You are on page 1of 18

ABSTRACT

In chemical engineering, a chemical reactor can be define as a container where reaction between
two or more chemical component or compound take place. A chemical reactor design deals with
multiple aspects of chemical engineering and chemical reactions. A plug flow reactor (PFR) is
one of the example of a reactors. In this experiment, the main objective is to investigate or study
the effect of residence time against conversion. There are two chemicals compounds that were
used in this experiment that is 0.1M sodium hydroxide (NaOH) and ethyl acetate (Et(AC)).
Besides that, from this experiment, data can also being obtain are reaction rate constant and rate
of reaction. The experiment were done in six different total flowrates that are 600 mL, 500 mL,
400 mL, 300 mL, 200 mL, and 100 mL. At the beginning of the experiment with total flowrate is
600 mL, the conversion of NaOH is 83.6% while at 500 mL the conversion is 82.0%. Both
flowrates have different residence time that is 6.6667 minutes for 600 mL and 8 minutes for 500
mL. The residence time for the rest of the flowrate are 10, 13.3333, 20 and 40 minutes with
conversion of 82.4%, 83.6%, 88.4% and 83.2% for flowrates of 400 mL, 300mL, 200mL and
100 mL respectively.

1 | Page

INTRODUCTION
In chemical engineering, a chemical reactor was used as a container-like to contain chemical
reaction in it. A chemical reactor design deals with multiple aspects of chemical engineering and
chemical reactions. The designer will always ensure that the reaction held in the reactor proceeds
with the highest efficiency towards the desired output product, producing the hifhest yield of
product that required the least amount of money to purchase and operate (Schmidt and Lanny,
1998)
A plug flow reactor (PFR), 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, namely in both radial and axial directions.

Plug flow conditions means that all the material processed through the reactor must have
the same residence time so that the chemicals exiting the reactor have witnessed the same
reaction conditions of reactive species contact-time aging-temperature history.

2 | Page

OBJECTIVE

To determine the effect of residence time on the conversion


To determine the reaction rate constant
To determine the rate of reaction

THEORY
Rate of Reaction and Rate Law
Simply put, rate of reaction can be roughly define as the rate of disappearance of reactants or the
rate of formation of products. When a chemical reaction is said to occur, a reactant diminishes
and a product produces, this is what constitutes a chemical reaction. For example:
aA+ bB

cC+ dD

A and B represent reactants while C and D represent products. In this reaction, A and B is being
diminished and C and D is being produced. Rate of reaction, concerns it with how fast the
reactants diminished or how fast the product id formed. Rate of reaction of each species
corresponds respectively to their stoichiometric coefficient. As such:
r A r B r C r D
=
= =
a
b
c d
The negative sign indicates reactants.
A usual equation for rA is:
r A=k C A C B
Where:
K = rate constant

= stoichiometric coefficient of A

CA = concentration of A species

= stoichiometric coefficient of B

CB = concentration of B species

3 | Page

Conversion
Taking species A as the basis, the reaction expression can be devided through the stoichiometric
coefficient of species A, hence the reaction expression can be arranged as follows:
b
c
d
A + B+ C + D
a
a
a
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. As show below:
X A=

moles of A reacted
mole of A fed

Plug Flow Reactor


The reactor is also known as tubular flow reactor which is usually used in industry
complementary to CSTR. It consist of a cylindrical pipe and is usually operated at steady state.
For analytical purpose, the flow in the system is considered to be highly turbulent and may be
modelled by that of a plug flow. Therefore, there is no radial variation in concentration along the
pipe.
In a plug flow 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 of provision for stirring prevent complete
mixing of the fluid in the tube. Hence the properties of the following stream will vary from one
point to another.
In an ideal tubular flow reactor, which is called plug flow reactor, specific assumption 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

4 | Page

Residence Time Distribution Function


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

5 | Page

APPARATUS
The unit used in the experiment is SOLTEQ Plug Flow Reactor (Model: BP101)

heate

Control

Pump 2
reactor
Pump 1

Waste
tank

The apparatus used in this experiment:


1.
2.
3.
4.

