UNIVERSITI TEKNOLOGI MARA FAKULTI KEJURUTERAAN KIMIA REACTION

ENGINEERING LABORATORY (CHE506)

NAME: STUDENT NO :
KHAIRUL AMIRIN BIN KHAIRUL ANUAR 2017632082
PUTERA NAJMEEN FARITH BIN ABDUL RAZAK 2017632096
NURUL AMIRAH BINTI MUSDAFA KAMAL 2017632124
NURUL AIDA BINTI MOHAMMAD 2017632132
NURUL KAMILAH BINTI KHAIROL ANUAR 2017632192
NURLINA SYAHIIRAH BINTI MD TAHIR 2017632214
GROUP : EH2205I
EXPERIMENT : PLUG FLOW REACTOR (BP101)
DATE PERFORMED th
: 8 OCTOBER 2018
SEMESTER :5
PROGRAMME / CODE : CHEMICAL ENGINEERING / EH220
SUBMIT TO : DR. FARID MULANA

No. Title Allocated Marks (%) Marks

1 Abstract/Summary 5
2 Introduction 5
3 Aims 5
4 Theory 5
5 Apparatus 5
6 Methodology/Procedure 10
7 Results 10
8 Calculations 10
9 Discussion 20
10 Conclusion 10
11 Recommendations 5
12 Reference 5
13 Appendix 5
TOTAL MARKS 100

Remarks:

Checked by: Rechecked by:

--------------------------- ---------------------------

Date: Date:
 TABLE OF CONTENT

1.0 ABSTRACT...................................................................................................................2

2.0 INTRODUCTION.........................................................................................................3

3.0 OBJECTIVES................................................................................................................3

4.0 THEORY........................................................................................................................5

5.0 MATERIALS & APPARATUS.................................................................................... 5

6.0 METHODOLOGY........................................................................................................8

7.0 RESULTS.....................................................................................................................11

8.0 CALCULATIONS.......................................................................................................15

9.0 DISCUSSION.............................................................................................................. 15

10.0 CONCLUSION............................................................................................................21

11.0 RECOMMENDATIONS............................................................................................ 22

12.0 REFERENCES............................................................................................................23

13.0 APPENDICES............................................................................................................. 24

LAB REPORT ON PLUG FLOW REACTOR (L5) 1

1.0 ABSTRACT

The goals of the experiment is to investigate the effect of residence time towards the
conversion of the saponification process between Sodium Hydroxide, NaOH and ethyl
acetate, Et(Ac). The saponification process is done using the SOLTEQ Plug Flow Reactor BP
– 101. The product sample is taken for every flowrate of sodium hydroxide, NaOH and ethyl
acetate, Et(Ac) which is at 250mL/min, 200mL/min, 150mL/min, 100mL/min and 50mL/min
for titration process in Experiment 2 for the manual conversion determination. The residence
time for each flowrate is 8 min, 10 min, 13.3333 min, 20 min and 40 min, respectively. The
conversion of the reactant to product is 68%, 64%, 57.2%, 56.8% and 54.4%, respectively.
The reaction rate constant, k is 2.6563 L/mol.min, 2.2222 L/mol.min, 1.6706 L/mol.min,
1.6435 L/mol.min and 1.4912 L/mol.min, respectively. The rate of reaction, -r A is 0.002720
mol/L.min, 0.002879 mol/L.min, 0.003060 mol/L.min, 0.003067 mol/L.min and 0.003100
mol/L.min, respectively. The rate of reaction decreases as the reaction rate constant
decreases. Higher flowrate of reactant increases the rate of reaction and thus, increasing the
conversion rate of the reactant to product.

LAB REPORT ON PLUG FLOW REACTOR (L5) 2

2.0 INTRODUCTION

In the industry, reactors are one of the most important equipment to create a desired products
from the raw materials. The design of a certain reactors are crucial. There are three types of
basic reactor which is Batch Reactor, Continuous Stirred Tank Reactor (CSTR), and Plug
Flow Reactor (PFR).

