Anda di halaman 1dari 14

EKB 3181 Chemical Engineering Lab - IV

Bachelor of Chemical Engineering (Hons)


LAB REPORT
EKB 3181 - CHEMICAL ENGINEERING LAB - IV

EXPERIMENT TITLE

ISOTHERMAL CSTR

NAME OF CANDIDATE
WITH REG NO.

SITI MARIAM BT ABDUL RAHIM


1103143010

SESSION DATE

18th OCTOBER 2016, TUESDAY

DATE OF SUBMISSION

24th OCTORBER 2016, MONDAY

NAMES OF GROUP MEMBERS


No
.
1
2
3
4

REG No.

NAME

1103143014
1103142004
1103142021
1103143020

Santya Gopalan
Mohaan Sockalingam
Assvinraj K munusamy
Brighton Marandu

SIGNATURES

MARKING
DETAILS

TOTAL

MARKS
AWARDED

Participation
and Attitude

(Name of Faculty Supervising)


Mr.

Lab Report
Total

CHEM. ENGG. LAB-IV INCHARGE


(Dr. TVN. Padmesh/)Faculty of
Chemical Engineering
Page
1

EKB 3181 Chemical Engineering Lab - IV

LABORATORY SUBMISSION FORM


Name
ID 1103143011
SARGUNA SANGARI A/P SELVARAJU
Title of
RTD STUDIES IN PACKED BED REACTOR
Course code
EKB 3181
Course name Chemical Engineering Lab IV
Group member
ID
Chong Siew Ling
1103143013
Elton George Thomas
1103142002
Sathiasilan Sundran
1103142020
Yuwetha Gunasagran
1103142008
Emad Yugu Yousif
1103142022
CRITERIA
Poo
Goo
Excelle
V
Ve
r
d
nt
ry
er
1 ABSTRACT
Objective experiment, brief the procedure,
2
4
6
8
10
main result

INTRODUCTION

dvantag &disadvantags
PROCEDURE
(Summary)
Using your OWN word, explain

Overview of the equipment, application,

the experimental procedure

10

10

15

20

25

RESULT AND DISCUSSION

Data are presented as deemed suitable


with complete label and units.
Explanations of the referred table and
figure are presented.
Discuss on the findings and relations to the
theory and objective of experiment.

CONCLUSION&RECOMMENDATION
Summary of the results to relate the
findings or results with the theory
applicable to the experimental.
Suggest improvements in apparatus or
measurement procedure, or experimental
procedures for future.

REFERENCES(ATLEAST3)
APPENDICES
Attach ALL calculation made in this
experiment
Raw data
FORMATS
TOTAL(70%)
Chop received:

TABLE OF CONTENTS
Page
2

EKB 3181 Chemical Engineering Lab - IV

S. No.

DESCRIPTION

PAGE No.

Abstract

Introduction

4-5

Procedure

5-8

Results and Discussions

8-12

Conclusions and Recommendation

12

References

13

Appendix

13-14

1. ABSTRACT
Page
3

EKB 3181 Chemical Engineering Lab - IV


The main objective of this experiment is to study the non-catalytic homogeneous reaction in a
CSTR under isothermal condition and the aim of the experiment is to determine the reaction rate
constant, (K) for saponification of ethylacetate with sodium hydroxide at a fixed temperature and study
the effect of temperature on the reaction rate constant, (K) and determine the activation energy, (E) for
this reaction. After setting up the apparatus, the experiment were started by setting the reaction

temperature at 50oC, air pressure at 0.8 kg/cm2 and flow rate of NaOH and ethyl acetate was
adjusted at equimolar flow rate for a certain time. After approximately 10 minutes, the sample were
collected exactly 10 ml from the outlet feed tank using measuring cylinder that already contains 20
ml of HCL solution. Then, the sample solution was titrated using phenolphthalein as an indicator to test
the presences of NaOH ions. The reading of the burette were noted down. At every 10 minutes

interval, set of 7 readings were taken three sustained reading were obtained. From this experiment,
the reaction rate constant for saponification of ethyl acetate sodium hydroxide at a fixed
temperature which is K 0.245 L/mol.min and the activation energy is 20.11 cal/mol thus this
experiment is achieved successfully. There were few errors occured during the experiment and so
there are some recommendations has been suggested in the conclusion. The entire objective have
been achieved and related to the theory of study.

