Group # 3

PPE-315L Polymer Reaction Engineering Lab

Determine the effect of residence time on the conversion in a tubular flow reactor.

SUBMITTED TO:
Ma’am. NIDA ABID

SUBMITTED BY:

FAIQUA JABEEN (2019-PE-7)

MARYAM MAHER (2019-PE-16)
JAVERIA KHALID (2019-PE-23)
HOOR BAIG (2019-PE-25)
MARYAM SALEEM (2019-PE-30)

Polymer and Process Engineering

University of Engineering and Technology, Lahore
 Group # 3

ABSTARCT
The experiment is carried out with the reaction of Sodium Hydroxide (NaOH) with 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. The experiment is
conducted in the Tubular Flow Reactor. The solutions were reacted in a PFR and the data was
tabulated. The graph of the conversion against residence time were also constructed. It was
concluded from results that that the residence time is linearly proportional to the conversion.
 Group # 3

Table of Contents
LIST OF FIGURES...........................................................................................................................

1.0 OBJECTIVE..............................................................................................................................1

2.0 APPARATAUS.........................................................................................................................1

2.1 REAGENTS..............................................................................................................................1

3.0 INTRODUCTION.....................................................................................................................1

4.0 THEORY...................................................................................................................................2

Reaction.......................................................................................................................................2

Residence time distribution.........................................................................................................2

Conversion...................................................................................................................................2

Rate of reaction............................................................................................................................3

Reaction rate constant..................................................................................................................4

5.0 CONSTRUCTION....................................................................................................................5

Laboratory Equipment.................................................................................................................5

Schematic diagram.......................................................................................................................6

6.0 APPLICATIONS.......................................................................................................................6

7.0 PROCEDURE............................................................................................................................7

8.0 OBSERVATION AND CALCULATIONS..............................................................................8

9.0 RESULT AND DISSCUSSION..............................................................................................14

10.0 CONCLUSION......................................................................................................................16

REFERENCES..............................................................................................................................17
 Group # 3

LIST OF FIGURES
Figure 1 Saphonification reaction....................................................................................................2
Figure 2 Laboratory tubular flow reactor........................................................................................5
Figure 3 Schematic diagram for laboratory tubular reactor setup...................................................6
Figure 4 Conversion vs residence time..........................................................................................14
Figure 5 Flowrate vs residence time..............................................................................................15
 Group # 3

1.0 OBJECTIVE
The objective of performing this experiment are;

 To understand tubular flow reactor performance and application.

 To construct the graph of Conversion against Residence Time.
 To calculate the residence by using the formula.

2.0 APPARATAUS
 Tubular reactor
 Water jackets
 Feed tanks
 Waste tank
 Pre-heater
 Feed pumps

2.1 REAGENTS
 Sodium hydroxide
 Ethyl acetate
 Water

3.0 INTRODUCTION
The tubular flow reactor (TFR) also known as the plug flow reactor (PFR) is used in
chemical reactions that occur in liquid phase under isothermal adiabatic conditions. The fluid
flows in it is continuous and in controlled manner. Tubular reactor is relevant to the batch reactor
because it provides the high driving force which continuously decreases the reaction down the
tube.

In ideal tubular reactor, the reaction time is same for the all the material flowing at the given
cross section of the tube. In the tubular flow reactor, the flow can be laminar for the viscous fluid
or turbulent for gases.

1
 Group # 3

TFR is used for the large scale production, continuous reaction and slow reactions. The tubular
flow reactor or PFR can bear high temperature of the reaction. The advantages of tubular flow
reactor are high conversion rate per reactor volume, efficient use of reactor volume and good for
large capacity processes. The disadvantage of the TFR is that the control of reactor temperature
and composition variations is difficult[1].

4.0 THEORY
Reaction
The chemical reaction is

aA +bB → cC+ dD

Saponification reaction will take place as ethyl acetate reacts with sodium hydroxide;

Figure 1 Saphonification reaction[2]

Residence time distribution

The average time that particle spent in a particular system or reactor is called residence time of
particle in the reactor. The residence time distribution of a reactor is property of the mixing
which occur in the reactor. There is no axial mixing in the tubular reactor and this gap is
reflected in the RTD.

