S.no. Name of The Experiment Date of Conduction Date of Submission P2 Cascade CSTR 4 February, 2021 9 February, 2021
S.no. Name of The Experiment Date of Conduction Date of Submission P2 Cascade CSTR 4 February, 2021 9 February, 2021
GROUP NUMBER: 9
GROUP MEMBERS:
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.
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):
-rA= k CACB
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
V1=V2=V3=V=1.2L
CA0 = CB0 = 0.25 mol/L
V(HCl) = 20ml
V(sample) = 10ml
Observation Table:
SAMPLE CALCULATIONS:
GRAPHS:
DISCUSSIONS:
In accordance with the power law model of rate law, the rate equation can be expressed as: -rA=
k CACB, 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
(CA0= CB0). 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, CA= CB. The rate law reduces to: -rA =
kCA2. 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.
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.
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.
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 CH3COONa) and alcohol( in this case
C2H5OH) 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:
-rA=kCACB
From the observation table we see that the volume 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.
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