UNIVERSITI TEKNOLOGI MARA

PENGAJIAN KEJURUTERAAN KIMIA

REACTION ENGINEERING LABORATORY
(CHE 506)

NAME & STUDENT : NOOR FARAH HANNAH BINTI WAHAB (2021868204)

NUMBER NOR FARISHA MASTURA BINTI FISSOL (2021614808)
NORAZILA BINTI MUHAMMAD SHAMSUDIN (2021846976)
NUR ADLEENA BINTI KHAIRUL NIZAM (2021813702)
ANIS HUSNA BINTI JANAI (2020853474)
GROUP : CEEH2205J
EXPERIMENT : PLUG FLOW REACTOR
DATE PERFORMED : 6TH JANUARY 2023
SEMESTER : 5
PROGRAMME/CODE : BACHELOR OF ENGINEERING (HONS) CHEMICAL /
CEEH220
SUBMIT TO : TS. HABSAH BINTI ALWI

No Title Allocated Marks (%) Marks

1 Abstract / Summary 5
2 Introduction 10
3 Objectives 5
4 Theory / Literature Review 10
5 Apparatus 5
6 Methodology / Procedure 10
7 Results 10
8 Calculations 10
9 Discussion 20
10 Conclusion 5
11 Recommendation 5
12 Reference / Appendix 5
Total Marks 100

Remarks:

Checked by:

…………………………………………..
Date:
TABLE OF CONTENTS
1.0 ABSTRACT.....................................................................................................................3
2.0 INTRODUCTION............................................................................................................3
3.0 OBJECTIVES...................................................................................................................4
4.0 THEORY..........................................................................................................................5
5.0 APPARATUS & MATERIALS.......................................................................................6
6.0 METHODOLOGY...........................................................................................................6
7.0 RESULTS.........................................................................................................................9
8.0 CALCULATIONS.........................................................................................................10
9.0 DISCUSSION.................................................................................................................13
10.0 CONCLUSION..............................................................................................................15
11.0 RECOMMENDATION..................................................................................................15
12.0 REFERENCES/APPENDIX..........................................................................................16

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1.0 ABSTRACT
The experiment has several objectives, including performing a saponification reaction
between NaOH and Et(Ac), determining the effect of residence time on the conversion, and
determining the reaction rate constant. The saponification reaction takes place in the SOLTEQ
Plug Flow Reactor BP-101. Sodium hydroxide (NaOH) and ethyl acetate (Et (Ac) flow rates
are 300, 250, 200, 150, 100, and 50 mL/min each. Product samples from each flow rate are
collected and used in experiment 2. A conversion versus residence time graph was created.
The results show that as the reaction rate constant decreases so does the reaction rate.

2.0 INTRODUCTION
The batch reactor, continuous stirred-tank reactor (CSTR), and plug flow reactor (PFR) are the
three main types of standard chemical reactors. Each of these reactor types has unique
characteristics, advantages, and disadvantages. The PFR model can simulate multiple
reactions as well as reactions with changing flow temperatures, pressures, and densities.
Although these complications are not addressed in this section, they are frequently relevant to
industrial processes.

The PFR tubular reactor is capable of handling both liquid and gas phases. Tubular reactors
are frequently used in the manufacture of gasoline, oil cracking, and the oxidation of sulfur
dioxide to sulfur trioxide. The reactor is a long vessel with feed entering at one end and
product exiting at the other. In some occurrences, the vessel is filled with a solid catalyst.

Figure 1: Plug Flow Reactor

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Plug Flow Reactor Model

Plug flow reactors are typically run at steady state. As they flow down the length of the
reactor, reactants are constantly consumed. Plug flow reactors can be one long tube or a series
of shorter tubes. Their diameters range from a few centimeters to several meters. The diameter
is chosen based on construction costs, pumping costs, desired residence time, and heat transfer
requirements. Long small diameter tubes are typically used for high reaction rates, while
larger diameter tubes are used for slow reaction rates.

3.0 OBJECTIVES
The objectives of the experiment are: -
1) To carry out a saponification reaction between sodium hydroxide, NaOH and ethyl
acetate, Et (AC).
2) To determine the reaction rate constant.
3) To determine the effect of residence time on the conversion.

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4.0 THEORY
In a chemical industry, reactors are the main equipment used to mix and cause reactions to
created desired products from the raw materials. For this experiment, plug flow reactor will be
used. Plug flow reactor (PFR) consist of long hollow tube in which the reactant would flow in
an axial direction in the shape of plug as shown in Figure 1. The tube is encased inside the
tank to maintain the temperature of the system. For PFR, it is assumed that the reactant is
perfectly mixed, and the composition of the reactant is different along the tube. The streams
are opposite of a batch reactor, which is when the reactor consists of a constant volume and
has no flow going in or out.