The residence timeτ , is a representation of how long it takes for the concentration to significantly
change in the sediment.

V TFR
τ=
νO

Where VTFR is the reactor volume and vo is the total feed flow rate.

2
 Group # 3

Conversion
Conversion is a way to define how many reaction convert during the reaction or how many
moles of products are formed for every mole of A consumed. Conversion X A is the number of
moles of A that have reacted per mole of A fed to the system.

moles of A reacted
X A=
moles of A fed

Rate of reaction
Rate of reaction is defined as the rate of disappearance of reactants or the rate of formation of
products[3]. Rate of reaction tells about how fast the number of moles of species reacts to form
another specie.

−r A −r B −r C −r D
= = =
a b c d

In this rate equation, negative sign shows reactants while the positive sign shows products[1].

The rate equation:

α β
−r A =k C A C B

Where;

 The exponents  and  are the partial reaction orders.

 CA and CB are the concentration of the species A and C respectively.
 k is the reaction rate constant.

The overall order of reaction is given by the following

n=α + β

As saponification reaction is is the second order reaction so, the rate of reaction will become;

−r A =k C A C B

Since CAO=CBO,

2
−r A =k C A

3
 Group # 3

2
−r A =k (C AO ( 1− X ))

−r A =k C 2AO ( 1−X )2

Reaction rate constant

The reaction rate constant k, can be calculated by the following formula:

υO X
k= ( )
V TFR C AO 1−X

Where;

 k is the reaction rate constant

 υ O the total inlet flow rate of solutions

 V TFR is the reactor volume

 C AO is the inlet concentration of reactant NaOH in the reactor

 X is the percentage of conversion[4].

4
 Group # 3

5.0 CONSTRUCTION
Tubular reactors consist of a cylindrical pipe with openings on each end for reactants and
products to flow through. Plugs of reactants are continuously fed into the reactor As the plug
flows down the reactor the reaction takes place, resulting in an axial concentration gradient.
Products and unreacted reactants flow out of the reactor continuously. Plug flow reactors may be
configured as one long tube or a number of shorter tubes. They range in diameter from a few
centimeters to several meters. The choice of diameter is based on construction cost, pumping
cost, the desired residence time, and heat transfer needs. Typically, long small diameter tubes are
used with high reaction rates and larger diameter tubes are used with slow reaction rates[5].

Laboratory Equipment

Figure 2 Laboratory tubular flow reactor

5
 Group # 3

Schematic diagram

Figure 3 Schematic diagram for laboratory tubular reactor setup

6.0 APPLICATIONS
Tubular reactors have a wide variety of applications in either gas or liquid phase systems.
Common industrial uses of tubular reactors are in

 Gasoline production
 Oil cracking
 Synthesis of ammonia from its elements

6
 Group # 3

 Oxidation of sulfur dioxide to sulfur trioxide.

 They can also be used as bioreactors for small scale production[5].

7.0 PROCEDURE
The steps needed to perform the experiment are;
 Prepare 20 liter of sodium hydroxide (NaOH ) 0.1 M and 20 liter of ethyl acetate (0.1 M)
solutions.
 Open the valve V6 and V8(Valves for feed inlet to reactors).
 Enter NaOH and Ethyl acetate solutions in plug reactor R1 and empty into the waste tank
B3.
 Adjust pumps (P1 and P2) for a constant flow rate of about 0.3 L/ min.
 Note-down the readings of flow rates.
 Approach 1 # Monitor inlet and outlet conductivity values until the reactors reaches
steady state.
 These values help in plotting calibration curve from which the concentration of NaOH
and
extent of conversion is determined.
 Approach 2 # Collect 50 ml sample and back titrate it to determine the concentration of
NaOH and extent of conversion.
 Repeat the experiment for different residence times by reducing the flow rates of NaOH
and ethyl acetate.
 After the experiment was performed switched off the pumps P1, P2 and P3 and inlet
Valves. Rinse the feed tanks with clean water.
 Turn off the power for control panel.