Conical flask
Measuring cylinder
Beakers
Burrette

6 | Page

PROCEDURE
OPERATING PROCEDURE
General start-up procedure
1. Make sure all valves are initially closed except for valves V4, V8 and V17.
2. The solution were prepared as followed:
a. 20 liters of sodium hydroxide, NaOH (0.1M)
b. 20 liters of ethyl acetate, Et(Ac) (0.1M)
c. 1 liter of hydrochloric acid, HCl (0.25M), for quenching
3. The feed tank B1 was filled with NaOH solution and B2 tank with Et(Ac) solution.
4. The water jacket B4 was filled and pre-heated B5 with clean water.
5. Switched on the control panel.
6. Valves V2, V4, V6, V8, V9 and V11 were open.
7. The both pumps P1 and P2 ware switched on.
8. P1 and P2 were adjusted to obtain approximately 300 ml/min at both flow meter FI-01
and FI-02.
9. Both solution were allowed to circulate into the reactor and overflow into the waste tank.
10. The valve V13 and V18 were opened. The pump P3 was switched on to circulate the
water through pre-heater B5. The stirrer motor M1 was switched on and the speed was set
around 200 rpm to ensure homogenous water jacket temperature.
11. The unit now ware ready for experiment.
General shut down procedure
1. All pump P1, P2 and P3 were switched off. The valve V2 and V6 were closed.
2. The heater were switched off.
3. The cooling water was keep to circulating though the reactor while the stirrer motor is
running to allowed the water jacket to cool down to room temperature.
4. If the equipment was not going to be used for long period of time, drain all liquid from
the unit by opening valves V1 to V19.
5. Rinsed the feed tank with distilled water.
6. The power for control panel were switched off.
A. Preparation Of Calibration Curve For Conversion Vs. Conductivity
1. The following solution were prepared:
a) 1 liter of sodium hydroxide, NaOH (0.1M).
b) 1 liter of ethyl acetate, Et(Ac) (0.1M).
c) 1 liter deionized water, H20.

7 | Page

2. The conductivity and NaOH concentration were determine for each conversion values
by mixing the following solutions into 100ml of deionized water:
a) 0% conversion 100 ml NaOH
b) 25% conversion 75 ml NaOH + 25 ml Et(Ac)
c) 50% conversion 50 ml NaOH + 50 ml Et(Ac)
d) 75% conversion 25 ml NaOH + 75 ml Et(Ac)
e) 100% conversion 100 ml Et(Ac)
B. Back Titration Procedure For Manual Conversion Determination
1. Filled up burrette with 0.1M of NaOH.
2. 10 ml of 0.25M HCl in a flask was measured.
3. A 50 ml sample was obtain from the experiment and immediately added the sample to
the HCl in the flask to quench the saponification reaction.
4. A few drops of pH indicator were added to the mixture.
5. The mixture were titrated with NaOH till the solution changed color from colorless to
pink. The initial and final reading were recoreded.
Experiment 3: Effects Of Residence Time On The Reaction
1. The general start-up procedure were perfomed.
2. Valve V9 and V11 were opened.
3. The both NaOH and ET(Ac) solution was allowed to enter the plug reactor R1 and empty
into the waste tank.
4. The P1 and P2 were adjusted to give a constant flow rate of about 300 ml/min at flow
meter FI-01 and FI-02. Make sure the both flow rate was same and recorded the data.
5. The inlet and outlet conductivity values were monitored until they do not change over
time to ensure that the reactor has reached steady state.
6. Open sampling valve V15 and sample 50 ml were collected. A back titration procedure
was carrying out to manually determine the concentration of NaOH in the reactor and
extent of conversion.
7. The experiment was repeated for different resideance time by reducing the feed flow rate
of NaOH and Et(Ac) to about 250, 200, 150, 100 and 50 ml/min. make sure that both
flow rates are the same for P1 and P2.