2. INTRODUCTION
A stirred-tank reactor (STR) may be operated either as a batch reactor or as a steady-state flow
reactor (better known as Continuous Stirred-Tank Reactor (CSTR)).The key or main feature of this
reactor is that mixing is complete so that properties such as temperature and concentration of the
reaction mixture are uniform in all parts of the vessel reactor (CSTR).In a CSTR it is designed that,
one or more fluid reagents are introduced into a tank reactor (typically) equipped with an impeller
while the reactor effluent is removed. The impeller stirs the reagents to ensure proper mixing. Run
at steady state with continuous flow of reactants and products; the feed assumes a uniform
composition throughout the reactor, exit stream has the same composition as in the tank.
(Fogler,2013).
In application, simply dividing the volume of the tank by the average volumetric flow rate through
the tank gives the space time, or the average amount of time a discrete quantity of reagent spends
inside the tank. Chemical reactors often have significant heat effects, so it is important to be able to
Page
4

EKB 3181 Chemical Engineering Lab - IV


add or remove heat from them. In a CSTR (continuous stirred tank reactor) the heat is added or
removed by virtue of the temperature difference between a jacket fluid and the reactor fluid. Often,
the heat transfer fluid is pumped through agitation nozzle that circulates the fluid through the jacket
at a high velocity. The reactant conversion in a chemical reactor is a function of a residence time or
its inverse, the space velocity. For a CSTR, the product concentration can be controlled by
manipulating the feed flow rate, which changes the residence time for a constant chemical reactor.
The advantages of isothermal CSTR are they are always continuous operation. Good temperature
control. Easily adapts to two phase runs. Good control of an operation. Simplicity of construction
with low operating (labor) cost and it is easy to clean. (Octave Levenspiel,2008)
The disadvantages are, by-passing and channeling possible with poor agitation and also Lowest
conversion per unit volume.(Fogler,2013)

3. PRODEURE
3.1. Materials
1.
2.
3.
4.
5.
6.
7.
8.

Syringe
Measuring cylinders
Conical flasks
Stopwatch
Beakers
Burette
2L of 0.1M NaOH solution
2L of 0.1M ethyl acetate

3.2. Starting Procedure


1. 20L of 0.1 M NaOH solution was prepared
2. 20L of 0.1M ethyl acetate solution was prepared
3. 20ml of 0.1M of hydrochloric acid was take in measuring cylinder
4. The burette was filled by 0.1M sodium hydroxide
5. All the valves V1-V11 were closed
6. Valves V4 and V6 was opened and sodium hydroxide solution was filled in feed tank A
7. Valves V4 and V6 then were closed
8. Valves V5 and V7 was opened to filled ethyl acetate solution in feed tank B
9. Valves V5 and V7 were the closed
10. The water bath was filled with water
Page
5

EKB 3181 Chemical Engineering Lab - IV


11. The ON/OFF switched in the given panel was ensured at OFF position
12. Electric supply was connected to the set up
13. The reaction temperature of 70C was set and the button of DTC was set
14. The heater and stirrer of the bath was started and waited till the constant temperature is
attained
15. Compressed air supply was connected to the set up at valve V1
16. Valve V1 was opened and air pressure was set 0.5 to 1kg/cm 2 by pressure regulator and
pressure gauge
17. Sodium hydroxide and ethyl acetate were pass into the reactor by allowing equal flow rate
controlled by valve V2-V3
18. 10ml of the sample was collected from the outlet in measuring cylinder which already
contain 20ml of hydrochloric acid after about 10min
19. The reaction temperature was noted down
20. The sample solution was transfer in a conical flask
21. The solution was titrated using phenolphthalein as an indicator against 0.1M sodium
hydroxide (NaOH was added in burette)
3.3 Closing Procedure
1.
2.
3.
4.
5.
6.

V1
V2
V3
V4
V5
V6
V7
V8
V9
V10
V11

The flow of the feed was stop by closing the valve V2-V3 when the experiment is over
The heater and stirrer of the water bath was switch OFF
The stirrer of the reactor was switch OFF
Air pressure was reduced to 0kg/cm2 by pressure regulator and pressure gauge
Valve V1 was closed
The reactor, feed tanks and water bath was drained by valve V8-V11.