Plug flow reactor (PFR) or Tubular flow reactor consist of long hollow tube in which the
reactant would flow in an axial direction in the shape of plug (Cylindrical shape) as shown in
Figure 1. These tube usually encased inside the tank to maintain the temperature of the system. In
the PFR, we would consider 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 a reactor that has a
constant volume and has no incoming or outgoing streams.

Figure 1 - Plug Flow Reactor Where the Reactant Flow In an Axial Direction in the
Shape of Plug

PFR become main choice for certain chemical process in the industry due to its non-
mixing property of the reactors. It is also very helpful in the continuous production of the
product. Flow of plug flow reactor is laminar, as with viscous fluids in small-diameter tubes,
and greatly deviate from ideal plug-flow behaviour.

Basically, for chemical reactions, it is impossible to proceed to 100% completion.

This is because due to the rate of reaction decreases when percent completion gradually
increases until the point where the system achieve dynamic equilibrium (no net reaction
occurs). In fact, the equilibrium point mostly is less than 100% complete. Thus, distillation is
used as a separation process, in order to separate any remaining reagents or by products from
the desired product. Sometimes the reagents may be reused at the beginning of the process as
a recycle back, such as in the Haber process.

LAB REPORT ON PLUG FLOW REACTOR (L5) 3

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.

LAB REPORT ON PLUG FLOW REACTOR (L5) 4

4.0 THEORY

Plug Flow Reactor (PFR) is one of the ideal reactor in industry. Many plants and company
used PFR as the site for their reactants to react in producing valuable desired product. This
reactor mainly famous for process that involves gas or fast reactions process. This is because,
in PFR the reactants are fed continuously and products are also continuously removed. PFR
becomes favourable because it is easy to maintain, as it does not have any moving parts.
Additionally, the most favourable reason is it has the highest conversion per reactor volume
of flow reactor. In designing and modelling a PFR, an ideal condition are assumed in order to
ease the calculation. The PFR behaviour are assumed to be perfect mixing at all times without
dead time occurs in any corner or area in the PFR. This composition is a function of residence
time and rate of reaction.

Figure 2 - The Schematic Diagram of A PFR

The ideal PFR mole balance with assumptions can be written as follows:
(Accumulation) = (in) − (out) + (generation)

= − + ∫( . )

Assumption made: dN A
1. In steady state condition, dt = 0 but only in the radial direction (Rodgers, 2013).

2. No axial mixing.
3. For a flow system, FA can be given in terms of entering molar flow rate FA0 and the conversion, X.
FA = FA0 − FA0X

Thus, rearranging the equation would obtained this equation,

FA0X = FA0 − FA

LAB REPORT ON PLUG FLOW REACTOR (L5) 5

 Rearranging eq.1,
0= 0 +∫ 0

[∫ − 0
]= 0
− = 0

∫ = 0∫
−

0
0

Ideal equation of a PFR is shown as below: = ∫ ( . )

−

4. In this experiment, the reaction order is second order thus it depends on concentration of both solution 0 and 0 (Engineering). However, to ease the calculation and
analysis, the concentration being fed to the reactor in in equimolar. Thus, the initial concentrations of reactants is CA0 = CB0. The rate law can be written as follow:
−rA = kCACB = kCA2
− = ( − ) ( . )

Rearranging in terms of residence time,

X X
dX dX
V = FA0 ∫ =v C
∫
0 A0
−r kC 2 (1 − X) 2

A A0
0 0

v0 dX
V= ∫
kC (1 − X) 2

A0
0
v X
V= 0 ( )

kC A0 1−X

= = ( ) ( . )
−

For constant PFR volume, flow rate and initial concentrations, the reaction rate constant is,

= ( ) ( . )
−

LAB REPORT ON PLUG FLOW REACTOR (L5) 6

5.0 MATERIALS & APPARATUS

5.1 Materials
1) 0.25M Hydrochloric Acid, HCl
2) 0.1M Sodium Hydroxide ,NaOH
3) 0.1M Sodium Acetate, Na(Ac)
4) Deionized Water, H2O

5.2 Apparatus
1) Burette
2) Conductivity Meter
3) Plug Flow Reactor

Plug flow
reactor

Figure 3 - Set Up Of Plug Flow Reactor

LAB REPORT ON PLUG FLOW REACTOR (L5) 7

 6.0 METHODOLOGY
6.1 General Start Up
1) Ensure all the valves are initially closed except valves V4, V8 and V17.
2) The solutions are prepared for each experiment.
3) The power for the control panel is turned on.

