TABLE OF CONTENT

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

Title
Abstract.
Introduction..
Objectives..
Theory...
Material And Apparatus
Methodology.
Data and Results
Calculations...
Discussion.
Conclusion.
Recommendations.
Reference...
Appendix...

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

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12 13
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Page 1

1.0 ABSTRACT
The experiment is carry out with the reaction of Sodium Hydroxide NaOH and Ethyl Acetate,
Et(Ac) to determine the effect of residence time to the conversion of the solution. This
experiment is conducted to determine the rate law using tubular flow reactor data and to
demonstrate the temperature dependence of the reaction and the rate constant. This experiment
are conducted in the SOLTEQ Tubular Flow Reactor (Model: BP 101). The solution were
reacted in a PFR and the data was tabulated. The graph of the conversion against residence time
were also constructed. The result for this experiment is shown that the residence time are linearly
proportional to the conversion. The objective for this experiment was achieved.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 2

2.0 INTRODUCTION
The chemical reactors are something that is crucial and important in a chemical industries. It is
the most important things as it is the place for the reaction to happen. The type of reactor must be
suited with the reaction that we seek for. One of the example of the reactors is Plug Flow Reactor
(PFR)
The Plug Flow Reactor (PFR) can also be named as Turbulent Flow Reactor (TBR) or
Piston Flow Reactor. It used for reaction in continuous, flowing systems in a shape of cylinder.
The solution that flow in the reactor are describe as Plugs. An ideal plug flow reactor has a fixed
residence time: Any fluid (plug) that enters the reactor at time
, where

will exit the reactor at time,

is the residence time of the reactor.

Plug Flow Reactor are usually used for a large scale production, slow reactions, and
continuous reaction. Besides that, high temperature reaction usually done in the PFR. This is
because the PFR can withstand the high temperature of a reaction. PFR have a high volumetric
unit conversion and can run for a long periods of time without maintenance. That is why it is
widely used in the manufacturing of chemicals.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 3

3.0

OBJECTIVE

1) To determine the rate law using tubular flow reactor data.

2) To demonstrate the temperature dependence of the reaction and the rate constant.
3) To understand tubular flow reactor performance and application.
4) To construct the graph of Conversion against Residence Time.
5) To calculate the residence by using the formula.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 4

4.0 THEORY
The chemical reaction is consider as
aA + bBcC + dD
Residence time, is the average amount of time that a particle spends in a particular
system. The residence time, is a representation of how long it takes for the concentration to
significantly change in the sediment.

Where VTFR is the reactor volume and v0 is the total feed flow rate. In this experiment, we adjust
the pump until the flow rate become constant. The flow rate for each experiment is variable but
the reactor volume remain constant for every experiment.
Conversion is an improved way of quantifying exactly how far has the reaction moved, or
how many moles of products are formed for every mole of A has consumed. Conversion XA is
the number of moles of A that have reacted per mole of A fed to the system.
XA

moles of A reacted
moles of A fed

A reaction rate constant, k quantifies the rate of a chemical reaction. The reaction rate is
often found to have the form
rA kC A C B

Where C A and C B are the concentration of the species A and B respectively, each raised to the
powers and , while k is the reaction rate constant. The exponents and are the partial
reaction orders. In this experiment, we can calculate the reaction rate constant, k by the following
formula.
(

Where, k is the reaction rate constant,

the total inlet flow rate of solutions,
reactor volume,
is the inlet concentration of reactant NaOH in the reactor, and
percentage of conversion.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

is the
is the

Page 5

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

formation of products. Rate of reaction can describe about how fast a number of moles of one
chemical species reaction to form another species. Rate of reaction of each species corresponds
respectively to their stoichiometric coefficient. As such
rA rB rC rD

a
b
c
d

The negative sign indicates reactants while the positive sign indicates products.
A usual equation for rate of reaction is
rA k AC ACB

Where C A and C B are the concentration of the species A and B respectively, each raised to the
powers and , while kA is the reaction rate constant. The exponents and are the partial
reaction orders. The overall order of reaction is given by the following:
n

In the experiment that we had done, the and is 1 each. The overall order is 2 and the
experiment is second order. So, we had use the following formula to find the rate of reaction.
Since CA0 = CB0 ,
(

(
(

))
)

Tubular reactors are one type of flow reactors. It has continuous inflow and outflow of
materials. In the tubular reactor, 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 stirring prevent complete mixing of the
fluid in the tube.
In an ideal tubular flow reactor, which is called plug 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.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 6