Valves
Air supply valve for feed tank
Flow Control Valve for Rotameter A
Flow Control Valve for Rotameter B
Feed Inlet Valve for Feed Tank A
Feed Inlet Valve for Feed Tank B
Air Vent Valve for Feed Tank A
Air Vent Valve for Feed Tank B
Drain Valve for Feed Tank A
Drain Valve for Feed Tank B
Drain Valve for Reactor
Drain Valve for Waterbath
Page
6

EKB 3181 Chemical Engineering Lab - IV


3.4 Calculation Procedure
1. The concentration of unreacted NaOH in the reactor, C Ao were calculated using
equation;

CAO = NNaOH
(1)
2. Concentrated of unreacted NaOH in the reactor, C A were calculated using equation;

CA = (Cao - [(NV/ (1000) ]/0.03)


(2)
3. The degree of conversion, XA were calculated using equation

XA = (CA0 Ca) / CAO


(3)
4. The residence time, were calculated using equation;

t = (Vr ) /( V0)
(4)
5. The rate constant for individual run were calculated using equation;

(CAO

CA)

(5)
(6)

6. The activation energy equation;

k= Ae-Ea/ RT

Page
7

CA2

EKB 3181 Chemical Engineering Lab - IV

Figure 1: Block Diagram of Isothermal CSTR.

4. RESULTS AND DISCUSSION


Table 1 shows the observation reading based on the experiment held in the lab. It states the volume
of NaOH used for titration over time taken.

Table 1: Volume of NaOH used for titration over time taken.


Time (min)
0
10
20
30
40
50
60
70

T (C)
50
55.5
49
49.6
51.9
51.9
50.5
51.9

VA(LPH)
10
10
10
10
10
10
10
10

VB(LPH)
10
10
10
10
10
10
10
10

V1 (ml)
0
37
22.4
19.5
19.5
17
17
17

Table 1 shows the readings of volume of sodium hydroxide (NaOH) used for titration over time take
taken. The time taken was every 10 min intervals. The temperature changes as the time increase, its
Page
8

EKB 3181 Chemical Engineering Lab - IV


shows unsteady trend. The volumetric flow rate of sodium hydroxide in feed tank A and volumetric
flow rate of ethyl acetate in tank B are shown constant throughout the experiment. Volume of
sodium hydroxide (NaOH) used for titration to change the sample of 10 ml collected solution with
20 ml of HCL from colourless to pink decreases as the time taken increase and reaches steady state.
This is because as the time increases, the concentration of ethyl acetate and sodium hydroxide
decreases. The observation data taken while conducting the experiment for isothermal CSTR. The
volume of sodium hydroxide used to titrate the sample solution were tabulated as shown in table 1.
Note that the pressure reading, 0.8 kg/cm2 of the setup kept constant throughout the experiment, at
each and every 10 minutes of interval 10 ml of sample solution collected from the outlet and mix it
with 20 ml of HCI. Besides that, the sample solution titrates against tested using phenolphthalein as
an indicator to test the presences of NaOH ions under alkaline condition, as the time taken
decreases and reaches steady state. It can be stated, at the starting of the reaction there were more
acids consumed more as needed base to neutralize the solution. It became lesser as saponification is
an alkaline solution, (Coulson and Richardson,1996).
Table 2 shows the calculation based on the raw data from table 1. It focuses on the calculation of
conversion of the reaction over the time taken.

Table 2: Conversion of the reaction over time taken


Time (min)
10
20
30
40
50
60
70

t (min)
0.231
0.231
0.231
0.231
0.231
0.231
0.231

XA
4.4
1.48
0.9
0.9
0.4
0.4
0.4

(1-XA)^2
11.56
0.2304
0.01
0.01
0.36
0.36
0.36

XA/(1-XA)^2
0.381
6.424
90
90
1.11
1.11
1.11

Table 2 shows the conversion of the reaction over the time taken. It can be seen that as the time
increases, the conversion decreases. This is because at the initial time the rate of reaction is faster.
The number of moles of reactants A reacted per mole of reactants. A fed decreases and it completely
changes to products as the time increases. In this non-catalytic homogenous reaction, the OH- ion is
Page
9

EKB 3181 Chemical Engineering Lab - IV


the most highly conductive species therefore the conductivities of the ethyl acetate and ethyl alcohol
may be ignored. Since the reaction solution is in dilute aqueous state, it can be assumed that sodium
acetate is completely ionized. The concentration of Na+ ions remains invariable before and after the
reaction. Holman, 2008 states that as the reaction time increases, the number of OH- ions decreases
continuously, and the conductance of the system declines continuously. From the calculation, at the
final reading, the rate constant is 0.245 L/mol.min as shown.
The graph in the Figure 2 of conversion against the residence time was plotted according to data in
Table 2.

