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0 Abstract
The conduction of this experiment is based on a few targets, namely to carry out
saponification reaction between Sodium Hydroxide, NaOH and Ethyl Acetate, Et(AC), to
determine the effect of residence time to the reaction's extent of conversion and lastly to
evaluate the reaction rate constant of this particular saponification reaction. To achieve these
targets, an experiment is finely designed so much so that these targets can be finely met. Such
experiment involves using a unit called SOLTEQ Plug Flow Reactor (Model: BP 101),
commonly known as PFR, as well as some common laboratory apparatus for titration process.
To put it simply, the two solutions Sodium Hydroxide, NaOH and Ethyl Acetate, Et(Ac) were
reacted in the PFR and the product is then analysed by the method of titration to determine
how well did the reaction go. Hence, the experiment was conducted and the results shows that
the amount of conversion of Sodium Hydroxide, NaOH is almost unchanged as residence
time increases. Further details can be obtained in the results and discussion sections.
2.0 Introduction
Type of chemical reactors remains a highly discussed subject in chemical process industries
worldwide.The reactor is of course, the place where chemical reactions take place. Hence it is
arguably the single most important part of any chemical process design. The design of a
reactor must be finely tuned so that its mechanisms suit the necesseties of the process that is
to be carried. Depends on the nature of the materials in both the feed and of course the
products, the reactors may take a wide range of forms. This is why full comprehension of a
reactor of a particular design as well as its working mechanisms is very much vital to actually
conduct a particular chemical process.
In this experiment, the Plug Flow Reactor (Model: BP101) is used as it has been properly
designed for students' experiment on chemical reactions in liquid phase under isothermal and
adiabatic conditions. Included in the unit is a jacketed plug flow reactor; individual reactant
feed tanks and pumps, temperature sensors and conductivity measuring sensor. By using this
particular unit, students will be capable to conduct the typical saponification reaction between
ethyl acetate and sodium hydroxide among the others reaction.
3.0 Objectives
This experiment is conducted to study the effects of residence time on a reaction by using a
Plug Flow Reactor. Also, reaction rate constant is also to be determined by saponification
reaction between Sodium Hydroxide, NaOH and Ethyl Acetate, Et(Ac).
4.0 Theory
4.1 Rate of Reaction and Rate Law
Simply put, rate of reaction can be roughly defined as the rate of disappearance of reactants or
the rate of formation of products. When a chemical reaction is said to occur, a
reactant(or several) diminishes and a product(or several) produced. This is what constitutes a
chemical reaction. For example :
aA+ bB cC +dD
where 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 itself with how
fast the reactants diminish or how fast the product is 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
r A=k C A C B
where
k
rate constant
CA
concentration of A species
CB
concentration of B species
stoichiometric coefficient of A
stoichiometric coefficient of B
4.2 Conversion
Taking species A as the basis, the reaction expression can be divided 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 seen below :
X A=
moles of A reacted
moles of A fed
mixing of the fluid in the tube. Hence the properties of the flowing stream will vary from one
point to another.
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.
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.
4.4 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, PFR 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 CSTR is thoroughly mixed and its RTD is hugely different as
compared to the RTD of PFR.
5.0 Apparatus/Materials
The unit used in this experiment is SOLTEQ Plug Flow Reactor (Model: BP101)
7.0 Results
Reactor Volume.
: 4L
: 0.1M (2L)
: 0.1M (2L)
: 0.25 M (0.01L)
Volume of sample, Vs
: 0.05L
Flow Rate of
Flow Rate of
NaOH
Et(Ac)
(ml/min)
300
250
200
150
(ml/min)
300
250
200
150
Table 1
Residence
Outlet Conductivity
Q1
Q2
Time,
(min)
5
5
5
5
11.0
9.5
8.4
7.5
9.7
8.4
7.4
6.4
Volume of
NaOH
0.3
0.2
0.1
0.1
100
50
100
50
5
5
6.7
5.7
5.5
4.7
Residence Time,
Conversion, X,
Table 2
Reaction Rate Constant,k
, (min)
6.6667
8.0000
10.0000
13.3333
20.0000
40.0000
(%)
50.6
50.4
50.2
50.2
50.4
50.4
(L.mol/min)
1.5365
1.2701
1.0080
0.7560
0.5081
0.2540
0.2
0.2
Residence Time,
Reactor volume ( L ) ,V
L
Total flow rate
,v
min 0
( )
4L
0.6 L/min
= 6.6667 min
placed in Table 2
Other residence times were calculated by the same way, and varying the flow rates.
