UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

CHEMICAL ENGINEERING LABORATORY 3
CHE (574)
NAME
: NIK NUR SHAHIRA BINTI IBRAHIM (2012209148)
GROUP
: EH220(4A)
EXPERIMENT
: EXPERIMENT OF TUBULAR FLOW REACTOR BP 101
DATE PERFORMED : 18 MARCH 2014
SEMESTER
:4
PROGRAMME / CODE : CHE 574
SUBMIT TO
: DR JEFRI JAAPAR

No.
1
2
3
4
5
6
7
8
9
10
11
12
13

Title
Abstract/ Summary
Introduction
Aims
Theory
Apparatus
Methodology/ Procedure
Result
Calculations
Discussion
Conclusion
Recommendations
Reference
Appendix

TOTAL MARKS
Remarks:
Checked by:
_________________
Date:

Allocated Marks
(%)
5
5
5
5
5
10
10
20
20
10
5
5
5
100

Marks

Contents
Abstract........................................................................................................................
Introduction....................................................................................................................
Aims............................................................................................................................
Theory..........................................................................................................................
Apparatus......................................................................................................................
Procedure......................................................................................................................
Result...........................................................................................................................
Discussion.....................................................................................................................
Conclusion...................................................................................................................
Recommendations..........................................................................................................
Reference....................................................................................................................
Appendix.....................................................................................................................

Abstract

This experiment was performed to carry out saponification reaction between Sodium
Hydroxide, NaOH and Ethyl Acetate, Et(AC), to determine the effect of residence time on the
conversion in a Tubular Flow Reactor (TFR) and to determine the reaction rate constant. A
unit called SOLTEQ Plug Flow Reactor (Model: BP 101) is used in this experiment,
commonly known as PFR. The two solutions Sodium Hydroxide, NaOH and Ethyl Acetate,
Et(Ac) were reacted in the PFR and the product is then analyzed by the method of titration to
determine how did the reaction go. Thus, the experiment was carried out and the results show
that as the residence time increases, the amount of conversion of Sodium Hydroxide, NaOH
is almost unchanged.

Introduction
Chemical reactor is a place where chemical reactions take place and it is one of the
important part of any chemical process design. A reactors design must finely create to suit
the mechanism of the process to be carried out. The reactor depends on the nature of the
materials in both the feed and the products. In this experiment, the Plug Flow Reactor
(Model: BP101) is used as it has been properly designed for students' experiment on chemical
reactions in liquid phase under isothermal and adiabatic conditions. The unit also includes a
jacketed plug flow reactor; individual reactant feed tanks and pumps, temperature sensors and
conductivity measuring sensor. This specific unit enable students to conduct the typical
saponification reaction between ethyl acetate and sodium hydroxide among the others
reaction.

Aims

Theory

To carry out a saponification reaction between NaOH and Et(Ac) in a TFR.

To determine the reaction rate constant.
To determine the effect of residence time on the conversion in a TFR.

Tubular flow reactor consists of a cylindrical pipe and operated at steady state
condition. For analytical purposes, the flow in the system is considered to be highly turbulent
and may be modeled by that of a plug flow. Therefore, there is no radial variation in
concentration along the pipe. Tubular reactors are one type of flow reactors. It has continuous
input and output of materials. The feed enters at one end of a cylindrical tube and the product
stream leaves at the other end. The long tube and the lack of provision for stirring prevent
complete mixing of the fluid in the tube. Hence the properties of the flowing stream will vary
from one point to another. In an ideal tubular flow reactor, specific assumptions are made
regarding the extent of mixing:
1. No mixing in the axial direction
2. Complete mixing in the radial direction
3. A uniform velocity profile across the radius.

Rate of reaction is defined as the rate of disappearance of reactants or the rate of

formation of products. Rate of reaction shows how fast the reactants diminish or how fast the
product is formed. A reactant disappeared and a product produced when a chemical reaction
occurred. For example:
aA + bB

cC + dD

In the chemical equation above, A and B represent reactants while C and D represent
products. A and B is being disappeared and C and D is being produced. Rate of reaction of
each species corresponds respectively to their stoichiometric coefficient. The negative sign
indicates reactants and the positive sign indicates products.
r A
a

r B
b

rC
c

Rate of equation for reactant A is:

r A
k

rate constant
CA

= k CA CB

concentration of A species

CB

concentration of B species

stoichiometric coefficient of A
stoichiometric coefficient of B

rD
d

While conversion shows how many moles of products are formed for every mole of A
has consumed.
X A=

moles of A reacted
moles of A fed

Residence time is a characteristic of the mixing that occurs in the chemical reactor.
There is no axial mixing in a plug flow reactor, PFR and this omission can be seen in the
residence time. The continuous stirred tank reactor CSTR is thoroughly mixed and its
residence time is hugely different as compared to the residence time of PFR.

