Manipal University

Department of Chemical Engineering

CE 1732- CHEMICAL REACTION ENGINEERING LAB

IV YEAR, 7TH SEMESTER, 2019

EXPERIMENT #3

Combination of Reactors

INSTRUCTOR:

Ir. Nandana Chakinala

Dr. Gaurav Kataria

GROUP #1
MEMBER: Tanima Sharma (169102024)

Experiment carried on: August 23, 2019

Report submitted on : August 30, 2019

PRELAB (10) ______

EXECUTIVE SUMMARY (10) ______
INTRODUCTION/OBJECTIVES/SCOPE/PROCEDURE (30) ______
RESULTS & DISCUSSION (30) ______
a) Data analysis and interpretation of information
b) Presentation of relevant information (including results
on graphical, tabular or equation forms)
CONCLUSIONS (5) ______
REFERENCES (5) ______
APPENDIX
a) Original data, sample calculations, Excel sheets (5) ______
GENERAL COMPLETENESS
a) Conciseness and neatness (5) ______

TOTAL (100) ______

Nomenclature

CSTR Continuous stirred tank reactor

PFR Plug flow reactor

MFR Mixed Flow reactor

Chemicals

𝐶2 𝐻5 𝑂𝐻 Ethanol

𝐶𝐻3 𝐶𝑂𝑂𝐶2 𝐻5 / E.A. Ethyl acetate

𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 Sodium acetate

H2O Water

HCl Hydrochloric acid

NaCl Sodium Chloride

NaOH Sodium Hydroxide

 Table of Contents
Nomenclature .....................................................................................................................................2
Chemicals ..........................................................................................................................................2
List of Figures ....................................................................................................................................3
List of Tables .....................................................................................................................................3
Executive Summary: ..........................................................................................................................4
Introduction:.......................................................................................................................................5
Experimental Setup: ...........................................................................................................................7
Materials Used: ..................................................................................................................................7
Procedure: ..........................................................................................................................................8
Preparing solutions: ........................................................................................................................8
Standardization of NaOH: ..............................................................................................................8
Experiment procedure: ...................................................................................................................8
Results and Discussions: ....................................................................................................................9
Conclusion: ...................................................................................................................................... 10
References: ...................................................................................................................................... 10
Appendix: ........................................................................................................................................ 11
A.1 Observation Tables ................................................................................................................ 11
A.2 Data required for Calculations ............................................................................................... 13
A.3 Sample Calculations .............................................................................................................. 13
A.4 Calculated Data ..................................................................................................................... 15

List of Figures
Figure 1:Combination of Reactors apparatus. ....................................................................................7
Figure 2: Effect of time on conversion for flowrate of 2.6 LPH ..........................................................9
Figure 3: Effect of time on conversion for flowrate of 5.4 LPH ........................................................ 10

List of Tables
Table 1. Standardization of NaOH .................................................................................................... 11
Table 2. Observation table for flowrate of 2.6 LPH .......................................................................... 11
Table 3. Observation table for flowrate of 5.4 LPH .......................................................................... 12
Table 4. Data required for calculations ............................................................................................. 13
Table 5. Calculated data for flowrate = 2.6 LPH ............................................................................... 15
Table 6. Calculated data for flowrate = 5.4 LPH ............................................................................... 16
Executive Summary:
The objective of the experiment was to study the non-catalytic homogeneous reaction between
NaOH and CH3COOC2H5 in a combination of reactors with a Plug Flow Reactor followed by a
CSTR. The experiment was performed at two different flowrates (2.6 LPH and 5.4 LPH). The
conversions obtained were 94%, and 93.6% at a flowrate of 2.6, and 5.4 LPH respectively. Thus,
the conversion slightly decreased with an increase in the flowrate. There was no trend observed in
change of conversion with time. This could be because of various errors while performing the
experiment, one of the major error being that the normality of NaOH and ethyl acetate taken was
too high. Because of these high normality, the conversion had reached its final value before the first
reading was taken and hence, was running in steady state for the complete duration of the
experiment.
Introduction:
In any chemical industry, reactors are the most important equipment used to carry out a specific
reaction in which a desired product is created from raw materials. There are three major types of
reactors used in industries, these are: i) batch reactor, ii) continuous stirred tank reactors (CSTR)
and, iii) plug flow reactors (PFR).