Figure 2: Diagram of Plug flow reactor

PFR has been selected as the main choice for certain chemical process in the industry due to
its non-mixing property of the reactors and continuous production of the product. Flow of plug
flow reactor is laminar which is suitable for the selected reaction. In short, it is impossible to
proceed 100%. This is because to the rate of reaction decreases when percent completion
gradually increases until the point where the system achieves dynamic equilibrium where no
more reaction can occur. Thus, distillation process is used as a separation process to separate
any undesired products such as by-products from the desired products. For any unreacted
reactants, it can be recycled back to the feed stream to cut cost.

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5.0 APPARATUS & MATERIALS
Apparatus

1. Burette
2. Conductivity Meter
3. Plug Flow Reactor

Materials

1. 0.25M Hydrochloric Acid, HCl

2. 0.1M Sodium Hydroxide, NaOH

3. 0.1M Sodium Acetate, Na (Ac)

4. Deionized Water, H2O

6.0 METHODOLOGY
Experiment 1 – Preparation of Calibration for Conversion vs. Conductivity
1) Prepared the following solution:
i. 1 liter of sodium hydroxide, NaOH (0.1M)
ii. 1 liter of sodium acetate, Na(Ac) (0.1M)
iii. 1 liter of deionised water, H2O

2) To measure the conductivity and NaOH concentration for every conversion value,
combine the following solutions into 100ml of deionised water:
i. 0% conversion: 100 ml NaOH
ii. 25% conversion: 75 ml NaOH + 25 ml Na(Ac)
iii. 50% conversion: 50 ml NaOH + 50 ml Na(Ac)
iv. 75% conversion: 25 ml NaOH + 75 ml Na(Ac)
v. 100% conversion: 100 ml Na(Ac)

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Experiment 2 – Back Titration for Manual Conversion Determination

1) A 0.1M NaOH solution is poured into the burette.

2) In a flask, 10 ml of 0.25M HCl is measured.

3) After obtaining 50 ml of sample from the experiment, the sample is immediately

added to the HCl inside the flask to quench the saponification reaction.

4) Add a few drops of pH indicator to the mixture.

5) The mixture is neutralised by titration with NaOH solution from the burette. The
amounts of NaOH titrated is recorded.

Experiment 3 – Effect of Residence Time on the Reaction

1) Follow the general startup steps outlined above.

2) V9 and V11 valves are opened.

3) NaOH and Et(Ac) solutions are both permitted to enter the plug flow reactor R1 and
drain into waste tank B3.

4) At flow metres FI-01 and FI-02, P1 and P2 are adjusted to provide a constant flow rate
of roughly 300ml/min. Ensure that the flow rates are the same.Flow rates are
measured.

5) The conductivity values at the inlet (QI-01) and outflow (QI-02) are being monitored
until they does not change over time.This is done to guarantee that the reactor is in a
stable condition.

6) The steady state conductivity values at the inlet and outflow are recorded. The
calibration curve is used to calculate the concentration of NaOH leaving the reactor
and the extent of conversion.

7) Optional: open sampling valve V15 and collect 50 ml of sample. A reverse titration
process is used to manually determine the concentration of NaOH in the reactor and
the level of conversion.

8) Repeat steps 4–7 for varied residence times by lowering the NaOH and Et(Ac) input
flow rates to about 250, 200, 150, 100, and 50 ml/min. Ensured that the flow rates are
the same.

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Page | 8
General Shut Down

1) pumps P1, P2, and P3is turned off. V2 and V6 valves are closed.

2) The heaters are turned off.

3) While the stirrer motor is working, the cooling water is continued circulating through
the reactor to allow the water jacket to drop to ambient temperature.

4) If the equipment is not going to be utilised for an extended length of time, all liquid is
drained from the unit by opening valves V1 to V19.

5) The control panel's power is switched off.

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7.0 RESULTS
Table 1: Effect of Residence Time on the Reaction by Back Titration.

