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S.no. Name of The Experiment Date of Conduction Date of Submission P2 Cascade CSTR 4 February, 2021 9 February, 2021

The document describes an experiment using a cascade of three continuous stirred tank reactors (CSTRs) to study the saponification reaction of ethyl acetate with sodium hydroxide. The objectives are to determine the reaction rate constant at ambient temperature. Samples are taken from each reactor and the amount of unreacted sodium hydroxide is measured through titration. The rate constant is calculated for each reactor using the conversion data. The results show increasing conversion and decreasing unreacted sodium hydroxide from the first to third reactor due to the cascade design.

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0% found this document useful (0 votes)
236 views14 pages

S.no. Name of The Experiment Date of Conduction Date of Submission P2 Cascade CSTR 4 February, 2021 9 February, 2021

The document describes an experiment using a cascade of three continuous stirred tank reactors (CSTRs) to study the saponification reaction of ethyl acetate with sodium hydroxide. The objectives are to determine the reaction rate constant at ambient temperature. Samples are taken from each reactor and the amount of unreacted sodium hydroxide is measured through titration. The rate constant is calculated for each reactor using the conversion data. The results show increasing conversion and decreasing unreacted sodium hydroxide from the first to third reactor due to the cascade design.

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DEEPSHIKA DUTTA
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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S.no.

Name of the Experiment Date of Date of


Conduction Submission

P2 Cascade CSTR 4 February, 2021 9 February, 2021

GROUP NUMBER: 9

GROUP MEMBERS:

OINDRILA GHOSH (2018A1PS0080G)


NISHANT HINGE (2018A1PS0385G)
ADITYA GOEL (2018A1PS0054G)
DEEPSHIKA DUTTA (2018A1PS0312G)
GANESH BHARATWAJ (2018A1PS0991G)

OBJECTIVE: ​To study the performance of a cascade of three equal volumed CSTRs in
series for the saponification of ethyl acetate with NaOH.

AIM: ​To determine the reaction rate constant for saponification of ethyl acetate with
NaOH at ambient temperature.

THEORY:

1. CSTR: CSTR, short for Continuous Stirred Tank Reactor, is a continuous reactor in
which the contents are well mixed due to constant agitation or stirring and remain at a
steady state.

2. Cascade: Cascade refers to a series of CSTRs placed one after the other. Here, 3 CSTRs
have been used in series.

3. Rate constant (k): ​The rate constant is the proportionality constant in the rate law
expression, at a given temperature. It is also known as the specific rate constant.

4. Saponification reaction:​ The reaction used in this experiment is a saponification


reaction,​ ​which is the base hydrolysis of a fat or oil, resulting in the formation of a soap
and an alcohol as a byproduct, is known as saponification. Saponification is used in the
soap industry, in fire extinguishers, etc.

5. Residence time (​τ)​:​ Residence time refers to the time required to process one reactor
volume of feed.

6. Conversion:​ The conversion of species A refers to the number of moles of A reacted per
mole of A fed.

In this experiment, we consider a ​bimolecular reaction (reacting species are ethyl acetate and
sodium hydroxide):

​ CH​3​COOC​2​H​5 ​ + NaOH = CH​3​COONa + C​2​H​5​OH (1)


(B) (A)

-r​A​= k C​A​C​B

Where, A represents NaOH and B represents CH​3​COOC​2​H​5​ .​


The initial concentrations of the reacting species are the same C​A0​= C​B0 (neglecting

change in density). Thus, if we take this into account, we have:.
2
-r​A =
​ kC​A​
C​A​= C​A0​ (1- X​A​)
Where X​A​ is the conversion of species A.