A PFR or an ideal tubular reactor is a long, straight, pipe-shaped tank in which the reactive fluid
transits at steady state (no accumulation). In a PFR, the concentration of the reactant changes from
point to point in the direction of the flow [1]. It is the opposite of the CSTR, where the reaction
mixture is perfectly mixed. The contents in a CSTR are continuously stirred, so the concentration
remains same throughout the reactor [1]. In some cases, for maximizing the conversion, multiple
reactors are used in series.

For the most effective use of a given set of ideal reactors we have the following general rules [1]:

1. For a reaction whose rate-concentration curve rises monotonically (any nth-order reaction,
n>0) the reactors should be connected in series. They should be ordered so as to keep the
concentration of reactant as high as possible if the rate-concentration curve is concave (n > I),
and as low as possible if the curve is convex (n < 1).
2. For reactions where the rate-concentration curve passes through a maximum or minimum the
arrangement of units depends on the actual shape of curve, the conversion level desired, and the
units available. No simple rules can be suggested.
3. Whatever may be the kinetics and the reactor system, an examination of the 1/(-rA) vs. CA
curve is a good way to find the best arrangement of units.

In this experiment a combination of plug flow reactor (PFR) followed by a continuously stirred tank
reactor (CSTR) is used. For this system, we may write the performance equations as:

For PFR:
𝑋1
𝑉1 𝑑𝑋
= ∫ (1)
𝐹0 (−𝑟)1
𝑋0

The outlet conversion from PFR is the inlet conversion to CSTR. Therefore, we can write,

For CSTR:
𝑉2 𝑋2 − 𝑋1
= (2)
𝐹0 (−𝑟)2
Where,

V1 is the volume of first reactor (PFR)

V2 is the volume of second reactor (CSTR)
F0 is the molar flowrate through both the reactors
X0 is the initial conversion before entering PFR (in this case X0 = 0)
X1 is the conversion of the stream coming out of PFR and entering the CSTR
X2 is the final conversion attained after the CSTR
(-r) is the rate equation for the reaction taking place

The reaction which is to be carried out in this experiment is between sodium hydroxide, NaOH and
ethyl acetate, Et(AC). It is a second order saponification reaction as per literature [2], and is given
as:

𝐶𝐻3𝐶𝑂𝑂𝐶2𝐻5+𝑁𝑎𝑂𝐻→𝐶𝐻3𝐶𝑂𝑂𝑁𝑎+𝐶2𝐻5𝑂𝐻 (3)

Since, while performing the reaction we take equal normality of 𝑁𝑎𝑂𝐻 and 𝐶𝐻3𝐶𝑂𝑂𝐶2𝐻5 solution
and maintain equal volumetric flowrates, the molar flowrate of NaOH becomes quite high as
compared to that of 𝐶𝐻3𝐶𝑂𝑂𝐶2𝐻5. Due to this difference between the molar flowrates we can
consider the reaction to be a pseudo first order reaction.

At the end of the reaction in equation (3), the product stream is collected. Before analyzing this
stream, the ongoing reaction has to be killed using HCl. This happens by the occurrence of the
following reaction:

𝑁𝑎𝑂𝐻 + 𝐻𝐶𝑙 → 𝑁𝑎𝐶𝑙 + 𝐻2 𝑂 (4)

After adding HCl, the mixture is titrated using NaOH, to find the amount of unreacted HCl. This in
turn gives the amount of NaOH is left after the reaction has taken place. Using this unreacted amount
of NaOH and the amount of NaOH initially taken, we can find the conversion.

The conversion can be calculated using:

𝐶𝐴
𝑋𝐴 = 1 − (5)
𝐶𝐴0

The aim of this experiment was to study the non-catalytic homogenous reaction of NaOH and
ethyl acetate in a series of reactors i.e. a PRF followed by a CSTR (or MFR).
 Experimental Setup:
Figure 2 shows the experimental setup for combination of reactors experiment. It consists of two
feed tanks, one for sodium hydroxide and one for ethyl acetate. The storage tanks are connected with
individual rotameters to adjust the flowrates. There are two reactors in series, PFR followed by a
CSTR. The reactants first enter the PFR followed by the CSTR provided with stirrers to continuously
stir the reactant contents. A drain valve is provided to collect the final product mixture.