Total feed Conductivity

Flowrate Flowrate Residence Volume of
flowrate of (mS/cm)
Sample of NaOH of Et (Ac) Time, Ꚍ NaOH, V1
solutions, vo
(mL/min) (mL/min) (min) Q1 Q2 (mL)
(mL/min)
1 300 300 600 6.67 8.2 9.8 14.5
2 250 250 500 8.0 7.9 8.3 17.1
3 200 200 400 10.0 7.7 8.7 13.6
4 150 150 300 13.33 7.5 8.4 18.1
5 100 100 200 20.0 7.5 8.1 14.0
6 50 50 100 40.0 7.3 7.6 13.6

Table 2: Back Titration Data Calculation

Reaction Rate Rate of Reaction, -
Volume of NaOH,
Sample Conversion (%) Constant, k rA
V1 (mL)
(L/mol.min) (mol/L.min)
1 14.5 58.0 2.0714 0.003654
2 17.1 68.4 2.7057 0.002702
3 13.6 54.4 1.1930 0.0024806
4 18.1 72.4 1.9674 0.0014987
5 14.0 56.0 0.6364 0.0012320
6 13.6 54.4 0.2935 0.0006103

Table 3: Data Collection for Calibration

Conversion Solution Mixture (mL) Concentration Conductivity
(%) 0.1M NaOH 0.1M Et (Ac) H2O of NaOH (M) (mS/cm)
0 100 0 100 0.0500 6.45
25 75 25 100 0.0375 4.23
50 50 50 100 0.0250 2.26
75 25 75 100 0.0125 0.70
100 0 100 100 0.0000 0.20

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8.0 CALCULATIONS
Sample Calculation

Calculations are based on the flowrate of 300 mL/min for both NaOH and Et (Ac)

Additional Information Value

Reactor Volume, VPFR 4L
Concentration of NaOH in feed vessel, CNaOH,f 0.1M
Concentration of NaOH in reactor, CNaOH 0.1M
Concentration of HCl for quenching, CHCl,s 0.25M
Volume of HCl for quenching, VHCl,s 10mL
Volume of sample, Vs 50mL

A. Calculation for Total Feed Flowrate, vo

Total Feed Flowrate , v o=Flowrate of NaOH ( min

mL
)+ Flowrate of Et ( Ac ) ( min
mL
)
Total Feed Flowrate , v =300 ( ) +300 ( ) Total Feed Flowrate , v =600 (
min )
mL mL mL
o o
min min

B. Calculation for Residence Time, τ

Reactor Volume , V PFR (L)
Residence Time , τ =
Total Feed Flowrate , v o ( minL )
4 (L)
Residence Time , τ =
0.6 ( )
L
min
Residence Time , τ =6.67 min

C. Calculations for Conversion, X (%)

a. Volume of unreacted quenching HCl, V2
C NaOH , f (M )
V 2= ×V 1 (mL )
C HCl , s ( M )

0.1 M
V 2= ×14.5 mL
0.25 M

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V 2=5.8 mL

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b. Volume of HCl reacted with NaOH in the sample, V3
V 3=( V HCl ,s−V 2 )=( 10.0 mL−9.24 mL )

V 3=4.2 mL

c. Moles of HCl reacted with NaOH in the sample, n1

( molL ) ×V ( mL)
n1=C HCl , s 3

n =(0.25
L )
× ( 4.2 mL ) × (
1000 mL )
mol 1L
1

n1=0.00105 mol

d. Moles of unreacted NaOH in sample, n2

n2 =n1

n2 =0.00105 mol

e. Concentration of Unreacted NaOH in the Reactor, CNaOH

n2 (mol)
C NaOH =
V s (mL)

C NaOH =
0.00105 mol 1000 mL
50 mL
×
1L ( )
C NaOH =0.021 M

f. Conversion of NaOH in the reactor, XNaOH

C NaOH ( M ) 0.021 M
X unreacted = =
C NaOH ,0 (M ) 0.05 M

X unreacted =0.42

X reacted =( 1− X unreacted ) ×100 %

X reacted =( 1−0.42 ) ×100 %

X reacted =58 %

g. Reaction Rate Constant, k

k=
( v o ( L/min ) X
V PFR ( L ) ×C AO (M ) 1−X )( )
( )(
L
0.6
k=
min
4 L× 0.1 M
0.58
1−0.58 )
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 L
k =2.0714
mol . min
h. Rate of Reaction, -rA
−r A =k C A C B

Since CAO = CBO = (1-X)

2 2
−r A =k ( C AO ) (1− X )

( )
2
L mol 2
−r A =2.0714 × 0.1 ×(1−0.58)
mol . min L

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 mol
9.0 −r A =0.003654 DISCUSSION
L .min
A Plug Flow Reactor (PFR) is a type of reactor that consists of a cylindrical pipe and is
typically used in steady-state operation. The feed enters one end of a cylindrical tube and exits
the other end of the cylindrical tube. The major purpose of this plug flow reactor (PFR)
experiment is to carry out a saponification reaction between NaOH and Et (Ac). The SOLTEQ
Plug Flow Reactor (Model BP 101) is used for this experiment, and NaOH and Et(Ac)
solutions are supplied into the reactor; these two solutions react together in the PFR to
complete the saponification reaction. The primary objective of this experiment is to
investigate the effect of residence time on the performance of this reactor. At the end of the
experiment, calculation of the reaction rate constant can be made and the effect of residence
time on conversion in the plug flow reactor can be observed.