EXPERIMENTAL SETUP

The experimental setup, as shown in the figure below, consists of three identical stirred tanks
made of stainless steel arranged in a cascaded manner, two feed tanks through which
chemicals are fed to the reactors. The flow rates can be adjusted by operating the
needle valve and measured by rotameter. The compressed air is used for circulation of
feed. Pressure Regulator and Pressure gauge are fitted at the compressed air line.
PROCEDURE

1. Prepare 20 L of N/2 NaOH solution by dissolving 80 gm of NaOH in 20 L of


water.
2. Prepare 20 L of N/2 ethyl acetate solution by mixing 176 gm of ethyl acetate
in 20 L of water.
3. Fill the respective tanks with these solutions.
4. Adjust the flow rate of the two streams so that in the feed mixture
C​A0​=C​B0​.(i.e. have equal flow rates using calibrated rotameters).
5. Use phenolphthalein as indicator
6. Take 18 conical flasks and add 20 ml of N/10 HCl in each.
7. Fill the burette with N/10 NaOH.
8. Record the ambient temperature of reaction mixture
9. Fix a feed rate for inlet streams. F​A​=F​B​ (say 1-2 LPH)
10. Allow the two reactant streams to enter the first CSTR at equal feed rate so
that in the reactor C​A0​=C​B0​. Start the mixer and wait till you get the liquid out
from the 3rd CSTR.
11. Collect 50ml of mixture from the sampling outlet and discard them to clear
the stagnant zone.
12. Collect the 10 ml of sample at the outlet of 1st CSTR , IInd and IIIrd CSTR in
the conical flask containing N/10 HCl.
13. This Process should be repeated at an interval of 10 min (0,10,20 min from the
minute that 3rd CSTR starts to overflow)
14. Record the volumetric feed rate of ethyl acetate and NaOH.
15. Recheck the flowrate manually by collecting the amount of mixture overflows
from reactor III by keeping the time as constant.
16. Record the volume of each reactor (V​1​=V​2​=V​3​).
17. Change the flow rate of each stream (keep F​A​=F​B​ so that C​A0​=C​B0​) and repeat
the above steps for various flow rates (2.5, 5, 7.5, 10 LPH) to see how the
system reacts.
18. Estimate the unreacted NaOH in each conical flask by titration or by
measuring the conductance of the solution.

OBSERVATIONS and CALCULATIONS:

V​1​=V​2​=V​3​=V=1.2L
C​A0​ = C​B0​ = 0.25 mol/L
V(HCl) = 20ml
V(sample) = 10ml

Observation Table:

S.No Time(min) V​o​ LPH V​NaOH V​NaOH V​NaOH

Reactor 1 Reactor 2 Reactor 3

1 10 15.6 12.5 13.5 16

2 20 15.72 11.9 12.4 18.1

3 45 15.6 10.5 11.1 11.9


Calculation table:

Reactor T (min) HCLO HCLR C​A X​A X​A​/(1-X​A​)​2 τ k


No (mols) (mols) (gmol/
L) (min) (l/
gmol-min)

1 10 0.002 0.00075 0.075 0.7 7.77777778 4.61538462 6.740741

2 10 0.002 0.00065 0.065 0.74 10.9467456 4.61538462 9.487179

3 10 0.002 0.0004 0.04 0.84 32.8125 4.61538462 28.4375

1 20 0.002 0.00081 0.081 0.676 6.43956714 4.58015267 5.623889

2 20 0.002 0.00076 0.076 0.696 7.53116343 4.58015267 6.577216


2

3 20 0.002 0.00019 0.019 0.924 159.972299 4.58015267 139.7091


2

1 45 0.002 0.00095 0.095 0.62 4.29362881 4.61538462 3.721145

2 45 0.002 0.00089 0.089 0.644 5.08142911 4.61538461 4.403905


5

3 45 0.002 0.00081 0.081 0.676 6.43956714 4.61538461 5.580958


5

SAMPLE CALCULATIONS:
GRAPHS:

Graph of Concentration of unreacted NaOH vs Time:

DISCUSSIONS:

1. OINDRILA GHOSH: ​The base hydrolysis of a fat or oil, resulting in the


formation of a soap and, an alcohol as a byproduct, is known as saponification​.
Saponification is used in the soap industry, in chemical fire extinguishers and in the
production of grease removers, herbicides, etc. In this experiment, we use sodium
hydroxide as the base, which reacts with ethyl acetate to give sodium acetate (soap) and
ethanol (an alcohol) in a cascade of 3 continuous stirred tank reactors (CSTRs).