5.0 MATERIAL AND APPARATUS

5.1

MATERIAL
1) Ethyl Acetate
2) Sodium Hydroxide
3) Water

5.2

APPARATUS
1) Tubular reactor (R1)
i. Stainless steel coil
ii. Volume: approx. 0.4-L
2) Water jacket (B4)
i. Cylindrical vessel made of borosilicate glass
ii. Capacity: approx. 10-L
iii. 2x1.0 kW cartridge heater
iv. Cooling tubes
v. Stirrer:50 2000 rpm with LCD display
a. max. torque 30 Ncm
b. 230VAC / 50-60 Hz / 75 W
c. Circulation pump (P3)
3) Feed tanks (B1, B2)
i. 20-L cylindrical vessels made of stainless steel
ii. Water de-ionizer fitted to tank B1
4) Waste tank (B3)
i. 60-L rectangular tank made of stainless steel
5) Pre-heater (B5)
i. 3-L cylindrical vessel made of stainless steel
ii. Internal coils for each reactants
6) Feed pumps (P1, P2)
i. Centrifugal pumps
ii. Max delivery rate: 1 usgpm (3.78 LPM)
iii. Max delivery height: 25 psi
iv. Power: 12V

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 7

7) Instrumentations
Flow measurements (FI-01, FI-02)
Temperature measurements (TIC-01, TI-02)
Conductivity measurements (QI-01, QI-02)
Valves and Instruments List
Valves list:
Tag
V1
V2
V3
V4
V5
V6
V7
V8
V9
V10
V11
V12
V13
V14
V15
V16

Location
Drain valve for feed tank B1
Inlet valve for pump P1
De-ionized water supply to feed tank B1
Drain valve for feed tank B2
Inlet valve for pump P2
Valve for feed inlet to reactor from FI 01
Drain valve for FI 01
Valve for feed inlet to reactor from FI 02
Drain valve for FI 02
Drain valve for water jacket B4
Drain valve
By-pass valve for pump P3
Inlet flow for pre-heater B5
Sampling valve
Sampling valve
Drain valve

V17

Cooling water outlet

Initial position
Close
Close
Close
Close
Close
Close
Close
Close
Close
Close
Close
Close
Close
Open
Close
Close
Close

Instruments list:
Tag
FI 01
FI 02
QI 01
QI 02
TIC
01
TI 02

Description
Liquid flow meter
Liquid flow meter
Conductivity
Conductivity

Units
L/min
L/min
mS/cm
mS/cm

Range
0.0 3
0.0 3
0.0 200.0
0.0 200.0

Accuracy
2%
2%
1% FS
1% FS

Temperature controller

0.0 100.0

0.5C

Pre-heater temperature

0.0 100.0

0.5C

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 8

FI
02

FI
01
V8

V3

V9

Sampling

V15

Feed
Tank
B1

V6

QI
02

V7

QI
01

Vent

LS1

M1

Pre-heater
B5
(3-L)
Waste Tank
B3
(60-L)

V2
TI
02

Tubular
Reactor
R1
(0.4-L)

Drain V16

V1

Drain

Pump
P1

Water
Jacket
B4
(10-L)

Feed
Tank
B2

In
V17

LS2
Out

V14
Electrical
Cart. Heater

W1, W2

(2x1.0 kW)

TIC
01

V10

Drain V11

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

V5

V4

Drain

Pump
P2

V13
V12
Sampling

Pump
P3

Page 9

c.w.
Water
De-ionizer

6.0 METHODOLOGY
6.1

General Start-Up Procedures

1) All valves were initially closed except valves V16.
2) The following solution were prepared::
i) 20 liter of sodium hydroxide, NaOH (0.1 M)
ii) 20 liter of ethyl acetate, Et(Ac) (0.1 M)
3) The feed tank B1 was filled with the NaOH solution and feed tank B2 with the Et(Ac)
solution.
4) Valve, V17 was opened. V10 and V11 were opened until water jacket, B4 is fill on
with 4 L of water. V11 was closed and valve V10, V12 and V13 were opened.
5) Pump, P3 was opened and was allowed clean water to flow through Pre-heater B5
with clean water by opening valve V10, V11, V12 and V13. The vent valve must be
open.
6) The power for the control panel was turned on. Valves V2, V5, V6 and V8 were
opened.
7) Both pumps P1 and P2 were switched on. P1 and P2 were adjusted to obtain flow of
approximately 0.30 L/min at both flow meters FI 01 and FI 02. Both flow rates must
be the same.
8) Both solutions were allowed to flow through the reactor R1 and overflow into the
waste tank B3.
9) Pump P3 was switched on to circulate the water through pre-heater B5. The stirrer
motor was switched on and the speed was set to about 200 rpm to ensure
homogeneous water jacket temperature.(Note: Pre-caution, the water level must be
higher than the heater.)
10) For experiment, the following additional steps were performed:
i) The heater was switched on.
ii) Valve V17 was opened to let the cooling water to flow through the cooling
tubes. The water supply valve was adjusted to obtain reasonable cooling water
flow in order to minimize the temperature overshoot at the TI 01 during heater
cut-off.
iii) The temperature set point on TI 01 was set to the desired temperature.
11) The unit was ready for experiment.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 10