In this experiment, the flow rate of both solutions was set as the varying component,
Following the completion of the experiment, the data containing the inlet flow rates of NaOH
and Et (Ac), inlet and outlet conductivity values, and volume of NaOH utilised in the titration
process are summarised in Table 1: Effect of residence time on the reaction by back titration.
A series of calculations were performed based on the tabulated data, as shown in the Sample
of Calculation section. Following that, the residence times, conversion of reactions, reaction
rate constants, and rate of reactions were calculated, Table 2: of the Result section tabulates
these values.

Based on the data obtained and the calculation made, The reaction rate constant for a total
flow rate of 600 mL/min is 2.0714 L/mol.min, for a flow rate of 500 mL/min is 2.7057
L/mol.min, for a flow rate of 400 mL/min is 1.19674 L/mol.min, for a flow rate of 300
mL/min is 1.9674 L/mol.min, for a flow rate of 200 mL/min is 0.6364 L/mol. According to
the reaction rate constant determined, the value of the reaction rate constant should decrease
as the flow rate decreases, but as the results show, the value of the reaction rate constant
increases as the flow rate increases, but at a total feed flow rate of 500 ml/min, the reaction
rate constant is larger than the reaction rate constant at 600 ml/min, and the same goes at 300
ml/min. This is most likely due to human errors occurring during the experiment's execution.
After calculating the reaction rate constant, the rate of reaction can also be calculated. The
estimated data for the rate of reaction shows that as the total flowrate increases, so does the
rate of reaction.

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 Figure 3: Comparison between conversion and residence time

A reactor's residence time is defined as the reactor volume divided by the total feed
flow rates, whereas conversion is a property that indicates how much of the reaction occurs,
which is the number of moles of A that reacted per mole of A delivered into the system. The
average amount of time that a particle spends in a given system is represented by residence
time, and conversion is a direct result of response time. The effect of residence time on
conversion can be observed on the graph, but as it can be seen on the graph, when comparing
both the conversion and the residence time, the values do not show up as they should
theoretically, where residence time represents the average amount of time that a particle
spends in a given system, and conversion is a direct result of response time. The graph shows
that the conversion does not increase with residence time but fluctuates where it increases at
residence time, 8 minutes, the conversion increases at 68.4% but decreases again when
residence time is 10 minutes to 54.4%, and this also happens at residence time 13.33 minutes
where the conversion fluctuates at 72.4% and then decreases to 56% conversion at residence
time 20 minutes. This could occur as a result of human mistake throughout the experiment,
such as during the titration and data collection processes.

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10.0 CONCLUSION
The saponification reaction involving NaOH and Et(Ac) was carried out in a plug flow
reactor, where it was mixed and reacted over time. The reaction rate constant for the
saponification process was determined in this experiment. The value of the reaction rate
constant that was found then, the rate of reaction was determined by making use of the
reaction rate constant in the calculation. Aside from that, the purpose of this experiment is to
ascertain the rate of reaction and evaluate it in relation to the total flow rates used.
Furthermore, the experiment can be used to investigate the relationship between residence
time and the amount of reactants converted. As a result of this investigation, it was found that,
theoretically, the conversion rate should rise along with the residence time, but on the other
hand, from the collected data, it shows fluctuations in both the residence time and the
conversion rate. This is most likely because of an error that occurred while the experiment was
being carried out.

11.0 RECOMMENDATION
Numerous measures and suggestions might be taken to achieve more accurate and dependable
findings. Which are:

1. To obtain more reliable data, repeat the experiments at least three times and determine
the average results.
2. Always ensure that the start-up and shut-down procedures are followed appropriately
to avoid equipment damage.
3. The inlet flow rates must be kept consistent by monitoring them at all times since they
impact the gathered data.
4. Glass apparatus must be handled with care to avoid breaking when doing experiments.
5. Wear Personal Protective Equipment (PPE) when doing the titration because we will
be handling chemicals.

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12.0 REFERENCES/APPENDIX

Figure 4: Data Collection During experiment

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