In accordance with the power law model of rate law, the rate equation can be expressed as: ​-r​A​=
k C​A​C​B​, where, A is NaOH and B is Et(Ac). Here, we take the same flow rate of both the
reactants (regulated using the rotameter) and thus, the initial concentration of both are the same
(​C​A0​= C​B0​). From the equation of the reaction, we know that reactants A and B react in the
stoichiometric ratio 1:1. This means that at every instant, ​C​A​= C​B​. The rate law reduces to: ​-r​A =

kC​A​2​. Thus, this is a ​bimolecular second order reaction​.

Before taking the first 10 ml sample from the reactors, we discard the first 50 ml from each tank.
In non-ideal/real reactors like in this experiment, there are non-idealities.​ Dead/stagnant zones
are formed near the bottom of the agitator. Here no mixing takes place and this is a clear
deviation from the CSTR assumption of perfect mixing. Thus, discarding the first 50 ml helps to
clear stagnant zones​. To the collected sample ​chilled HCl​ is added, which quenches the reactor
reaction and the HCl reacts with the unreacted NaOH present in the sample.

Conclusions from the observation table and graph:


a. As we move from tank 1 to tank 3, the amount of NaOH required for neutralization
increases​: This implies that more HCl is present in the quenched sample. This is because
less HCl is used up by the unreacted NaOH in the collected sample. This, in turn, implies
that less of unreacted NaOH is present, that is, the conversion is higher.
b. Residence time is the same for all the reactors:​ This is because for the same flow rate,
the average time spent in the same volume is the same. Residence time is evaluated as
reactor volume divided by volumetric flow rate. The three reactors have the same volume
and the volumetric flow rate is maintained at the same value for a particular run.
c. Flowrate and residence time are inversely related: ​This is because as flow rate
increases, for the same volume, the average amount of time spent by the species in the
reactor decreases.
d. Positive slope of the concentration of NaOH vs time plot:​ This is unexpected and
should ​not​ have a non zero slope ideally. Positive slope implies that with time, the
concentration of unreacted NaOH increases for a particular tank. However, the various
parameters like volumetric flow rate, volume of the tank, initial concentration remaining
constant, the conversion should remain the same with time in an ideal reactor. The
positive slope can be attributed to non-idealities and experimental errors.

The rate constant is evaluated analytically and the ​average​ of all the values is obtained as
23.36463 l/min.gmol.

CSTR vs PFR:​ Compared to PFR, CSTR has a lower theoretical efficiency or volumetric unit
conversion. In addition, due to the absence of moving parts, maintenance of PFRs is much easier.
In CSTRs, various types of non-idealities may be present: backmixing, channeling, dead zone
formation, etc. In PFRs there is hot spot formation, making temperature control very difficult. In
CSTRs, due to continuous mixing, there is no hot spot formation. Also, it is easier to clean and
construct CSTRs compared to PFRs.

Reason for using a cascade:​ In PFRs, the concentration decreases progressively along the
length of the reactor. In CSTRs, the concentration drops immediately to a low value. Thus, for
reactions with order greater than zero, PFR is better as the reaction rate increases with
concentration. When CSTRs are placed in series, the concentration is the same in each individual
reactor but it decreases progressively from one reactor to another. Due to the step wise drop in
concentration, a large number of CSTRs in series is expected to closely approximate a PFR.
Applications:​ CSTRs find applications in industrial processing of homogeneous liquid phase
flow reactions, where constant agitation is required- loop reactors for pharmaceutical production,
biogas production, fermentation, lagoon treatment systems, anaerobic digesters for stabilization
of wastewater biosolids, etc.

2. NISHANT HINGE:
In this experiment, we studied the saponification reaction taking place in 3
Controller Stirred tank reactors arranged in SERIES. The Reactors were
arranged in such a manner that the overflow from one reactor would be fed
for the next reactor.
The volume of each reactor was roughly 1.2L and the reaction taking place inside
the reactor is a saponification reaction between 0.5N ethyl acetate and 0.5N
sodium hydroxide. Saponification is a reaction between a base and esters to give
salts of long chain fatty acids(soap) and alcohol.
Both the solutions are injected in equal volumetric proportions so as to make the
effective concentration as 0.25N. It's important to let the system achieve steady
state and hence, we should let out the first portion of the product mixture before
taking any sample.

