MANIPAL UNIVERSITY

DEPARTMENT OF CHEMICAL ENGINEERING

CE 1732- CHEMICAL REACTION ENGINEERING LAB

IV YEAR, 7TH SEMESTER, 2019

EXPERIMENT #10

Study of a non-catalytic homogenous reaction in a Plug Flow Reactor

INSTRUCTOR:

Ir. Nandana Chakinala

Dr. Gaurav Kataria

GROUP #4

MEMBERS: SAHIL AGRAWAL (169102022)

MUKUND SAI TEJA

AKASH

Experiment carried on: October 18, 2019

Report submitted on: November 01, 2019
PRELAB (10) ______
EXECUTIVE SUMMARY (10) ______
INTRODUCTION/OBJECTIVES/SCOPE/PROCEDURE (30) ______
RESULTS & DISCUSSION (30) ______
CONCLUSIONS (5) ______
REFERENCES (5) ______
APPENDIX
a) Original data, sample calculations, other information (5) ______
GENERAL COMPLETENESS
a) Conciseness and neatness (5) ______
TOTAL (100) _____

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Contents
EXECUTIVE SUMMARY………………………………………………………………………… 3
AIM………………………………………………………………………………………………….4
INTRODUCTION………………………………………………………………………………….. 4
PROCEDURE……………………………………………………………………………………… 5
EXPERIMENTAL SETUP………………………………………………………………………….5
RESULT & DISCUSSION………………………………………………………………………….6
CONCLUSION …………………………………………………………………………………………………………………………….7
PRECAUTIONS……………………………………………………………………………………. 7
REFERENCES……………………………………………………………………………………... 8
OBSERVATION TABLE………………………………………………………………………….. 9

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EXECUTIVE SUMMARY

The main objective of this experiment to study the kinetics of non-catalytic homogeneous
reaction between sodium hydroxide and ethyl acetate in a plug flow reactor and to determine
the order of reaction and rate constant was achieved by performing a second order
bimolecular reaction of NaOH and ethyl acetate to give sodium acetate and ethanol in a plug
flow reactor at different flowrates of both ethyl acetate and NaOH. This reaction was carried
between 0.01N solutions of both the reactants and the outlet samples for the reactor were
collected at 0,1,3 mins and every 5 mins were titrated by initially adding 0.05N HCl to stop
the reaction and then titrating against NaOH solution using phenolphthalein as an indicator.
The conversion values for the experiment at the feed rate of 2600 and 3800 ml/hr ranges
between 99-97% and 97-99%, where due to some genuine faults the conversion values is in
the first flowrate is decreasing & then increasing.

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AIM
To study the non-catalytic homogenous saponification reaction in a plug flow reactor and
calculate (i) order of the reaction, (ii) rate constant and (iii) activation energy.

INTRODUCTION
Tubular reactors are a type of flow reactors. These have continuous inflow and outflow of
materials. In this type of reactor, feed enters at one end of cylindrical tube and the product
leaves from the other end. There is radial mixing taking place inside the tubes. This mixing
results in continuous change of properties of the flowing streams along the length of the
reactor. Mass balance for a plug flow reactor over a small element is given as follows
Input=Output + disappearance by reaction+ accumulation
F A=F A + d F A + (−r A ) dV … … … ..(2.1)
d F A =d [ F A 0 ( 1−X A ) ]=−F A 0 d X A … … ..(2.2)
XA
τ v d XA
= =∫ … … … … … ( 2.2 )
C A 0 F A 0 0 −r A
Equation 2.2 is known as the performance equation which interrelates the feed flow rate, the
reactor volume and the rate of reaction. In this saponification reaction, Ethyl acetate is the
limiting reagent. The reaction taking place is given as follow:
C H 3 COOC 2 H 5 + NaOH → C H 3 COONa +C2 H 5 OH
dCA
−r A = … … … … … … .. ( 2.3 )
dt
−r A =k C aA CbB … … … … … .(2.4)
where,
NA = moles of reactant at time t, moles
CA = concentration of A at any time t in the reactor, mol/lit
V = Volume of the reactor, lit
-rA = rate of reaction, (units depend on the order of the reaction)
k = rate constant, CA1-nsec-1
t = time of reaction, sec
−r A =k C 2A 0 ( 1−X A ) ( M −X A ) … … ( 2.5 )
CB0
M=
CA 0
Substituting equation 2.5 in equation 2.2 and integrating we get, for M>1,
1 M− X A
C A 0 ( M −1 ) [
ln
M ( 1− X A )]=kτ … … … … ( 2.6 )