0.25
f(x) = 0.41x + 0

0.2
0.15

residence time ,t(min)


0.1
0.05
0

0.1

0.2

0.3

0.4

0.5

0.6

XA/(1-XA)^2

Figure 2 shows residence time, (min) versus conversion, X A/ [1-XA]2 graph

By analysing figure 2, it can be clearly seen that the conversion is directly proportional to the
residence time. The conversion increases along residence time throughout the experiment. From the
graph, the value of the slope is zero . The residence time is calculated by dividing the reactor volume

with the total flow rate. Since throughout the experiment the rotameter readings for tank A and B
Page
10

EKB 3181 Chemical Engineering Lab - IV


constant as we used the same reactor throughout our experiment, thus our residence time is kept

constant which is 0.231 minutes. Therefore, our solution of NaOH and Et(Ac) can be expect resides
in the reactor for 0.231 minutes. This is because the residence time in graph constant. From the graph,
it can conclude that the reactants being reproduce. This could happen due to reaction occurs in backward
direction. The relative corresponding equilibrium concentration have been achieved before the data is
taken. Based on the gradient equation on the graph.
Arrhenius equation represents the fraction of molecules having an energy equal to or greater than
the energy required for activation. Based on the Arrhenius equation, it can be calculated that the
activation energy, Ea is 20.11cal/mol. The overall activation energy calculated were in positive value.
Thus, can conclude that the rates of reaction increase with the increase in temperature. This support the
assumption that the reaction is already reached the relative corresponding equilibrium concentration and
reversed the reaction in backward direction, where NaOH is actually being produced back. The set

point temperature for reaction were set at 50C yet the temperature fluctuates from 49.6 C till 55.5
C because of the heat loss during the reaction thus the rate of reaction was not persistent and the
reaction went to the peak level and then it drop to the normal level. Thus, can conclude that the rates
of reaction increase with the increase in temperature.
There were some errors were observed which lead to defects in result towards the middle part of the

graphs where there might be some heat loss from the system to the surrounding which leads to
inaccurate temperature readings. Misinterpreting the colour of the indicator near the end point. This
will also affect the results. The other error is that the system is not of the same pressure causing the
flow rate to be not stable during the experiment conduction.

5. CONCLUSIONS AND RECOMMENDATION

Page
11

EKB 3181 Chemical Engineering Lab - IV


The main objective of this experiment is to study the non-catalytic homogeneous reaction in a
CSTR under isothermal conditions. From the experiment conducted rate constant of the
saponification of ethyl acetate with sodium hydroxide was determined. The greater the value of the
rate constant, the faster the reaction. At the final reading, the reaction rate constant, K for
saponification of ethyl acetate with sodium hydroxide is 0.245 L/mol.min and the activation energy
is 20.11 cal/mol. There are few suggestions to get more accurate and precise results for this
experiment, which are ensure that no leakage at the valve on the unit. This to prevent the result will
affect. Make sure that the valve is open or close, follow as the general start-up procedure carefully.
Flow rates should be constantly monitored so that it remains constant throughout the reaction, as
needed. Titration should be immediately stopped when the indicator turned pink.

6. REFERENCES
1. Fogler, H. (2013). Essentials of Chemical Reaction Engineering. Pearson Education
International.
2. Octave Levenspiel, (2008); chemical reaction engineering, 3 rd edition, Choudhary Press,
Delhi, India. Pg 27 -28
3. Coulson, J.M, Richardson, J.F (1996). "Chemical Reaction Engineering" Vol-1. 5th Ed.
ND: Asian Books Ltd. pp 349-350.
4. Holman, J.P (2008). "Chemical Engineering 9th Ed. ND: McGraw Hill. pp 25-27.

Page
12

EKB 3181 Chemical Engineering Lab - IV

7. APPENDIX
Data Table:

Real gas constant R


Working volume of reactor Vr

1.987 cal/mol K
r2 h * 1000
(0.07)2 (0.15) * 1000
= 2.31L
20ml
10ml
0.1 g eq/L
0.1 g eq/L
0.1 g eq/L

Volume of HCI VHCI


Volume of sample VSAMP
Normality of NaOH in feed solution NNaOH
Normality of NaOH used for titration N1
Normality of HCI NHCI

CAO = NNaOH
(1)
= 0.1mole/L
CA = (Cao - [(NV/ (1000) ]/0.03)
(2)
= (0.1-[(0.10 x 17) /1000 ]/0.03)
= 0.043mole/L
XA = (CA0 Ca) / CAO
(3)
= (0.1-0.043)/0.1
= 0.57

Page
13

EKB 3181 Chemical Engineering Lab - IV


t

(Vr

/(

V0)

(4)
= (2.31L) / 10LPH)
= 0.231 min

K = 1/Gradient x Cao (L/mole min)


(5)
= 1/(0.4083)x 0.1
= 0.245 L/mol.min

k= Ae-Ea/ RT
0.577= 1013 e-Ea/(1.987) (323)
Ea=20.11cal/mol

Page
14

(6)