Task Experiment 1&2 Experiments 3&4

B1 Deionized water 0.1M NaOH solution
B2 0.05M NaCl solution 0.1M Et(Ac) solution
4) The water jacket B4 and preheater B5 is filled with a clean water. The valves V13

and V18 is opened. Pump P3 is switch on to calculate the water through pre-
heater B5.
5) A stirrer motor M1 is switched on and the speed is set for about 200 rpm.
6) Valve V2, V4 and V10 is opened. Pump P1 is switched on. P1 is adjusted to flow
rate of 150 ml/min at flow meter, FI-01. Valve V10 is closed and pump P1 is
switched off.
7) Valve V6, V8, V12 is opened. Pump P2 is switched on. P2 is adjusted to flow rate
150 ml/min at flow meter FI-02. Valve V12 is closed and pump P2 is switched off.
8) The unit is now ready for the experiments.

6.2 Experiment 1 – Preparation of Calibration for Conversion vs. Conductivity

1) The following solutions are prepared:

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) The conductivity and NaOH concentration for each conversion values is
determined by mixing 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)

LAB REPORT ON PLUG FLOW REACTOR (L5) 8

6.3 Experiment 2 – Back Titration for Manual Conversion Determination
1) The burette is filled up with 0.1M NaOH solution.
2) 10 ml of 0.25M HCl is measured in flask.
3) 50 ml of sample from the experiment is obtained and the sample is immediately
added to the HCl in the flask to quench the saponification reaction.
4) A few drops of pH indicator is added into the mixture.
5) The mixture is titrated with NaOH solution from the burette until the mixture is
neutralized. The amount of NaOH titrated is recorded.

6.4 Experiment 3 – Effect of Residence Time on the Reaction

1) The general start-up procedures are performed as above.
2) Valve V9 and V11 are opened.
3) Both NaOH and Et(Ac) solutions are allowed to enter the plug flow reactor R1
and empty into the waste tank B3.
4) P1 and P2 are adjusted to give a constant flow rate of about 300ml/min at flow
meters FI-01 and FI-02. Make sure that both flow rates are the same. The flow
rates are recorded.
5) The inlet (QI-01) and outlet (QI-02) conductivity values are being monitored
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 are recorded. The
concentration of NaOH exiting the reactor and extent of conversion from the
calibration curve is obtained.
7) Optional : sampling valve V15 is opened and 50 ml of sample is collected. A back
titration procedure to manually determine the concentration of NaOH in the
reactor and extent of conversion is carried out.
8) The experiment steps 4 to 7 is repeated for different residence time by reducing
the feed flow rates of NaOH and Et(Ac) to about 250, 200, 150, 100 and 50
ml/min. Make sure that both flow rates are the same.

LAB REPORT ON PLUG FLOW REACTOR (L5) 9

6.5 General Shut Down

1) Pump P1, P2 and P3 is switched off. Valve V2 and V6 is closed.

2) The heaters is switched off.
3) The cooling water is kept circulating through the reactor while the stirrer motor is
running to allow the water jacket to cool down to a room temperature.
4) All liquid is drained from the unit by opening valve V1 to V19 if the equipment is
not going to be used for a long period of time.
5) The power is turned off for the control panel.

LAB REPORT ON PLUG FLOW REACTOR (L5) 10

7.0 RESULTS

Table 1 - Data Collection for Calibration Curve Preparation in Experiment 1.