Figure 1:Combination of Reactors apparatus.

Materials Used:
 2 L of 0.05 N solution of HCl
 15 L of 0.1135 N solution of E.A.
 15 L of 0.1135 N solution of NaOH
Procedure:
Preparing solutions:
1. For making 0.1135N solution of ethyl acetate (Mw = 88) mix 150 g of ethyl acetate in 15 L of
water.
2. For making 0.05 N of HCL (Mw = 36.5) mix 8.334 ml of 37 wt% in 2L of water.
3. For making 0.1135 N NaOH (Mw = 40) mix 60 g of NaOH pellets in 15 L water.
(Please refer to appendix A.3 for calculations of standardization and solution preparation)

Standardization of NaOH:
1. NaOH is standardized using HCl. This is required because NaOH is hygroscopic in nature.
2. Fill the HCl in the burette up to the 0 level mark.
3. Take 10mL of NaOH in a conical flask
4. Add 2 drops of phenolphthalein indicator to it.
5. Add the HCl from the burette drop by drop into the conical flask until end point is reached i.e.
the pink color disappears.
6. Note down the volume of HCl consumed.
7. Repeat the steps 3-4 times to get accurate results.
8. Apply N1V1 = N2V2 to find the normality of NaOH
Here,
N1 = normality of HCl (0.05N)
N2 = normality of NaOH to be calculated
V1 = volume of HCl consumed in titration in ml
V2 = volume of NaOH in ml

Experiment procedure:
1. Ensure all the valves are closed.
2. Calibrate the rotameters.
3. Fill the feed tanks with 15L of NaOH in one of the tanks and 15L of ethyl acetate in another.
4. Set equal flowrates of both the reactants using rotameters provided.
5. Remove all the air bubbles in the pipe.
6. Take 10ml of sample from both the reactors after every 10min until steady state is reached
7. Add 20 ml HCl to it, in order to kill the reaction.
8. Titrate the solution against 0.1135 N NaOH in sets of three mixtures of 10ml each.
9. Note the amount of NaOH consumed.
10. Repeat steps 3-12 at two different flowrates.
11. Apply N3V3= N4V4 to find the volume of HCl remaining in the mixture
Here,
N3 = normality of NaOH (0.1135N)
N4 = normality of HCl (0.05 N)
V3 = volume of NaOH consumed in titration in ml
V4 = volume of HCl to be calculated in ml
12. Repeat the above steps for another flowrate
Results and Discussions:
The calculated results of the experiment are shown in Table 6, and 7 of the Appendix. The
calculations were performed as shown in Appendix A.3. The results are graphically represented in
Figure 2 and 3.

Figure 2 and 3 show the effect of time on the conversion of NaOH. The conversion should increase
with time, but from the graphs we can see that there is no particular trend of change in conversion
with increase in time for both flowrates. Since, the system is a PFR followed by a CSTR, the
conversion at the end of CSTR should be more than the conversion at the end of PFR. We can see
from the graphs that this is true, except for a few anomalies.

We know that on increasing flowrate, the residence time in the reactor increases because of which
the reactants get enough time to react and hence, the conversion should increase. From the results
in the Appendix, we can see that there is a slight decrease in conversion with an increase in flowrate
but the change is insignificant.

Also, we can see that the reaction has reached a very value of conversion at initial time only, i.e. at
the first reading taken at 10 minutes. This could be a reason why there is no particular trend in the
graphs. All these errors in results show that there were great experimental errors involved with it. A
plausible reason for this could be that the normality of NaOH and ethyl acetate taken were too high.
Because of these high concentrations, there was a very fast conversion at the operating flowrates.
The reactions were probably complete even before the first set of readings was taken and hence, the
results show no trend with change in flowrate or time.