In a CSTR,​ agitators are used to achieve close to complete mixing of the


reactants.​ This is still not possible in real life scenarios and
stagnant-zone/dead-zones are formed at the bottom​ of the reactor where
unreacted mixture accumulates. Hence before collecting the sample for titration, it
is advisable to get rid of the first 50 ml of the sample to clear the accumulation in
the stagnant zone.

The 10 ml sample taken is mixed with 20 ml of 0.1N HCL and two drops of
phenolphthalein. The HCL reacts with unreacted sodium hydroxide. This complete
mixture is titrated against 0.1N standard solution of NaOH in order to ​find the
concentration of unreacted ethyl acetate.​ The data obtained from different Runs
is analysed and formulated.​ Rate law constant is found analytically using the
formulas​ as mentioned in the sample calculations.

The reactor is fed with an equimolar mixture of both the reactants, hence the
reaction is first order with respect to individual reactants but overall second order
reaction. ​Since the reactants are mixed in equal proportions, the reaction is
bimolecular in nature.
Graph is plotted for studying the trend of Concentration vs Time. From the
observation Table, We can observe that the​ volume of NaOH required for
neutralization is decreasing with increasing time.​ This means that more and
more HCL is consumed with time. Hence the amount of unreacted NaOH in the
reaction is increasing with time. This is clearly depicted in the graph with positive
slope. This type of trend ​shouldnt generally be observed because the rate of
reaction must attain a steady state value as time passes​. 45 minutes is more
than enough time for the setup to achieve steady state because parameters like
flow rate and temperature and pressure are kept fairly kept constant from the start
of the experiment. Since the flow rate is kept approximately equal to 15 lph
throughout the experiment, the ​residence time is almost constant throughout
the experiment which doesn't explain why the concentration of unreacted
NaOH is increasing with time.

Advantages of CSTR:
1. Continuous Operation is possible unlike a batch reactor.
2. Temperature Control is effective unlike a PFR.
3. Easy to Construct Operate and clean
4. Low Operating Cost.
Disadvantages of a CSTR:
1. Lowest Conversion per unit volume ratio.
2. Large reactor size required.
3. Stagnant zones/ Dead-zone formation leads to deviation from ideality.

3. DEEPSHIKA DUTTA:
The aim of the experiment is to study the performance of a cascade of three
CSTRs of equal volume. Feed tanks were fed with NaOH and Ethyl Acetate and a
saponification reaction which is base hydrolysis of fats/lipids was carried out.
The reaction had N/2 NaOH and N/2 ethyl acetate. Since the feeds are of the same
volume, the net concentration becomes N/4 or 0.25N.
Saponification reactions are in general irreversible second order reactions with rate
rA = -kCACB where CA is concentration of first reactant, CB is concentration of
second reactant. We took 10 mL of the sample and allowed 0.1N HCl to react
with it. Now, it is titrated against 0.1N NaOH to get the concentration of unreacted
ethyl acetate.We found the residence time is the same for all reactors, since the
reactors are of the same volume and volumetric flow rate is also the same for all
the reactors.
From the graph, we found that concentration of unreacted NaOH increases with
time. However, for the third reactor, the concentration first decreases then
increases. The more the unreacted NaOH, the more is the HCl consumption. The
reason can be due to deviation from ideality for various reasons.We also face
non-ideality in CSTRs. While they are known to be perfect mixing reactors, there
are formation of dead zones, where mixing doesn’t take place.
CSTRs have various applications and advantages.
High temperature reactions are carried out in CSTRs. PFRs are avoided in
exothermic reactions due to the formation of hotspots. CSTRs ​are most commonly
used in industrial processing, primarily in homogeneous liquid-phase flow
reactions, where constant agitation is required.
PFR has a higher theoretical efficiency than a CSTR of the same volume. That is,
given the same space-time (or residence time), a reaction will proceed to a higher
percentage completion in a PFR than in a CSTR.
CSTRs are also easy to construct as well.