Solution Mixture Concentration Conductivity
Conversion
0.1 M 0.1 M H2O of NaOH (M) (mS/cm)
NaOH Et (Ac)

0% 100 mL - 100 mL 0.0500 23.6000

25% 75 mL 25 mL 100 mL 0.0375 14.9000
50% 50 mL 50 mL 100 mL 0.0250 9.2100
75% 25 mL 75 mL 100 mL 0.0125 4.2300
100% - 100 mL 100 mL 0.0000 0.0654

Conversion vs. Conductivity

Conversion, X
y = -0.0424x + 0.9406
R² = 0.9783

y = -0.0424x + 0.9406
R² = 0.9783

Conductivity (ms/cm)

Figure 4 - The graph of Conversion, X, against Conductivity, Q, obtained from calibration

curve preparation in experiment 1.

The graph shows the graph of conversion versus conductivity. The conversion is
decreasing linearly as the conductivity increase.

LAB REPORT ON PLUG FLOW REACTOR (L5) 11

Experiment 2: Effect of Residence Time on the Reaction

Table 2 - A Constant Flowrate Recorded At Flowmeters FI-01 and FI-02

Initial Flowrate Of Inlet Conductivity, Q1 Outlet Conductivity, Q2
Solutions
(mL/min) (mS/cm) (mS/cm)

Pump 1 250 10.4 7.0

Pump 2 250 10.6 6.9

❖ Information added:

a) Reactor Volume, VPFR :4L

b) Concentration of NaOH in feed vessel, CNaOH,f : 0.1 M
c) Concentration of NaOH in the reactor, CNaOH : 0.1 M
d) Concentration of HCl for quenching, CHCl,s : 0.25 M
e) Volume of HCl for quenching, VHCl,s : 10 mL
f) Volume of sample, Vs : 50 mL

LAB REPORT ON PLUG FLOW REACTOR (L5) 12

 Table 3 - Data Collection Obtained From Experiment 3
Flowrate Flowrate Total feed Residence Conductivity Reaction Rate of
flowrate of (mS/cm) Volume of NaOH Conversion Rate Reaction,
of NaOH of Et (Ac) Time, τ
solutions, vo (mL) , X (%) Constant, k -rA
(mL/min) (mL/min) (mL/min) (min) Q1 Q2 (L/mol.min) (mol/L.min)

250 250 500 8.00 9.5 8.3 17.0 68.0 2.6563 0.002720
200 200 400 10.00 9.4 7.7 16.0 64.0 2.2222 0.002879
150 150 300 13.33 8.9 7.3 14.3 57.2 1.6706 0.003060
100 100 200 20.00 8.1 6.1 14.2 56.8 1.6435 0.003067
50 50 100 40.00 7.8 5.2 13.6 54.4 1.4912 0.003100

13
 Conversion vs. Residence Time
50
45
40
Conversion, X (%)

35
30
25
20
15
10 Residence Time, τ (min)
5
0 0 10 20 30 40 50

Figure 5 - The graph of Conversion, X, against Residence time, τ, obtained from the
calculations in experiment 3.

The graph shows the plot of conversion versus residence time. The curve shows a
decreasing pattern until t = 20 min, before increasing as the curve approaching to t = 40 min.

14
8.0 CALCULATIONS
❖ These calculations were determined for the flowrates of 250 mL/min: -

A. Calculation for Residence Time, τ.

Reactor volume, VPFR (L)

Residence Time, τ =
L
Total feed flowrate, v ( )

o min

1. Total flowrates of sodium hydroxide, NaOH, and ethyl acetate, Et (Ac) are,

Total flowrate, Vo = Flowrate of NaOH + Flowrate of Et (Ac)

= 250 mL/min NaOH + 250 mL/min Et (Ac)

