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Plug Flow Reactor
Plug Flow Reactor
Title
Abstract/Summary
Introduction
Aims
Theory
Apparatus
Methodology/Procedure
Results
Calculations
Discussion
Conclusion
Recommendations
Reference
Appendix
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ABSTRACT
The aims of this experiment are to carry out saponification reaction between Sodium
Hydroxide, NaOH and Ethyl Acetate, Et(AC) and to determine the effect of residence time to
the reaction's extent of conversion. This experiment also evaluates the reaction rate constant
of a particular saponification reaction.
In this experiment, the Plug Flow Reactor (Model: BP101) as well as some common
laboratory apparatus for titration process 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.
Before starting the experiment, the general start-up is ensured to carry out properly with lab
assistant, En Jamil in order to avoid any disturbance that may affect the results. The two
solutions Sodium Hydroxide, NaOH and Ethyl Acetate, Et(Ac) are reacted in the PFR and
the product is taken as a sample then analysed by the method of titration with different flow
rates of 300, 250, 200, 150, 100 and 50 ml/min to determine how well did the reaction go.
For each flow rate, a 50 mL sample is collected to be use in the back titration. After that, the
stable conductivity is recorded for every 5 minutes before collecting the samples. In the back
titration, the samples that had been collected are titrated with NaOH for saponification
reaction until it changes colour from colourless into light pink. Next, the amount of NaOH
titrated are recorded and tabulated in Table 1. From Table 1, a few of calculations are done
and tabulated in Table 2 and a graph of Conversion against Residence Time in Figure 3 had
been plotted. The results showed that the amount of conversion of Sodium Hydroxide,
NaOH increases as residence time increases. Further details can be obtained in the results
and discussion sections. The experiment was successfully conducted.
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 necessities 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.
The Tubular Flow Reactor (Model: BP 101) or known as Plug Flow Reactor has been
designed to introduce students of Chemical Engineering to the behaviour of a plug flow
reactor by studying the second order reaction between dilute caustic soda and ethyl acetate.
The unit is small in scale for ease of operation but capable of demonstrating the principles of
industrial scale reactor behaviour. The unit includes a 10 litres reactor vessel as a water
jacket, and is equipped with a variable speed stirrer, inlet and outlet ports for the feed and
product streams, sampling, conductivity measurements and temperature measurements and
control. A cooling coil and immersion heater are provided inside the vessel to provide
constant reaction temperature. The desired reaction temperature is achieved by controlling
the heating using a digital temperature controller located on the front panel. Two noncorroding feed storage vessels are supplied, together with chemically resistant pumps and
flow meters. A product collection vessel is also provided and if necessary, the products are
neutralised before discharging to the laboratory drains. The tubular reactor is a coil of long
tubing wound around a cylinder inside the vessel to give a total reactor volume of
approximately 0.4 litres. The spiral design is practically the best approximation to plug flow
conditions, as the secondary flow ensures good radial mixing while minimising longitudinal
dispersion. The two reactants are pre-heated prior to mixing and entering the reactor. 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.1
1 http://www.solution.com.my/pdf/BP101(A4).pdf
AIMS
The objectives of this experiment are:
1) To study the effects of residence time on a reaction by using a Plug Flow Reactor.
2) To determine the reaction rate constant by saponification reaction between Sodium
Hydroxide, NaOH and Ethyl Acetate, Et(Ac).
3) To study the relationship between the residence time and the conversion of the
reactants.
THEORY
Rate of Reaction and Rate Law
The rate of reaction tells us how fast a number of moles of one chemical species are being
consumed to form another chemical species.2 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
(1)
Where:
A and B represents reactant 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
is how fast the reactants diminish or how fast the product is formed. Rate of reaction of each
species corresponds respectively to their stoichiometric coefficient. Such as:
r A r B r C r D
=
= =
a
b
c d
(2)
The negative sign indicates reactants.
rA
rA
r A=k C A C B
is:
(3)
Where:
2 Fogler, 2004, pp. 4 8
3 Fogler, 2004, pp. 81 83
5
= Rate constant
CA
= Concentration of A species
CB
= Concentration of B species
= Stoichiometric coefficient of A
= Stoichiometric coefficient of B
The proportionality constant, k is called the rate constant, and its value is characteristic of
the reaction and the reaction conditions. A given reaction has a particular rate constant value
under a given set of conditions, such as temperature, pressure, and solvent; varying the
temperature or the solvent usually changes the value of the rate constant. The numerical
value of k, however, does not change as the reaction progresses under a given set of
conditions.4
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:5
b
c
d
A + B+ C + D
a
a
a
(4)
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
(5)
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.
PFR are used to model the chemical transformation of compounds as they are transported
in systems resembling "pipes". The pipe can represent a variety of engineered or natural
conduits through which liquids or gases flow.
An ideal PFR has a fixed residence time. Any fluid (plug) that enters the reactor at time t will
exit the reactor at time
t+ , where
. A PFR has
a residence time distribution that is a narrow pulse around the mean residence time
distribution.
A typical plug flow reactor could be a tube packed with some solid material (frequently a
catalyst). Typically these types of reactors are called packed bed reactors or PBR.