8 | Page

RESULT
PREPARATION OF CALIBRATION CURVE
Solution Mixtures
Conversion
(%)

Concentratio
n of NaOH
(M)

Conductivity
(mS/cm)

0.1 M NaOH

0.1 M Et(Ac)

H20

100

100

0.0500

9.780

25

75

25

100

0.0375

6.540

50

50

50

100

0.0250

3.960

9 | Page

75

25

75

100

0.0125

0.895

100

100

100

0.0000

0.207

Table 1.0: Table of preparation of calibration curve

Conductivity (mS/cm) vs Convertion (%)


12
10
8

Conductivity (mS/cm)

6
4
2
0

20

40

60

80

100

120

Convertion (%))

Figure 1: Graph Conductivity versus Conversion

Flowrate of
NaOH
(ml/min)

Flowrate of
Et(Ac)
(ml/min)

Time

300

300

250

250

10 | P a g e

Outlet conductivity

Volume of
NaOH (ml)

Q1

Q2

6.9

6.3

20.9

7.0

6.6

20.5

200

200

6.9

6.3

20.6

150

150

6.7

6.0

20.9

100

100

6.2

5.3

22.1

50

50

5.7

4.6

20.8

Residence time, ,
(min)

Conversion, X, (%)

Reaction rate
constant, k,
(L.mol/min)

Rate of reaction, -rA,


(mol.L/min)

6.6667

83.6

7.6463

2.056x10-3

8.0000

82.0

5.6944

1.845x10-3

10.0000

82.4

4.6818

1.450x10-3

13.3333

83.6

3.8232

1.028x10-3

20.0000

88.4

3.8104

5.127x10-4

40.0000

83.2

2.4762

6.989x10-4

11 | P a g e

Conversion versus Residence Time


90

88

86

Conversion X, (%)

84

82

80

78

10

15

20

25

30

Residence Time (min)

FIGURE 2: Graph shows conversion versus residence time.

12 | P a g e

35

40

45

CALCULATION
Sample Calculation
Volume of sample, V

= 50ml

Concentration of NaOH in feed vessel, CNaOH,r


Volume HCl quenching, VHCl,s

=0.1 mol/L
=10ml

Concentration HCl standart solution, CHCl,s

=0.25 mol/L

Concentration NaOH for titration, CNaOH,s

=0.1mol/L

V0= Total inlet flow rate


VTFR= Volume of reactor

= 4L

CAO= Inlet concentration of NaOH

= 0.1 M

A) Sample flowrate

= 300 mL/min of NaOH


= 300 Ml/min of Et(Ac)

B) Volume of titrating NaOH


C) Volume of quenching HCl unreacted with NaOH in sample

= 20.9 mL =0.0209 L

CNaOH , std
( B)
CHCl , std

mol
L

( 0.0209 L )
mol
0.25
L
0.1

=8.3610-3 L
D) Volume of HCl reacted with NaOH in sample V HCl ( C)
10 mL8.36 mL
= 1.6410-3 L
E) Mole of HCl reacted with NaOH in sample

=CHCl, std (D)


= 0.25 mol/L (1.6410-3) L
=4.110-4 mol

13 | P a g e

F) Mole of NaOH unreacted in sample

= (E)
= 4.110-4 mol

G) Concentration of NaOH unreacted with Et(Ac), CA

( E)
V

4.1 104 mol


=
0.05 L
=8.210-3 mol/L
CA
1
=
C AO

H) Steady state fraction conversion of NaOH (XA)

8.2 10 mol/ L
= 1 0.05 mol/ L
=0.836
I) Concentration of NaOH reacted with Et(Ac)

= CNaOH,H20-(G)
= 0.05 mol/L (8.210-3) mol/L
=0.0418 mol/L

J) Mole of NaOH reacted with Et(Ac)

= (I) Vs
=0.0418 mol/L 0.05 L
=2.0910-3 mol

K) Concentration of Et(Ac) reacted with NaOH

J
VS

2.09 103 mol


=
0.05 L
= 0.0418 mol/L
L) Concentration of Et(Ac) unreacted, CB

= CEA,O-(K)
=0.1 mol/L- 0.0418 mol/L
=0.0582 mol/L

14 | P a g e

M) Residence Time,

V TFR
FO

4.0 L
= 0.6 L /min
=6.6667 min

N) Reaction rate constant, k

VO
X
V FTR C AO 1 X

0.6 L/min
0.836
= ( 4 L ) ( 0.1 M ) 10.836

=7.6463 M.L/min
O) Rate of reaction,-rA

= k ( C AO ) ( 1X )

2
2
= 23.5 ( 0.1 ) ( 10.836 )

=2.056x10-3 M.L/min

Repeat step (A) to (O) with all total flowrate which is 500mL, 400mL, 300mL, 200mL, and 100
mL.