6.2

General Shut-Down Procedures

1) Pumps P1, P2 and P3 were switched off. Valves V2 and V5 were closed.
2) The heater was switched off.
3) The cooling water kept circulating through the reactor while the stirrer motor was
running to allow the water jacket to cool down to room temperature.
4) The stirrer and the cooling water were off.
5) If the equipment is not going to be used for long period of time, all liquid were
drained from the unit by opening valves V1 to V17. The feed tanks were rinsed with
clean water.
6) The power for the control panel was turned off.

6.3

Experiment Procedures
1) The general start-up procedures were performed.
2) Valves V6 and V8 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 0.30 L/min at flow
meters FI 01 and FI 02. Both flow rates must be the same. The flow rates were
recorded.
5) Start monitoring 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 were found out
from the calibration curve.
7) Optional: Sampling valve V15 was opened and a 50 ml sample was collected. A back
titration procedure was carried out to manually determine the concentration of NaOH
in the reactor and extent of conversion.
8) The experiment (steps 4 to 7) was repeated for different residence times by reducing
the feed flow rates of NaOH and Et(Ac) to about 0.25, 0.20, 0.15, 0.10 and 0.05
l/min. Both flow rates must be the same.
9) The general shutdown procedures were performed.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

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7.0 DATA AND RESULTS

No

1
2
3
4
5
6

No

1
2
3
4
5
6

Volume,
VTFR
(L)
4
4
4
4
4
4

Flow rate of
NaOH
(L/min)
0.30
0.25
0.20
0.15
0.10
0.05

Inlet
Outlet
Conductivity Conductivity
(mS/cm)
(mS/cm)
17.00
11.50
16.50
10.70
16.30
10.50
15.60
9.90
13.70
9.60
12.60
8.70

Flow rate of
Et(Ac)
(L/min)
0.30
0.25
0.20
0.15
0.10
0.05

Total Flow Rate

of solutions,
(L/min)
0.60
0.50
0.40
0.30
0.20
0.10

Residence
Time,
(min)
6.6667
8.0000
10.0000
13.3333
20.0000
40.0000

Conversion, X
(%)

Reaction Rate
Constant, k
(L/mol.min)
0.0000
8.8117 x 10-3
1.6260 x 10-2
2.5281 x 10-2
3.4883 x 10-2
4.8701 x 10-2

Rate of
Reaction
(mol/L.min)
0.0000
8.6888 x 10-5
1.5744 x 10-4
2.3659 x 10-4
3.0481 x 10-4
3.4115 x 10-4

0.0000
0.7000
1.6000
3.2609
6.5217
16.3043

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 12

Graph of Conversion Against Residence Time

Conversion

Linear (Conversion)

18

16

14

Conversion (%)

12

10

2
1.6
0.7

0
0

5
6.66
7

10
8.00

15

20

25

30

35

40

45

Residence Time (min)

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

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8.0

CALCULATIONS

Sample Calculation for residence time,

No
1

Calculations

No
4

Calculations

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 14

Sample Calculation for Conversion, X

Conversion
0%
25%
50%
75%
100%
No

Solution Mixtures
0.1 M NaOH 0.1 M Na(Ac)
H2 O
100 ml
100 ml
75 ml
25 ml 100 ml
50 ml
50 ml 100 ml
25 ml
75 ml 100 ml
100 ml 100 ml

From the Graph of Conversion

Against Residence Time

No

Concentration
of NaOH (M)
0.0500
0.0375
0.0250
0.0125
0.0000

Conductivity
(mS/cm)
10.2
7.9
6.2
5.1
3.9

Calculations

4
(
(

)
)
%

5
(
(

)
)

(
(

)
)

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 15

Sample Calculation for The Reaction Rate Constant, k

Where,
k
= Reaction rate constant
= Total inlet flow rate of solutions (ml/min)
= Reactor volume (ml)
= Inlet concentration of reactant NaOH in the reactor (mol/L)
= Conversion (%)
No
1