= 500 mL/min

= 0.5 L/min
4L
Thus, Residence Time, τ = 0.5 L/min = 8 min

B. Calculation for Conversion, X.

1. Concentration of NaOH entering the reactor, CNaOH,o

C C
= NaOH,f
NaOH,o
2

0.1 M
=
2

= 0.05 M

LAB REPORT ON PLUG FLOW REACTOR (L5) 15

 2. Volume of unreacted quenching HCl, V2 C
NaOH,s
V2 = × V1
CHCl,s
0.1 M
= 0.25 M × 17.0 mL

= 6.8 mL

3. Volume of HCl reacted with NaOH

V =V
in −the
V
sample, V3
3 HCl,s 2
= (10 − 6.8) mL
= 3.2 mL

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

n =C ×V
1 HCl,s 3

mol 1L

= 0.25 × 3.2 mL ×
L 1000 mL

= 0.0008 mol

5. Moles of unreacted NaOH in sample, n2

n2 = n1
= 0.0008 mol

6. Concentration of unreacted NaOH in the reactor, CNaOH

n
2
C =
NaOH

V
s

0.0008 mol 1000 mL

= ×

50 mL 1L

= 0.016 M

LAB REPORT ON PLUG FLOW REACTOR (L5) 16

 7. Conversion of NaOH in the reactor, XNaOH C
NaOH
X =
unreacted CNaOH,o
0.016 M
= 0.05 M = 0.32
X = (1 − X ) × 100%
reacted unreacted
= (1 − 0.32) × 100%
= 68%

C. Calculation for Reaction Rate Constant, k.

vo X

k= ( )
V C 1−X

TFR
Ao

1. Total feed flowrate, vo = 0.5 L/min

2. Volume of reactor, VTFR =4L

3. Inlet concentration of NaOH, CAo, in the reactor = 0.1 M
4. Conversion, X = 0.68

❖ All the values above are substituting into the rate constant equation where,

L
0.5 0.68 L
min

k=[ ]( ) = 2.6563

(4 L)(0.1 M) 1 − 0.68 mol. min

LAB REPORT ON PLUG FLOW REACTOR (L5) 17

 D. Calculation for Rate of Reaction. -rA.
−rA = kCACB
CA = CAo (1 − X)
CB = CBo (1 − X)
Since CAo = CBo ,
−rA = k(CAo )2(1 − X)2

❖ From the equation above, the rate of reaction obtained is,

L mol 2 mol
2
(1 − 0.68)
−r = (2.6563 ) (0.1 ) = 0.002720

mol. min L L. min

NOTE: The same way of calculations was used to evaluate the residence time, conversion,
reaction rate constant and rate of reaction for different flowrates of 200 mL/min, 150
mL/min, 100 mL/min and 50 mL/min.

LAB REPORT ON PLUG FLOW REACTOR (L5) 18

9.0 DISCUSSION

In this plug flow reactor (PFR) experiment it is primarily to carry out a saponification
reaction between NaOH and Et(Ac). At the end of the experiment, the reaction rate constant
is determined by using formula and the effect of residence time on the conversion in the PFR.
This experiment are conducted using the SOLTEQ Plug Flow Reactor (Model BP 101) where
NaOH and Et(Ac) solution are fed into the reactor by varying the feed flow rates to obtain
several residence time and the effect of each one is studied.

Besides, a calibration curve for conductivity versus conversion is also prepared for
saponification reaction of ethyl acetate Et(Ac) and sodium hydroxide NaOH. For the
calibration curve of conductivity versus conversion, the slope and y-axis intercept value is
determined from the equation of the curve yield using excel. Based on Figure 4, the slope = -
0.0424, while the y – axis intercept = 0.9406.

In this experiment, different initial feed flowrates, conductivity value and the volume
of NaOH used in the titration process is organized in Table 3. From the data, the residence
time, conversion of the reactions and the reaction rate constant is determined through a series
of calculation by using formula for plug flow reactor experiment.

A graph of conversion against residence time is plotted and it is shown in Figure 5.

The residence time and the conversion of the reaction is obtained from the calculation using
formula. The reactors residence time is defined as the reactor volume divided by the total
feed flow rates while conversion is a property that shows how much of the reaction take place
which is the number of moles of A that reacted per mole of A fed to the system.

From the graph plotted in Figure 5, the conversion of the reaction is inversely
proportional to the residence time of the reactant in the reactor. It shows that when the
residence time of the reactor increases, the conversion of the reactant will decreases.
Residence time shows the average amount of time that a particle spends in a particular system
and conversion is a direct function of time spent for reaction. Apparently, the higher the
residence time, the higher conversion. This may be due to the error of total feed flowrate of
solutions occurred while conducting the experiment.