15 | P a g e

DISCUSSION
In this experiment, sodium hydroxide, NaOH and ethyl acetate, Et(Ac), were used in the plug
reactor. The effect of residence time against conversion were calculated and tabulated. For the
first total flow rate which is 600mL, the residence time, , calculated was 6.6667 min with the
conversion of NaOH is 83.6%. At the 8th minute of residence time, the conversion of NaOH was
dropped to 82.0% while at the 10th minute of residence time, the conversion of NaOH increased
by 0.4% or equivalence to 82.4%. As the residence time increased to 13.33 min, conversaion of
NaOH has increased to 83.6%. At 20 min residence time, the conversion of NaOH had sudden
increase whre the conversion is 88.4% and lastly at 40 min residence time, the conversion of
NaOH has drop drastically to 83.2%. Theoretically, as the residence time increase, the
conversion should increase but referring to figure 2 from this experiment there is fluctuation
occur.
In titration procedure, when both flowrates are at 300 mL/min, the volume of NaOH
titrated is 20.9mL. when the flowrates are at 250 mL/min, the volume of NaOH required is 20.5
mL and later at 200, 150, 100 and 50 mL, the volume of NaOH required is 20.6, 20.9, 22.1 and
20.8 respectively. This follows accordingly to the theory that whereas concentration is higher at
lower flowrate, more volume of NaOH are required in titration to neutralize the sample.
16 | P a g e

From the graph plotted, initially it shows a drop of NaOH conversion from 6.6667 min to
8 min of residence time. This is deu to error while performing the experiment. The sample might
be left so too long exposed to the air while preparing for the titration. As for the rest of the graph,
the conversion of NaOH gradually increased with residence time. The data mainly shows that the
longer the residence time, the higher the percentage of conversion which abides the expected
result where tho longer time left in the reactor, more reaction occurs between NaOH and Et(Ac).
The rate of reaction for this reactor shows that it decreases over time. There was a stable
supply of heat, making temperature a constant variable, and no unnecessary heat is applied onto
the system. This make the particle speed slower as time increases, losing energy. In the end, the
reaction becomes slower until it reaches equilibrium where there are no more changes in the rate
of reaction.

CONCLUSION
The objective of this experiment was to investigate the effect of residence time against
conversion of NaOH. At the beginning of this experiment, at residence time 6.6667 minute, the
conversion is 83.6%. There is a slightly decreases in the conversion at the residence time is
equal to 8 minute where the conversion is only 82%. From 10 minute to 13.3333 minute of
residence time, there is a constantly increase in conversion which is 82.4% to 83.6%
respectively. At 20 minute of residence time, there is drastically increase in conversion where the
conversion is 88.4%. Lastly, at the residence time 40 minute, the conversion is 83.2%.
Throughout the experiment, the rate of reaction keep on decreasing steadily until it reach
equilibrium.
RECOMMENDATION

All valve should be properly placed before starting the experiment.


Titration should be done as soon as the sample is taken, to avoid any contaminations in

the sample.
Temperature should also be constantly monitored so that it remains the same throughout
the experiment.

17 | P a g e

Perfume general start-up and shut down procedure so that the equipment is in the best
shape.

REFERENCE
1. http://www.umich.edu/~elements/5e/asyLearn/bits/pfrfinal/index.htm, OCTOBER 2016
2. https://www.cs.montana.edu/webworks/projects/stevesbook/contents/chapters/chapter008
/section002/blue/page004.html, OCTOBER 2016
3. Schmidt, Lanny D, The Engineering of Chemical Reactions. New York: Oxford
University Press, 1998.
4. J. Shaw, Reactor Operation. Queen Mary Collage, University of London, 2001.
5. Fogler, H.S (2006), Elements of Chemical Reaction Engineering (3rd Edition). Prentice
Hall.

18 | P a g e