Apparatus

Plug Flow Reactor Model Bp101

Burette
Measuring cylinder
Beakers
pH indicator
Conical flask
0.1M Sodium Hydroxide, NaOH
0.1M Ethyl Acetate, Et(Ac)
0.1M Hydrochloric Acid, HCl
De-ionized water

Procedure
General Start-up Procedures
1. All the valves are ensured closed except V4, V8 and V17.
2. The following solutions are prepared: 20 liter of NaOH (0.1M) 20 liter of Et(Ac) (0.1M)1
liter of HCL (0.25M) for quenching
3. Feed tank B1 was filled with NaOH while feed tank B2 was filled with the Et(Ac).
4. The water jacket B4 was filled with water and pre-heater B5 was filled with clean water.
5. The power for the control panel was turned on.

6. Valves V2, V4, V6, V8, V9 and V11 were opened.

7. Both pumps P1 and P2 were switched on. P1 and P2 were adjusted to obtain flow rate
approximately 300mL/min at both flow meters Fl-01 and Fl-02. Both flow rates were made
sure to be equal.
8. Both solutions then were allowed to flow through the reactor R1 and overflow into waste
tank B3.
9. Valves V13 and V18 was opened. Pump P3 then was switched on in order to circulate the
water through pre-heater B5. The stirrer motor M1 was switched on and set up to speed
about200 rpm to ensure homogeneous water jacket temperature.
Experiment Procedures
1. The general starts up procedures were performed.
2. Valves V9 and V11 were opened.
3. Both the NaOH and Et(Ac) solutions were allowed to enter the plug reactor R1 and empty
into the waste tank B3.
4. P1 and P2 were adjusted to give a constant flow rate of about 300 ml/min at flow metersFI01 and FI-02. Both flow rates were ensured same. The flow rates were recorded.
5. The inlet (QI-01) and outlet (QI-02) were started to monitor the conductivity values until
they do not change over time. This is to ensure that the reactor has reached steady state.
6. Both inlet and outlet steady state conductivity values were recorded. The concentration
of NaOH exiting the reactor and extent of conversion from the calibration curve.
7. Optional: Sampling was opened from valve V15 and 50ml of sample was collected. A
back titration procedure was carried out manually to determine the concentration of NaOH in
the reactor and extent of conversion.
8. The experiment was repeated from step 4 to 7 for different residence times by reducing the
feed flow rates of NaOH and Et(Ac) to about 250,200,150,100 and 50 ml/min. Both flow
rates were made sure to be equal.
Titration Procedures
1. The burette was filled up with 0.1 M NaOH solution.
2. 10 mL of 0.25 M HCl was poured in a flask.
3. 50 mL samples that were collected from the experiment at every controlled flow
rate (300,250, 200, 150, 100 and 50 mL/min) were added into the 10mL HCl to quench the
saponification reaction.
4. 3 drops of phenolphthalein were dropped into the mixture of sample and HCl.

5. The mixture then was titrated with NaOH until it turns light pink.
6. The amount of NaOH titrated was recorded.

Result
Conversion

0%
25%
50%
75%
100%

Solution Mixtures
0.1M NaOH 0.1M Na(Ac)

Concentratio
Water
n of NaOH
(M)
100mL
0.0500
25mL
100mL
0.0375
50mL
100mL
0.0250
75mL
100mL
0.0125
100mL
100mL
0.0000
Table 1: Preparation of Calibration Curve

Conductivity
(mS/cm)

100mL
75mL
50mL
25mL
-

10.7
9.7
7.5
5.6
4.0

Reactor volume: 4L
Concentration of NaOH in feed tank: 0.1M
Concentration of Et(Ac) in feed tank: 0.1M
N
o

1
2
3
4

Flow
rate of
NaOH
(mL/
min)

300
250
200
150

Flow
rate of
Et(Ac)
(mL/
min)

300
250
200
150

Total
flow
rate of
solutio
ns,
V0
(mL/
min)
600
500
400
300

Reside
nce
time,
(min)

Outlet
conducti
vity
(mS/cm)
Q1 Q
2

Volu
me
of
NaO
H

Convers
ion, X
(%)

Reactio
n Rate
Constan
t
(L/mol.
min)

Rate of
Reactio
n
(mol/L.
min)

6.67

11.
1

7.
3

0.3

50.6

1.54

3.76

12.
0

7.
0

0.2

11.
5

6.
8

0.1

10.
9

6.
2

0.1

8.00
10.00
13.33

103
50.4

1.27

3.12
103

50.2

1.01

2.50
103

50.2

0.76

1.88
103

5
6

100
50

100

200

50

20.00

100

40.00

10.
2

5.
4

0.2

8.6

4.
8

0.2

50.4
50.4

Calculation
Residence time
For flow rates of 300 ml/min,

Total flow rate,

V0

Reactor volume ( L ) , V
L
Total flow rate
,V0
min

( )