7
 Group # 3

8.0 OBSERVATION AND CALCULATIONS

Formulas used
Reactor Volume V TFR
Residence time τ=
Total Feed Rate v o

vo X
k= ( )
V TFR C AO 1−X

Where

K= reaction rate constant

v o= total inlet flow rate of solution

VTFR = reaction volume (ml)

CAO= Inlet concentration of reactant NaOH in the reactor (mol/L)

X= conversion (%)

Residence Time
Reactor Volume V TFR
Residence time τ=
Total Feed Rate v o

4L
Residence time τ=
0.6 L/min

¿ 6.6667 min

4L
Residence time τ=
0.5 L/min

¿ 8.00 min

4L
Residence time τ=
0.4 L/min

8
 Group # 3

¿ 10 min

4L
Residence time τ=
0.3 L/min

¿ 13.333 min

4L
Residence time τ=
0.2 L /min

¿ 20 min

4L
Residence time τ=
0.1 L /min

¿ 40 min

Sample calculation for the reaction rate constant, k

vo X
k= ( )
V TFR C AO 1−X

k=
0.60 L/ min
( 1−0.000000
0.000000
)
(
(4 L)
0.1 mol
L )
0.0000 L
¿
mol . min

k=
0.50 L/min
( 1−0.007
0.007
)
( 4 L)(0.1 mol
L )
8.8117 ×10−3 L
¿
mol . min

k=
0.40 L/min
( 1−0.016
0.016
)
(4 L) (
0.1 mol
L )
1.6260× 10−2 L
¿
mol . min

9
 Group # 3

k=
0.30 L /min
( 0.032609
)
( 4000 mL ) (0.1 mol
L ) 1−0.032609

2.5281×10−2 L
¿
mol . min

k=
0.20 L/ min
( 1−0.065217
0.065217
)
(
(4 L)
0.1 mol
L )
3.4883× 10−2 L
¿
mol . min

k=
0.10 L/min
( 1−0.165217
0.165217
)
(
(4 L)
0.1 mol
L )
−2
4.8701× 10 L
¿
mol . min

Sample calculation for rate of reaction, −r A

Since CA0=CB0

−r A =k C A C B

2
−r A =k C A

−r A =k ¿

2
−r A =k C A 0 ¿

−r A = ( mol .min )
0.0000 L
¿

0.000 mol
¿
L .min

( )
−3
8.8117 × 10 L
−r A = ¿
mol .min

10
 Group # 3

−5
8.6888× 10 mol
¿
L . min

( )
−2
1.6260 ×10 L
−r A = ¿
mol . min

1.5744 ×10−4 mol

¿
L . min

( )
−2
2.5281 ×10 L
−r A = ¿
mol . min

2.3659× 10−4 mol

¿
L . min

( )
−2
3.4883 ×10 L
−r A = ¿
mol . min

−4
3.0481×10 mol
¿
L . min

−r A = (
4.8701× 10−2 L
mol .min
¿ )
3.4115× 10−4 mol
¿
L . min

From graph of Conversion against residence time

X1 = 0%

X2 = 0.70%

X3 =1.60%

X 4 −0 % ( 9.90−10.2 ) mS /cm
= =3.26 %
25 %−0 % ( 7.9−10.2 ) mS /cm

X 5−0 % ( 9.60−10.2 ) mS /cm

= =6.52%
25 %−0 % ( 7.9−10.2 ) mS /cm

X 6−0 % ( 8.70−10.2 ) mS /cm

= =16.304 %
25 %−0 % ( 7.9−10.2 ) mS / cm
11
 Group # 3

Tables
 Residence time at various flow rates

Table 1 Residence time at various flow rates

No. of Volume Flow rate of Flow rate of Total flow rate of Residence Time
Obs VTFR NaOH Et (Ac) solutions τ
(L) (L/min) (L/min) Ѵo (min)
(L/min)
1 4 0.30 0.30 0.60 6.667
2 4 0.25 0.25 0.50 8.0
3 4 0.20 0.20 0.40 10.0
4 4 0.15 0.15 0.30 13.33
5 4 0.10 0.10 0.20 20.0
6 4 0.05 0.05 0.10 40.0

