chemical Engineers’ Handbook. 7th Edition,
New York : McGraw- Hill Inc., 1997, pp 177-179

[5] Rate Constants and The Arrhenius Equation. Retrieved on APRIL 1, 2016 from
http://www.chemguide.co.uk/physical/basicrates/arrhenius.html

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CONTINOUS STIRRED TANK REACTOR
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13.0 APPENDICES

(data refer to the last page)

Continous Stirred Tank Reactor (CSTR)

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CONTINOUS STIRRED TANK REACTOR
(CSTR)

Titration Process of Sodium Hydroxide and Sample solution

The colour of the solution become light pink or pale pink

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CONTINOUS STIRRED TANK REACTOR
(CSTR)

TABLE OF CONTENTS

1.0 ABSTRACT/SUMMARY..................................................................................................1
2.0 INTRODUCTION.............................................................................................................2
2.1 What Is The Continous Stirred Tank Reactor (CSTR) And How Does Its
Function?.............................................................................................................................2
2.2 Application Of Continous Stirred Tank Reactor (CSTR) In Industries
And Various Field.............................................................................................................2
2.3 Advantages and Disadvantages of Continous Stirred Tank Reactor
(CSTR)..................................................................................................................................4
3.0 OBJECTIVES.....................................................................................................................4
4.0 THEORY............................................................................................................................5
4.1 IDEAL STIRRED-TANK REACTOR..........................................................................5
4.2 BATCH STIRRED-TANK REACTOR (BSTR)..........................................................5
4.3 EFFECT OF TEMPERATURE ON RATE OF REACTION.....................................7
5.0 APPARATUS.....................................................................................................................8
6.0 PROCEDURE...................................................................................................................9
6.1 In the reactor.............................................................................................................9
6.2 During titration..........................................................................................................9
7.0 RESULT...........................................................................................................................10
7.1 The feed concentration, standard solution concentration with volume
and volume of sample used......................................................................................10
7.2 The volume of Sodium Hydroxide needed to neutralize the sample
solution..............................................................................................................................11
7.3 The concentration and mole fraction af reacted and unreacted
sodium hydroxide,NaoH with Ethyl Acetate........................................................11
8.0 SAMPLE CALCULATION.............................................................................................13
9.0 DISCUSSION.................................................................................................................15
10.0 CONCLUSION.............................................................................................................17
11.0 RECOMMENDATION.................................................................................................17
12.0 REFERENCES.............................................................................................................18

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13.0 APPENDICES..............................................................................................................19

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