= Flow rate of NaOH + Flow rate of Et(Ac)

= 300 mL/min NaOH + 300 mL/min Et(Ac)

= 600 mL/min = 0.6 L/min.
Hence,
Residence time, = 4L/0.6L/min = 6.67 min

Conversion
For flow rates of 300mL/min:
Moles of reacted NaOH,

n1

n1=Concentration NaOH Volume of NaOH titrated

= 0.1 M 0.0003L
= 0.00003 mole
Moles of unreacted HCl,

n2

1.25
103

Table 2: Experiment 3

Residencetime , =

0.51
0.25

6.15
104

Moles of unreacted HCl = Moles of reacted NaOH

n2=n1
n2=0.00003mole
Volume of unreacted HCl,
V 1=

V1

n2
concentration HCl quench

= 0.00003 / 0.25
= 0.00012L
Volume of HCl reacted,

V2

V 2=Total volume HClV 1

= 0.01 0.00012
= 0.00988L
Moles of reacted HCl,

n3
n3

= Concentration HCl

V1

= 0.25 0.00988
= 0.00247 mole
Moles of unreacted NaOH,
n4

n4

n3

= 0.00247 mole
Concentration of unreacted NaOH
C NaOH unreacted =

n4
0.00247
=
=0.0494 M
volume sample
0.05

X unreacted =concentration of NaOH unreacted concentration NaOH

= 0.0494/0.1 = 0.494
= 0.506
Conversion for flow rate 300mL/min
0.506 100% = 50.6%

Reaction rate constant, k

k=

v0
X
(
)
V TFR C A 0 1X

For flow of 300mL/min

k=

0.6
0.506
=1.54 L . mol/min
4 0.1 10.506

Rate of reaction,

r A

r A

CA 0
= k ( (1 X)2
2

For flow rates of 300 mL/min

r A

0.1
3
= 1.54 ( (10.506)2 = 3.76 10
mol.L/min
2

Conversion vs Residance Time

50.7
50.6
50.5
50.4
Conversion (%) 50.3
50.2
50.1
50
5

10

15

20

25

30

35

40

45

Residance time (min)

Discussion
Plug Flow Reactor (PFR) is a reactor that comprises of a cylindrical pipe and is performed at
steady state in which the feed enters at one end of a cylindrical tube and the product stream
leaves at the other end. The properties of the flowing stream will vary from one point to
another point. The fluid is thin and unmixed layer. In this experiment, the solutions used
NaOH and Et(Ac) reacts together in the reactor to complete saponification reaction. The main
objective of this particular experiment is to study the effect of residence time on the
performance of this reactor. Residence times are manipulated variable in the experiment.
Residence times were manipulated by the means of changing the flow rates of the feed
solutions.
The total flow rates and outlet conductivity value are tabulated in Table 2. A series
of calculations were made and the values of residence times, conversion of the reactions,
reaction rate constants and rate of reactions were determined and tabulated in Table 2 and a
graph is plotted to study the conversion against time residence. Conversion is a property that
shows how much of the reaction has taken place. Hence, by comparing this property with the
residence time parameter, one can analyse the effects of increasing residence time to the
reaction itself. It shows that the conversion of the reaction remains fairly constant with the
increasing residence time. Therefore, residence time is not a factor of reaction conversion.
This is because PFR lacks a good mixing process. Since the PFR is designed not to stir the
solution vigorously to maximise mixing process, the conversion of the reaction by using PFR
is fairly low. The experiment also aims to evaluate the reaction rate constants and rate
of reaction values of the reaction..

Conclusion
The experiment was conducted to carry out a saponification process between Sodium
Hydroxide, NaOH and Ethyl Acetate, Et(Ac). By using a Plug Flow Reactor, PFR, these two
substances were flowed into the reactor, mixed and react for a certain period of time to
completing the saponification process. The experiment also performs to determine the
reaction rate of this particular reaction. Thirdly, this experiment conducted to study the
relationship between the residence time and the conversion of the reactants. This relationship
was successfully studied.
Recommendations
There are several recommendations during conduct this experiment:

Wear protective clothing, shoes, helmet and goggles throughout the

laboratory session to prevent injured.
It is better to time the sample well so that time-wasting in taking samples can be
reduced or, if possible, avoided.
All valves should be properly placed before the experiment started.
Flow rates should be constantly monitored so that it remains constant throughout the
reaction, as needed.
Titration should be immediately stopped when the indicator turned pink.
Pumps should never be run dry.

Reference
1. Fogler, H.S (2006). Elements of Chemical Reaction Engineering (3rd Edition).
PrenticeHall.
2. Levenspiel, O. (1999). Chemical Reaction Engineering (3rd Edition). John Wiley.
3. Laboratory Manual Tubular Flow Reactor.

Appendix