Calculations

)(

)(

)(

4
(

)(

5
(

)(

)(

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 16

Sample Calculation for Rate of Reaction,

Since CA0 = CB0 ,

(

(
(

No
1

))
)

Calculations
(

)(

) (

2
(

)(

) (

)(

) (

)(

) (

)(

) (

)(

) (

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 17

9.0

DISCUSSION
Calibration Curve of Conductivity Vs Conversion
12

Conductivity (mS)

10

9.7

8
6
4

3.7

2
0
0%

20%

40%

60%
80%
Conversion, X (%)

100%

120%

The graph shows that the conductivity is inversely proportional with the conversion.
Conductivity decreases as the conversion increases. This graph shows the theotherical value and
relationship between conversion and conductivity. Based on the graph, we can relate
conductivity and conversion into linear equation where,
y = mx + c
Where, y = The Conductivity (mS)
x = The Conversion , X (%)
m = The gradient (slope)
c = The y-intercept
The gradient (slope) of the graph ,

The y-intercept of the graph,

Thus, the linear equation of the graph is

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 18

Graph of Conductivity Vs Conversion

14
12

Conductivity (mS/cm)

10.8

10
8.4

8
6
4
2
0

8
10
Conversion, X (%)

12

14

16

18

The graph shows experimental value which the recorded conductivity is inversely
proportional with the conversion calculated. The conductivity decreases as the conversion
increases. However, when compared to the theotherical graph, we can conclude that the
experimental value deviated from the theory. Therefore , the linear equation from the
experimental value is also deviated from the theory, where,
y = mx + c
Where, y = The Conductivity (mS)
x = The Conversion , X (%)
m = The gradient (slope)
c = The y-intercept
The gradient (slope) of the graph ,

The y-intercept of the graph,

Thus, the linear equation of the graph is

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 19

In order to determine the conversion of NaOH, the value of the conductivity is taken as
the guidelines. However, since a few data taken for the conductivity falls a bit higher than in the
theotherical value, extrapolation of graph is needed to determine the value of conversion at the
respected residence time. Thus, the following graph is plotted to determine the conversion and to
determine the relationship between conversion and the residence time.

Graph of Conversion Against Residence Time

Conversion

Linear (Conversion)

18
16

Conversion (%)

14
12
10
8
6
4
1.6
0.7

2
0
0

10

6.66
7

8.00

15

20

25

30

35

40

45

Residence Time (min)

The graph shows that the conversion is directly proportional with the residence time. The
conversion increases as the residence time increases. Residence times refer to the time taken
needed to process one volume of the reactor fluid at the entrance condition where as the
conversion refers to how many moles of products are formed for every mole of NaOH
consumed.
Three values of conversion which are 0.0% at 6.6667 min, 0.7% at 8 min and 1.6% at 10
min are recorded from the extrapolation of the graph. Conversion data table need to be
completed in order to calculate the reaction rate constant which will lead us to the final objective
of the experiment which is to determine the rate of reaction of the experiment.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 20

Plug flow reactor (PFR) or Turbulent flow reactor (TFR) is a reactor for chemical
reactions in a continuous, flowing system in a shape of cylindrical. The fluid going through the
reactor are refers as a plugs, each with a fix and uniform volume. The fluid or solution in the
reactor is well mixed. The residence time of the plug is a position of the fluid in the reactor. The
volume of solution that flow into the reactor equal to the volume of the solution out from the
solution.
In this experiment, we used NaOH and Et(Ac). The Hydrolysis of Ethyl Acetate is one of
the most well-known reactions as model example for second order reaction. These solution are
mixed together into the Plug Flow Reactor (PFR). Based on the result that we have collected, the
residence time can be calculated and be include in the table. The lower the total flow rate of
solutions, the higher the residence time for each test. The residence time is the amount of time
the particles spends in the particular system. The residence time is affected by the flow rate of
the solution in the Tubular Flow Reactor.

Graph of Residence Time vs Flow rates

45
Residence Time (min)

40
35
30
25
20
15
10
5
0
0

0.1

0.2

0.3
0.4
Flow Rates, ( L/min)

0.5

0.6

0.7

The graph shows that the residence time is inversely proportional with the flow rates. As
the flow rates increases, the residence time decreases.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 21