For M=1,
XA
=kτ … … … … … … … … … … … … .. ( 2.7 )
1−X A

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 In an ideal plug flow reactor, there is only radial mixing and no axial mixing and a
uniform velocity profile across the radius is maintained. The plug flow reactor is
characterized by the fact that the elements of the reactor do not mix with any other
element.

PROCEDURE
Preparation of solution
Ethyl acetate: To prepare 20L of 0.01N of ethyl acetate add 17.622g of it to 20 L of water.
Sodium hydroxide: To prepare 20L of 0.01N NaOH add 8.04g of NaOH.
Hydrochloric acid: 37.5 wt% HCL was provided. To make 2L 0.05N HCl add 8.33ml of 37.5
wt% HCL to 2L of water.

Standardization
Standardization of HCl
 HCl is standardized using sodium carbonate of 0.01N.
 Fill the sodium carbonate in the burette upto the 0 level mark.
 Take 10mL of HCl in a conical flask
 Add 2 drops of phenolphthalein indicator to it.
 Pour the Sodium carbonate from the burette drop by drop into the round bottom flask
until end point is reached.
 Note down the volume if sodium carbonate consumed.
 Repeat the steps 3-4 times to get accurate results.

Start
1. The flow rates of reactants from both the tanks are to be fixed to 700 mph using the
rotameter at equal flow rates and the temperature is to be maintained at room temperature
2. Once steady state is achieved in 20-25 min, take 10 mL sample of reaction mixture from
the outlet of PFR.
3. The sample is to be added immediately after withdrawal into 20 mL 0.065N HCl kept in a
conical flask.
4. Take 10 mL of liquid from the conical flask and titrate it against 0.025N NaOH using
phenolphthalein as indicator.
5. Repeat the same procedure (3-6) for flowrates 1400, 2600, 5400 mph of sodium
hydroxide and ethyl acetate.

Shut Down

1. After nothing down the readings let the feed tanks drain till they are completely empty.
2. Clean the feed tanks if any film of reactants remain on the walls of the reactor.

EXPERIMENTAL SETUP

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The experimental setup was provided by Lelesil Innovative System. The setup consist of two
feed tanks to supply the sodium hydroxide and ethyl acetate solutions. The temperature of the
tanks is maintained at room temperature. Two rotameters are connected to the feed tank pipes
to control the flowrates of solutions. A single PFR is connected to the feed tanks. The plug
flow reactor has a tubular arrangement inside the tank filled with water to provide heating
mechanism. There is one valve connected to the plug flow reactor to collect the outlet
sample. A control panel is provided to turn the apparatus ON/OFF and to maintain the
temperature.

Figure 1: Experimental setup of plug flow reactor.

RESULT & DISCUSSION

The aim of this experiment was achieved by performing a second order bimolecular reaction
of NaOH and ethyl acetate to give sodium acetate and ethanol in a plug flow reactor at
different flowrates of both ethyl acetate and NaOH. This reaction was carried between 0.01N

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solutions of both the reactants and the outlet samples for the reactor were collected at 0,1,3 &
every 5 mins and were titrated by initially adding 0.05N HCl to stop the reaction and then
titrating against NaOH solution using phenolphthalein as an indicator.
The outlet concentrations from the plug flow reactor were determined by titrations and
further calculations at the feed rate of 2600 and 3800 ml/hr in which the conversion values
ranged between 99-97% and 97-99% and the conversion vs time data was extracted.
For the flowrate 2600 mlph, the conversion was decreasing from 99.223% to 96.116% and
then increased from 96.116% to 97.605%. This error is occurred due to present of some
amount of the older solution in the reactor.
For flowrate 3800 mlph , The conversion is ranging from 97.217% to 99.806%, which is
correct as in a PFR the conversion will increase with time.