The reaction rate constant, k for every different initial feed flowrate is 2.6563
L/mol.min for flow rate 250 mL/min. For flow rate 200 mL/min the k-value is 2.2222
L/mol.min and reaction rate constant for 150 mL/min is 1.6706 L/mol.min. For flow rate 100

LAB REPORT ON PLUG FLOW REACTOR (L5) 19

and 50 mL min the reaction rate constant is 1.6435 and 1.4912. We can see that the reaction
rate constant is decreased when the feed flowrate is decreased as well. Thus, showing that the
rate of chemical reaction at constant temperature depends only on the concentrations of the
substances that influence the rate according to the law of mass action.

The rate of reaction, -rA is also determined after the rate of reaction has been
calculated. The rate of reaction for 250 mL/min is 0.0002720 mol/L.min while 0.002879
mol/L.min is the rate of reaction for 200 mL/min. For flow rate 150 mL/min, the rate of
reaction is 0.003060 mol/L.min, 0.003067 and 0.003100 mol/L.min is the rate of reaction for
flow rate 10 and 50 mL/min. It indicates that when the reaction rate constant is decreases, the
rate of reaction is also decreases. The specific rate constant is proportionally constant relating
the rate of the reactions to the concentrations of reactants. A rate law is an expression
showing the relationship of the reaction rate to the concentrations of each reactants.

LAB REPORT ON PLUG FLOW REACTOR (L5) 20

10.0 CONCLUSION

From the experiment above, the flowrate of the sodium hydroxide, NaOH and ethyl acetate,
Et(Ac) is 250mL/min, 200mL/min, 150mL/min, 100mL/min and 50mL/min. The residence
time for each flowrate is 8 min, 10 min, 13.3333 min, 20 min and 40 min, respectively. The
conversion of the reactant to product is 68%, 64%, 57.2%, 56.8% and 54.4%, respectively.
The reaction rate constant, k is 2.6563 L/mol.min, 2.2222 L/mol.min, 1.6706 L/mol.min,
1.6435 L/mol.min and 1.4912 L/mol.min, respectively. The rate of reaction, -r A is 0.002720
mol/L.min, 0.002879 mol/L.min, 0.003060 mol/L.min, 0.003067 mol/L.min and 0.003100
mol/L.min, respectively. The rate of reaction decreases as the reaction rate constant
decreases. Higher flowrate of reactant increases the rate of reaction and thus, increasing the
conversion rate of the reactant to product.

LAB REPORT ON PLUG FLOW REACTOR (L5) 21

11.0 RECOMMENDATIONS

There are several precautions and recommendations that we can do to ensure more accurate
and reliable results. Which is:

1) Repeat the trials at least three times and calculate the average results to get a more
accurate data.
2) Always make sure that the start-up procedure and shut down procedure was done
correctly to prevent damage at the equipment.
3) The flow rates of the inlet need to be kept constant by monitor it at all times because
the flow rates will affect the collected data.
4) Glass apparatus need to be handle carefully to prevent it from broken while
conducting experiment.
5) Make sure to wear the Personal Protective Equipment (PPE) while conducting the
titration as we handling the chemicals.

LAB REPORT ON PLUG FLOW REACTOR (L5) 22

12.0 REFERENCES

Alqurri, S. (7 Jun, 2017). Tubular reactor. Retrieved from Slide Share:

https://www.slideshare.net/saidalqurri/tubular-reactor
Engineering, F. o. (n.d.). Lab Report Plug Fow Reactor. UiTM Shah Alam.
Fogler, H. S. (2006). Element of Chemical Reaction Engineering. Michigan: Prentice Hall.
Plug flow reactor model. (n.d.). Retrieved from Wikipedia:
https://en.wikipedia.org/wiki/Plug_flow_reactor_model
Rodgers, T. (2013). Chemical Reaction Engineering. Retrieved from
https://personalpages.manchester.ac.uk/staff/tom.rodgers/documents/CRE_Notes.pdf

LAB REPORT ON PLUG FLOW REACTOR (L5) 23

13.0 APPENDICES

LAB REPORT ON PLUG FLOW REACTOR (L5) 24