 Rate of reaction at varying residence time

Table 2 Rate of reaction at varying residence time

No. of Inlet Outlet Conversion Reaction Rate Rate of

Obs Conductivity Conductivity X Constant Reaction
(mS/cm) (mS/cm) (%) K (mol/L.min)
(L/mol.min)
1 17 11.5 0 0.0000 0.0000

12
 Group # 3

2 16.5 10.7 0.7 8.8117 x 10-3 8.6888 x 10-5

3 16.3 10.5 1.6 1.6260 x 10-2 1.5744 x 10-4
4 15.6 9.9 3.26 2.5281 x 10-2 2.3659 x 10-4
5 13.7 9.6 6.52 3.4883 x 10-2 3.0481 x 10-4
6 12.6 8.7 16.30 4.8701 x 10-2 3.4115 x 10-4

 Sample calculation for Conversion X

Table 3 Sample calculation for Conversion X
Conversion Solution Mixtures Concentration Conductivity
X (ml) of NaOH (mS/cm)
(%) 0.1 M 0.1 M H2O (M)
NaOH Na (Ac)
0 100 - 100 0.050 10.2
25 75 25 100 0.037 7.9
50 50 50 100 0.025 6.2
75 25 75 100 0.012 5.1
100 - 100 100 0 3.9

13
 Group # 3

9.0 RESULT AND DISSCUSSION

In order to control the conversion of NaOH, the value of the conductivity is taken as the
guidelines. The following graph is plotted to govern the conversion and to determine the
relationship between conversion and the residence time.

Conversion vs Residence time

18

16

14

12
Conversion (%)

10
X(%)
8 Linear (X(%))
6

0
5 10 15 20 25 30 35 40 45

Residence time (min)

Figure 4 Conversion vs residence time

The graph shows that the conversion is at proportional with the residence time. The conversion
increases because the residence time increases. This is because the more time reactants spend in
the reactor the more they react to form product and thus greater is the conversion.

14
 Group # 3

Residence time vs flowrate

45
40
35
Residence time (min)

30
25
Residence time
20
Linear (Residence time)
15
10
5
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7

Flow rate (L/min)

Figure 5 Flowrate vs residence time

The graph shows lower the entire flow rate of solutions, the higher the residence time for every
check. The residence time is stricken by the flow rate of the solution in the Tubular Flow
Reactor.

15
 Group # 3

10.0 CONCLUSION
From the results it has been observed that the objectives of the experiment are successfully
achieved. From experiment, saponification between Sodium Hydroxide, NaOH and Ethyl
Acetate, Et (Ac) in tubular reactor, TFR is determined. By the usage of a Plug Flow Reactor,
PFR, both Sodium Hydroxide, NaOH and Ethyl Acetate, Et (Ac) have been flowed into the
reactor, blended and permit to react for a certain time period. The rate of reaction and reaction
rate constant is determined. It was observed that as the residence time increases the conversion
increases determine the reaction rate constant.

16
 Group # 3

REFERENCES
1. Levenspiel, O., Chemical reaction engineering. 1998: John wiley & sons.
2. Helmenstine, A.M. Saponification. thought co January 08, 2020; Available from:
https://www.thoughtco.com/definition-of-saponification-605959.
3. Smith, J.M., Chemical engineering kinetics. 1981.
4. Fogler, H.S. and P.H. PTR, Elements of Chemical Reaction Engineering (Prentice Hall
International Series in the Physical and Chemical Engineering Sciences)(Hardcover).
2005.
5. Sam Catalano, A.W., Kelsey Kaplan, Thomas Plegue. Plug Flow Reactors. Visual
Encyclopedia of Chemical Engineering January 09, 2022]; Available from:
https://encyclopedia.che.engin.umich.edu/Pages/Reactors/PFR/PFR.html.

17