4. ADITYA GOEL: ​In this experiment, we studied a cascade of 3 CSTRs in series.


We take a cascade of CSTRs in series as a number of CSTRs in series approaches
towards a PFR, which has high conversion per unit volume. These reactors consist
of agitators to ensure proper mixing of the reaction mixture, but there is a
formation of ​dead zones at the bottom of the reactor​ giving unreacted mixture.
This is one of the non-ideality in CSTRs and is the reason why we discard 50 mL
of the reaction mixture from each reactor before taking the 10 mL sample for
titration.

The reaction carried out is a saponification reaction, which is the base hydrolysis
of a fatty acid or oil to give soap( in this case ​CH​3​COONa)​ and alcohol( in this case
C​2​H​5​OH)​ as a by-product. It is used in herbicides, manufacture of soap, chemical
based fire extinguishers etc.Saponification reaction is a ​bimolecular second order
reaction​ which means that it is first order with respect to both A( in this case
NaOH) and B(in this case ethyl acetate) while it is second order overall. Hence,
the reaction rate can be represented as:
-r​A​=kC​A​C​B

From the observation table we see that the v​olume of NaOH required for
titration decreases with increasing residence time​. This implies that as the
residence time increases, the volume of HCl left unreacted after neutralisation of
unreacted NaOH from reaction mixture decreases, which implies that as residence
time increases, less and less NaOH reacts under steady state. ​This trend should
not be observed​ since the reactor should attain steady state after such a long time
and as time given for the reactants to react increases, more and more NaOH should
be consumed, leading to less HCl required for neutralisation and more NaOH
required for this unreacted HCl.

CSTRs find a lot of ​applications ​in chemical engineering. It can be used for:
1. Biogas production
2. Fermentation
3. As loop reactor for pharmaceutical production
In environmental engineering in:
1. Anaerobic digesters for stabilization of wastewater biosolids
2. Lagoon treatment systems for natural wastewater treatment
3. Activated sludge process for wastewater treatment.

CSTRs have some major ​advantages ​over PFR like Good temperature control,
low operating cost, they are simple to clean, they can adapt to two phase runs etc.

They have certain ​disadvantages ​too like they have low conversion per unit
volume, there is formation of dead zones where no mixing occurs, very large
reactors are required for high conversions, there is by-passing and channeling with
poor agitation.

5. GANESH BHARATWAJ: ​In this experiment we studied the performance of


three CSTRs in series. The reaction was a saponification reaction, the same as the
reaction in the case of the P1 experiment.
The reaction is first order with respect to the individual reactants since the reactor
was fed with equal reactants if A and B. The overall reaction is second order.
In this experiment we found the value of the rate constant analytically, instead of
using graphical methods.
From the graph plotted for concentration vs time, we can see that the volume of
NaOH required for titration decreases with increasing residence time. This is
because more HCl is consumed with increasing time. However, the trend shown in
the graph should not be the trend desired as we expect the increase to be steady, a
straight line trend.
Advantages of CSTR include:
1. Continuous operation
2. Good temperature control
3. Low operating cost
4. Easy to clean
5. Simplicity of construction
Disadvantages of CSTR include:
1. Lowest conversion per unit volume
2. Very large reactors needed to obtain high conversion
3. Dead zones can develop, where no mixing occurs
4. By-passing and channeling is also possible if agitation is poor.
Some applications of CSTR are:
1. In Chemical Engineering: Biogas production, fermentation, as a loop
reactor for pharmaceutical production.
2. In Environmental Engineering: For wastewater treatment, such as lagoon
treatment and activated sludge process, and as anaerobic digesters for the
stabilization of wastewater biosolids.

CONCLUSION

The saponification reaction carried out in this experiment is a bimolecular second order
reaction. The average value of k is obtained to be 23.36463 l/g-min.mol for the reaction.

REFERENCES

1. H. Scott Fogler “ Elements of Chemical Reaction Engineering” 4th Edition


2. Octave Levenspiel “Chemical Reaction Engineering “ 3rd ed, Wiley, NY, 2001
3. P2 lab presentation slides
4. P2 lab manual

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