Time vs Conversion for 2.6 LPH

0.98

0.97

0.96

0.95
Conversion

0.94

0.93

0.92

0.91

0.9
0 10 20 30 40 50 60
Time

PFR CSTR

Figure 2: Effect of time on conversion for flowrate of 2.6 LPH

 Time vs Conversion for 5.4 LPH
0.98

0.97

0.96
Conversion

0.95

0.94

0.93

0.92

0.91

0.9
0 5 10 15 20 25 30 35 40 45
Time

PFR CSTR

Figure 3: Effect of time on conversion for flowrate of 5.4 LPH

Conclusion:
The objective of this experiment is to study the kinetics of non-catalytic homogeneous reaction
between sodium hydroxide and ethyl acetate in a combination of plug flow reactor followed by a
CSTR. We concluded from the results that there was no apparent change observed in the conversion
with increase in flowrate or time. All these results are inaccurate as the conversion should ideally
increase with time and decrease with increasing flowrate. It was concluded that the results obtained
had errors because the experiment was performed with too high concentrations of reactants. At these
concentrations the reaction had taken place before taking the first reading and hence, the further
obtained results were inaccurate and insignificant.

References:
[1] O. Levenspiel, “Chemical Reaction Engineering” 3rd edition, John Wiley and Sons, 2016, p.
319-421.
[2] A. Mukhtar, U. Shafiq, Q. Omar, H. Abdul Qadir, M. Qizilbash, and B. Ahmed Awan, “Kinetics
of Alkaline Hydrolysis of Ethyl Acetate by Conductometric Measurement Approach Over
Temperature Ranges (298.15-343.15K),” Austin Chem. Eng., vol. 4, p. 1046, 2017.
Appendix:
A.1 Observation Tables

Table 1. Standardizat ion of NaOH

Volume of NaOH titrated Volume of HCl
Sr. No.
(ml) (ml)
1 10 22.3
2 10 23.2
3 10 22.8
22.7

Table 2. Observat ion table for flowrate of 2.6 LPH

Sample Volume Volume of HCl Sample Volume Volume of NaOH

Sr.No. Time Reactor
(ml) added (ml) Titrated (ml) consumed (ml)

1 10 1.5
2 PFR 10 20 10 1.4
3 10 1.6
10
4 10 1.8
5 CSTR 10 20 10 1.5
6 10 1.5
10 10 1.6
11 PFR 10 20 10 1.6
12 10 1.6
20
13 10 1.5
14 CSTR 10 20 10 1.5
15 10 1.6
19 10 1.1
20 PFR 10 20 10 1.2
21 10 1.5
30
22 10 1.5
23 CSTR 10 20 10 1.8
24 10 1.5
28 10 1.5
29 PFR 10 20 10 1.7
30 10 1.8
40
31 10 1.6
32 CSTR 10 20 10 1.7
33 10 1.7
 37 10 1.4
38 PFR 10 20 10 1.5
39 10 1.4
50
40 10 1.5
41 CSTR 10 20 10 1.7
42 10 1.6
37 10 1.5
38 PFR 10 20 10 1.6
39 10 1.8
60
40 10 1.7
41 CSTR 10 20 10 1.5
42 10 1.5

Table 3. Observat ion table for flowrate of 5.4 LPH

Sample
Sr. Sample Volume Volume of HCl Volume of NaOH
Time Reactor Volume
No. (ml) added (ml) consumed (ml)
Titrated (ml)
1 10 1.4
2 PFR 10 20 10 1.4
3 10 1.6
10
4 10 1.6
5 CSTR 10 20 10 1.5
6 10 1.5
10 10 1.4
11 PFR 10 20 10 1.6
12 10 1.6
20
13 10 1.5
14 CSTR 10 20 10 1.5
15 10 1.6
19 10 1.2
20 PFR 10 20 10 1.1
21 10 1.1
30
22 10 1.7
23 CSTR 10 20 10 1.6
24 10 1.5
28 10 1.2
29 PFR 10 20 10 1.5
30 10 1.4
40
31 10 1.4
32 CSTR 10 20 10 1.5
33 10 1.7
 A.2 Data required for Calculations

Table 4. Data required for calculat ions

Density of HCl 1.18 g/ml
Normality of HCl 0.05 N
Normality of EA 0.1135 N
Normality of NaOH 0.1135 N
Initial Moles of NaOH 1.7025 moles