CONCLUSION

From the above experiment it can be concluded that due to some genuine faults, the
experiment data wasn’t extracted precisely which led to some error in the conversion. Non
catalytic homogenous reaction of NaOH and ethyl acetate was analyzed in a Plug Flow. The
conversion obtained for the flowrate of 2600 mlph was 99.223 – 97.605% and for the
flowrate of 3800 mlph it was 97.214 -99.806 %.

PRECAUTIONS
1. Ensure that the reading taken should be with less error.
2. Take safety measures while performing the experiment as per the MSDS.
3. Always wear safety gears with full cover shoes while doing experiment.

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REFERENCES
1. O. Levinspiele, “Chemical Reaction Engineering” 2nd edition, John Wiley and Sons,
2007, 319-421
2. Perry's Chemical Engineers' Handbook. New York :McGraw-Hill, 1984.
3. H. Scott Fogler, ‘Elements of Chemical Engineering’, Fourth Edition, Pearson
International Edition, 2006.

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APPENDIX

OBSERVATION TABLE
Table1: Experimental data for flowrate 1

Vol. of Vol. of
solution NaOH
taken consumed
Time(min) (ml) (ml)
0 10 32.1
1 10 30.6
3 10 29.7
5 10 28.7
10 10 27.3
15 10 29.1
20 10 29.4
25 10 29.6

Table 2: Calculated data for flowrate 1

Vol. of HCl HCl Moles of

remaining remaining HCl Initial Conversion
(ml) (g) remaining moles Conversion (%)
0.24 0.2832 0.008 1 0.992 99.223
0.54 0.6372 0.017 1 0.983 98.252
0.72 0.8496 0.023 1 0.977 97.670
0.92 1.0856 0.030 1 0.970 97.022
1.2 1.416 0.039 1 0.961 96.116
0.84 0.9912 0.027 1 0.973 97.281
0.78 0.9204 0.025 1 0.975 97.476
0.74 0.8732 0.024 1 0.976 97.605

Table 3: Experimental data for flowrate 2

Time(min) Vol. of Vol. of

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 solution NaOH
taken consumed
(ml) (ml)
0 10 29
1 10 29.2
3 10 30.1
5 10 31.2
10 10 32.7
15 10 32.9
20 10 33

Table 4: Calculated data for flowrate 2

Vol. of
HCl HCl Moles of
remaining remaining HCl Initial Conversion
(ml) (g) remaining moles Conversion (%)
0.86 1.0148 0.028 1 0.972 97.217
0.82 0.9676 0.027 1 0.973 97.346
0.64 0.7552 0.021 1 0.979 97.929
0.42 0.4956 0.014 1 0.986 98.641
0.12 0.1416 0.004 1 0.996 99.612
0.08 0.0944 0.003 1 0.997 99.741
0.06 0.0708 0.002 1 0.998 99.806

Sample calculations: Considering Flowrate 1, for PFR at 15 minutes,

𝑁1𝑉1 = 𝑁2𝑉2,
0.01 ∗ 29.1 = 0.05 𝑉𝐻𝐶𝑙,
𝑉𝐻𝐶𝑙 = 5.82𝑚𝑙,
𝑉𝐻𝐶𝑙 = 6.66 − 5.82 = 0.84𝑚𝑙
𝐻𝐶𝑙 =0.84 ∗ 1.18 = 0.9912𝑔 𝐻𝐶𝑙
0.9912
𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝐻𝐶𝑙 CA0= =0.02712
36.5
Initial moles (CA) =1

CA−CA 0 1−0.02712
X A= = =97.28 %
CA 1

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