8.2 Conversion
n2
concentration HCl quenc h
0.00003
0.25
= 0.00012 L
Volume of HCl reacted, V2
V2
= Concentration HCl x V2
= 0.25 x 0.00988
= 0.00247 mole
= n3
= 0.00247 mole
n4
volume sample
0.00247
0.05
= 0.0494 M
Xunreacted
Xunreacted =
=
= 0.494
Xreacted
Xreacted = 1 - Xunreacted
= 1 - 0.494
= 0.506
Conversion for flow rate 300mL/min
0.506 x 100% = 50.6 %
placed in Table 2
Hence, at flow rate 300mL/min of NaOH in the reactor, about 50.6% of NaOH is reacted with
Et(Ac). Other conversions were calculated by the same way, and varying the flow rates.
8.3 Reaction Rate Constant,k
k=
VTFR
CAO
= 0.506
v0
X
V TFR C AO 1X
k=
0.6
0.506
(4)( 0.1) 10.506
= 1.5365L.mol/min
placed in
Table 2
Other Reaction Rate Constants were calculated by the same way, and varying the flow rates.
8.4 Rate of Reaction, -rA
-rA = k (CA0)2 (1-X)2
For flow rates of 300 ml/min :
-rA
placed in Table 2
Other Rate of Reactions were calculated by the same way, and varying the flow rates.
Conversion, %
60
58
56
54
52
50
48
46
44
42
40
5
10
15
20
25
30
Figure 1
35
40
45
9.0 Discussions
Plug Flow Reactor(PFR) is a type of reactor that consists of a cylindrical pipe and is usually
operated at steady state. 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 flowing
stream will vary from one point to another. The fluid in PFR is considered to be thin, unmixed
layer of volume segments or 'plugs', hence the name.
=
Residence Time,
Reactor volume ( L ) ,V
L
Total flow rate
,v
min 0
( )
From the equation above, it can bes seen that residence time is a function of total flow rates of
the feed. Hence, by varying the flow rate of the feed solutions, several residence times can be
obtained and the effects of each one, studied.
After, the experiment is conducted, raw data consisting inlet flow rates, conductivity value
and volume of NaOH used in the titration process are tabulated in Table 1 of the Result
Section. From the raw data obtained, a series of calculations were made, as seen in the Sample
of Calculation section, and the values of residence times, conversion of the reactions, reaction
rate constants and rate of reactions were determined. These values are tabulated in Table 2 of
the Result section.
As the data of residence time and conversion from table 2 is plotted into a graph, the graph is
shown in figure 2. The reason for plotting a graph consisting these two parameters is so that
the effects of residence time can be studied. Conversion is a property that shows how much of
the reaction has taken place. Hence, by comparing this property with the residence time
parameter, one can analyse the effects of increasing residence time to the reaction itself.
By analysing figure 2, it can be clearly seen that the conversion of the reaction remains fairly
constant with the increasing residence time. Therefore, one can postulate that residence time
is not a factor for reaction conversion, as far as plug flow reactors are concerned. One can also
postulate that the reason for this phenomenon is that the PFR lacks a good mixing process.
Since the PFR is designed not to stir the solution vigorously to maximise mixing process, the
conversion of the reaction by using PFR is fairly low.
The experiment also aims to evaluate the reaction rate constants and rate of reaction values of
the reaction. Both of these properties have been determined in the result section.
10.0 Conclusion
The experiment was conducted with several objectives in mind. The first one is to carry out a
saponification process between Sodium Hydroxide, NaOH and Ethyl Acetate, Et(Ac). By
using a Plug Flow Reactor, PFR, these two substances were flowed into the reactor, mixed
and let to react for a certain period of time. By doing that, saponification process was
completed. The experiment also targets to determine the reaction rate of this particular
reaction. This was also done by calculating the reaction rate as seen in the Sample Calculation
section. Lastly, the main objective of this experiment is to study the relationship beteween the
residence time and the conversion of the reactants. This relationship was successfully studied
and graphed in Figure 2 of the Result section.
11.0 Recommendations
1. It is better to time the sample well so that time-wasting in taking samples can be reduced or,
if possible, avoided.
2. All valves should be properly placed before the experiment started.
3. Flow rates should be constantly monitored so that it remains constant throughout the
reaction, as needed.
4. Titration should be immediately stopped when the indicator turned pink.
5. Pumps should never be run dry.
12.0 References
1. Fogler, H.S (2006). Elements of Chemical Reaction Engineering (3rd Edition). Prentice
Hall.
2. Levenspiel, O. (1999). Chemical Reaction Engineering (3rd Edition). John Wiley.
3. Laboratory Manual Tubular Flow Reactor.
4. The Plug Flow (Retrieved from http://www.konferenslund.se/p/L16.pdf on 18th October
2013)
5. Reaction Kinetics (Retrieved from http://smk3ae.files.wordpress.com/2007/10/reaksikinetik.pdf on the 18th October 2013)
13.0 Appendix