Due to the less concentration that we used, the longer the residence time for the solution
in the reactor. The less the concentration, thus less the collision kinetic between the particles to
produce the product of the saponification process, Sodium acetate, CH3COONa, and Ethyl
Alcohol, C2H5OH. The General Equation for this saponification reaction are
CH3COOC2H5 + NaOH CH3COONa + C2H5OH
We also observed that the Inlet conductivity and the outlet conductivity is decreasing
going along with the decreasing flow meter. The conductivity or specific conductance is a
measure of ability of an electrolyte or a solution to conduct electricity. The conductivity is
decreasing due to the less ionic content in the water. This explained the result for decreasing
conductivity that we recorded at the reactor. Due to the less concentration of the solutions going
down the table that we tabulate, the conductivity can be seem decreasing too.
The conversion, x, can be calculated by using the formula X=Moles of Reacted/Moles of
Feed. Conversion is the ratio of the feed used or the ratio the product formed. In this case the
product formed is Sodium Acetate and the Ethyl Alcohol. After calculated the conversion for all
flowrate, the conversion become increase the longer it resides in the reactor.
The reaction rate constant, k or also can be called as Kinetic Constant. This constant can
be calculated by using a formula. This is a second order reaction, therefore the unit for the
constant are Liter Mole-1 Min-1. The rate of reaction, -ra are calculated with the formula also and
shown on the sample calculation and the table. The rate of reaction for the second law are
or

After derive the equation, we can calculate the rate of reaction by using the data that we
collected from the reactor, rate constant, k and the conversion, X.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 22

10.0 CONCLUSION
From the experiment, we were able to found out a saponification between Sodium
Hydroxide, NaOH and Ethyl Acetate, Et(Ac) in tubular flow reactor, TFR. By using a Plug Flow
Reactor, PFR, both Sodium Hydroxide, NaOH and Ethyl Acetate, Et(Ac) were flowed into the
reactor, mixed and let to react for a certain period of time. By doing that, saponification process
was completed.
Next, we were able to determine the reaction rate constant. This was done by calculating
the reaction rate as seen in the Sample Calculation section. The value of the reaction rate
constant that we get was 0.0000 L/mol.min, 8.8117x10-3 L/mol.min, 1.6260x10-2 L/mol.min,
2.5281x10-2 L/mol.min, 3.4883x10-2 L/mol.min and 4.8701x10-2 L/mol.min respectively.
Last but not least, we able to determine the effect of residence time on the conversion in a
TFR. Thus, we were able to plot graph of conversion, X against residence time.
We can conclude that the experiment was successfully conducted since we were able to
fulfill the objective of this experiment.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

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11.0 RECOMMENDATION
Experimenters need to fully understand the procedure of the experiment in order to avoid
making mistakes that should not ever happen during the experiment. This can be done by reading
the lab manual over and over again in order to grasp what the experiment is all about and how to
make sure that the experiment went well.

In order to make sure that the data collected is accurate, the experiment needs to be done
repeatedly for at least three times per experiment. This is to ensure that the data taken is not fall
far from the data theory. Then, the average value taken is used for the calculation involved in the
experiment. Besides, the values should be taken in approximately 4 decimal places so that the
data will be more precise and accurate.

When conducting the experiment there are some errors where the data deviate from the
theoretical value. The reason of the errors could be because the time interface for the value of
conductivity at inlet and outlet to be stable is too short. Since there are quite few times where the
value seems to already stabilize but actually are not and the data might have been taken during
that particular time which then lead to the deviation from the theoretical value of the
conductivity. Therefore, experimenters should be more aware about the time and be carefull not
to misunderstand which value needs to be taken into account.
Other than that, student should follow the rules and guidelines before doing the
experiment. They need to wear lab coat, gloves and wear shoes for safety purposes. They also
need to make sure they alert with the precautions mention in the lab manual and never play
around during the experiment being conduct.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 24

12.0 REFERENCES
Books
1) Levenspiel O., Chemical Reaction Engineering, John Wiley (USA), 1972.
2) Fogler H.S. , Elements of Chemical Reaction Engineering, 3rd Ed., Prentice Hall
(USA) , 1999.
3) Smith J.M., Chemical Engineering Kinetics, McGraw Hill (Singapore), 1981.
4) Astarita G., Mass Transfer With Chemical Reaction, Elsevier, 1967.

5) Scott Fogler ,Element of Chemical reaction Engineering, Fourth Edition H., Pearson
International Edition, 2006 Pearson Education, Inc.

Web
1) Batch Reactor Kinetic Analysis. Jan 15, 2005.
www.csupomona.edu/~tknguyen/che435/Notes/P5-kinetic.pdf , retrieved in August
2015.
2) Wikipedia , https://en.wikipedia.org/wiki/Plug_flow_reactor_model ,retrieved in
August.

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 25

13 APPENDIX

Tubular Flow Reactor (TFR)

EFFECT OF RESIDENCE TIME ON THE REACTION IN TFR

Page 26