A.3 Sample Calculations

Preparation of HCl for standardization of NaOH and for killing the reaction

Normality of HCl required = 0.05 N

Therefore, moles of HCl to be added in 2 L water = 0.1 moles
Molecular mass of HCl = 36.5 g / mole
Available HCl is 37 wt. % in water
0.1 moles ∗36.5 g/mole
Therefore, mass of HCl to be added in 2 L water = = 9.85 gm
0.37

Density of HCl = 1.18 g/ml

Hence, volume of HCl to be added in 2 L water to make 0.05 N solution =

9.85 g
= 8.3334 ml
1.18 g/ml

Calculations for standardization of NaOH

We added 0.2 g of NaOH in 50 ml and titrated 10 ml of this solution with 0.05 N HCl obtained using
above steps

N1 = normality of HCl (0.05N)

N2 = normality of NaOH to be calculated
V1 = volume of HCl consumed in titration in ml
V2 = volume of NaOH in ml

Using N1V1 = N2V2, we get

N2= N1V1 / V2
= 0.05 N*22.7 ml / 10 ml
= 0.1135 N – Normality of NaOH obtained after standardization
Preparation of NaOH for Reaction

As shown above we got NaOH to be 0.1135 N on adding 0.2 gm in 50 ml.

So, for making 15 L of 0.1135 N NaOH, we need: 0.2 g in 50 ml

X g in 15 L

X= 0.2*15000/50 = 60 gm

Preparation of Ethyl Acetate for Reaction

Normality of E.A. required = 0.1135 N

Therefore, moles of E.A. to be added in 15 L water 1.7025 moles
Molecular mass of E.A. = 88.11 g / mole
Therefore, mass of E.A. to be added in 15 L water = 1.7025 moles * 88.11 g / mole = 150 gm

Calculations to find conversion

N1 = Normality of NaOH = 0.1135 N

V1 = Volume of NaOH consumed in titration = 1.5 ml
N2 = Normality of HCl = 0.05 N
V2 = Volume of HCl remaining in the reaction mixture after killing the reaction = ?

Using N1V1 = N2V2, we get

V2= N1V1 / N2
= 0.1135 N*1.5 ml / 0.05 N
= 3.405 ml

Volume of HCl added in each titration sample = 20/3 ml = 6.667 ml

Therefore, Volume of HCl consumed to kill the reaction = 6.667 – 3.405 ml = 3.262 ml
Density of HCl = 1.18 gm / ml
Mass of HCl consumed to kill the reaction = Volume * Density = 3.262 ml * 1.18 gm / ml
= 3.84916 gm
Molecular mass of HCl = 36.5 moles/ gm
Therefore, moles of HCl consumed to kill the reaction = mass / molecular mass = 3.84916/ 36.5
= 0.10545 moles
From the reaction stoichiometry in equation (4), we can say that the moles of HCl used to kill the
reaction is equal to the moles of NaOH left unreacted. Hence, moles of unconverted NaOH =
0.10545 moles
Initial moles of NaOH = 1.7025 moles
(initial moles of NaOH – unconverted moles of NaOH)
From equation (5), we know conversion =
𝑖𝑛𝑖𝑖𝑎𝑙 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑁𝑎𝑂𝐻

(1.7025– 0.10545)
= = 0.938
1.7025
 A.4 Calculated Data

Table 5. Calculated data for flowrate = 2.6 LPH

Titration HCl consumed to kill the Moles of Initial

Sr.No. Time Reactor volume of reaction unreacted Moles of Conversion
HCl Volume (ml) Moles NaOH NaOH

1 3.405 3.262 0.105 0.105 1.703 0.938

2 PFR 3.178 3.489 0.113 0.113 1.703 0.934 0.938
3 3.632 3.035 0.098 0.098 1.703 0.942
10 0.940
4 4.086 2.581 0.083 0.083 1.703 0.951
5 CSTR 3.405 3.262 0.105 0.105 1.703 0.938 0.942
6 3.405 3.262 0.105 0.105 1.703 0.938
10 3.632 3.035 0.098 0.098 1.703 0.942
11 PFR 3.632 3.035 0.098 0.098 1.703 0.942 0.942
12 3.632 3.035 0.098 0.098 1.703 0.942
20 0.941
13 3.405 3.262 0.105 0.105 1.703 0.938
14 CSTR 3.405 3.262 0.105 0.105 1.703 0.938 0.940
15 3.632 3.035 0.098 0.098 1.703 0.942
19 2.497 4.170 0.135 0.135 1.703 0.921
20 PFR 2.724 3.943 0.127 0.127 1.703 0.925 0.928
21 3.405 3.262 0.105 0.105 1.703 0.938
30 0.935
22 3.405 3.262 0.105 0.105 1.703 0.938
23 CSTR 4.086 2.581 0.083 0.083 1.703 0.951 0.942
24 3.405 3.262 0.105 0.105 1.703 0.938
28 3.405 3.262 0.105 0.105 1.703 0.938
29 PFR 3.859 2.808 0.091 0.091 1.703 0.947 0.945
30 4.086 2.581 0.083 0.083 1.703 0.951
40 0.945
31 3.632 3.035 0.098 0.098 1.703 0.942
32 CSTR 3.859 2.808 0.091 0.091 1.703 0.947 0.945
33 3.859 2.808 0.091 0.091 1.703 0.947
37 3.178 3.489 0.113 0.113 1.703 0.934
38 PFR 3.405 3.262 0.105 0.105 1.703 0.938 0.935
39 3.178 3.489 0.113 0.113 1.703 0.934
50 0.939
40 3.405 3.262 0.105 0.105 1.703 0.938
41 CSTR 3.859 2.808 0.091 0.091 1.703 0.947 0.942
42 3.632 3.035 0.098 0.098 1.703 0.942
37 3.405 3.262 0.105 0.105 1.703 0.938
38 PFR 3.632 3.035 0.098 0.098 1.703 0.942 0.944
39 4.086 2.581 0.083 0.083 1.703 0.951
60 0.942
40 3.859 2.808 0.091 0.091 1.703 0.947
41 CSTR 3.405 3.262 0.105 0.105 1.703 0.938 0.941
42 3.405 3.262 0.105 0.105 1.703 0.938
Table 6. Calculated data for flowrate = 5.4 LPH

Titration HCl consumed to kill the Moles of Initial

Sr. No. Time Reactor volume of reaction unreacted Moles of Conversion
HCl Volume (ml) Moles NaOH NaOH

1 3.178 3.489 0.113 0.113 1.703 0.934

2 PFR 3.178 3.489 0.113 0.113 1.703 0.934 0.937
3 3.632 3.035 0.098 0.098 1.703 0.942
10 0.938
4 3.632 3.035 0.098 0.098 1.703 0.942
5 CSTR 3.405 3.262 0.105 0.105 1.703 0.938 0.940
6 3.405 3.262 0.105 0.105 1.703 0.938
10 3.178 3.489 0.113 0.113 1.703 0.934
11 PFR 3.632 3.035 0.098 0.098 1.703 0.942 0.940
12 3.632 3.035 0.098 0.098 1.703 0.942
20 0.940
13 3.405 3.262 0.105 0.105 1.703 0.938
14 CSTR 3.405 3.262 0.105 0.105 1.703 0.938 0.940
15 3.632 3.035 0.098 0.098 1.703 0.942
19 2.724 3.943 0.127 0.127 1.703 0.925
20 PFR 2.497 4.170 0.135 0.135 1.703 0.921 0.922
21 2.497 4.170 0.135 0.135 1.703 0.921
30 0.932
22 3.859 2.808 0.091 0.091 1.703 0.947
23 CSTR 3.632 3.035 0.098 0.098 1.703 0.942 0.942
24 3.405 3.262 0.105 0.105 1.703 0.938
28 2.724 3.943 0.127 0.127 1.703 0.925
29 PFR 3.405 3.262 0.105 0.105 1.703 0.938 0.932
30 3.178 3.489 0.113 0.113 1.703 0.934
40 0.936
31 3.178 3.489 0.113 0.113 1.703 0.934
32 CSTR 3.405 3.262 0.105 0.105 1.703 0.938 0.940
33 3.859 2.808 0.091 0.091 1.703 0.947