ResidenceTime , =
Reactor volume ( L ) , V
L
Total flow rate
,v
min 0
( )
(6)
The theory of residence time distributions generally begins with three assumptions:
1) The reactor is at steady-state
2) Transports at the inlet and the outlet takes place only by advection
3) The flow is incompressible.
The incompressibility assumption is not required but compressible flows are more difficult to
work with and less common in chemical processes. A further level of complexity is required
for multi-phase reactors, where a separate RTD will describe the flow of each phase, for
example bubbling air through a liquid.
In an ideal plug-flow reactor there is no axial mixing and the fluid elements leave in the same
order they arrived. Therefore, fluid entering the reactor at time, t will exit the reactor at
time
t+ , where
E ( t ) =( t )
(6)
The variance of an ideal plug-flow reactor is zero.
The RTD of a real reactor deviate from that of an ideal reactor, depending on the
hydrodynamics within the vessel. A non-zero variance indicates that there is some dispersion
along the path of the fluid, which may be attributed to turbulence, a non-uniform velocity
profile, or diffusion. If the mean of the E(t) curve arrives earlier than the expected time
it
indicates that there is stagnant fluid within the vessel. If the RTD curve shows more than one
main peak it may indicate channeling, parallel paths to the exit, or strong internal circulation.8
APPARATUS
1)
2)
3)
4)
5)
Chemicals used:
1) pH Indicator (Phenolphthalein)
2) 0.1 M Sodium Hydroxide, NaOH
3) 0.1 M Ethyl Acetate, Et(Ac)
4) 0.25 M Hydrochloric Acid, HCl
11
PROCEDURE
General Start-Up Procedures
1) All the valves are ensured closed except valves V4, V8 and V17.
2) The following solutions are prepared:
a. 20 liter of NaOH (0.1M)
b. 20 liter of Et(Ac) (0.1M)
c. 1 liter of Hydrochloric Acid, HCL (0.25M) for quenching
3) Feed tank B1 is filled with NaOH solution while feed tank B2 is filled with the Et(Ac)
solution.
4) The power for the control panel is turned on.
5) The water jacket B4 is filled with water and pre-heater B5 is filled with clean water
6) Valves V13 are V18 are opened.
7) Pump P3 then is switched on in order to circulate the water through pre-heater B5.
8) The stirrer motor M1 was switched on and set up to speed about 200 rpm to ensure
homogeneous water jacket temperature.
9) Valves V2, V4 and V10 are opened. Pump P1 is switched on. P1 is adjusted to
obtained flow rate approximately 300 ml/min at both flow meters Fl-01. Valve V10 is
closed and pump P1 is switched off.
10) Valves V6, V8 and V12 are opened.
11) Pump P2 is switched on. P2 is adjusted to obtained flow rate approximately 300
ml/min at both flow meters Fl-02. Valve V12 is closed and pump P2 is switched off.
General Shut-Down Procedures
1) Pumps P1, P2 and P3 are switch off. Valves V2 and V6 are closed.
2) The heaters are switched off.
3) The cooling water is kept circulating through the reactor while the stirrer motor is
running to allow the water jacket to cool down to room temperature.
4) All liquid is drained from the unit by opening valves V1 to V19. The feed tanks are
rinsed with clean water.
5) The power is turned off for the control panel
12
13
RESULTS
Reactor volume
=4L
C NaOH
Flow Rate of
= 0.10 M (2 L)
C NaOH , s
= 0.10 M (2 L)
C HCl, s
= 0.25 M (0.01 L)
Vs
= 0.05 L
Flow Rate of
Outlet
Residence
NaOH (ml/min)
Et(Ac) (ml/min)
Time, (min)
300
250
200
150
100
50
300
250
200
150
100
50
5
5
5
5
5
5
Volume of
Conductivity
Q1
Q2
8.8
7.3
8.6
7.0
8.5
6.6
7.6
5.8
7.4
5.2
6.7
6.7
NaOH (ml)
13.5
9.9
13.1
17.0
13.5
19.0
Table 1
Residence Time,
Conversion, X
, (min)
(%)
(L.mol/min)
6.667
8.000
10.000
13.333
20.000
40.000
77.0
69.8
76.2
84.0
77.0
88.0
5.0217
2.8891
3.2017
3.9375
1.6739
1.8333
Table 2
14
Rate of Reaction,
r A (L.mol/min)
2.6564E-3
2.6350E-3
1.8136E-3
1.0080E-3
0.8854E-3
2.6400E-3
Residence time
Conversion, X (%)
100
90
80
70
60
50
40
30
20
10
0
10
15
20
25
30
35
15
40
45
CALCULATIONS
FR: 300 ml/min
1) Residence Time
ResidenceTime , =
Reactor volume ( L ) , V
L
Total flow rate
,v
min 0
( )
ml
ml
300
NaOH
+300
Et ( Ac )
=
min
min
=
ResidenceTime , =
600
ml
min
0.6
L
min
4L
0.6 L/min
6.667 min
2) Conversion
n1
0.1 M 0.0135 L
= 0.00135 mol
n2
n1
n2
0.00135 mol
16
V1
n2
concentration HCl quench
0.00135mol
0.25
0.0054 L
17
0.0 10.0054
0.0046 L
Concentration HCl V 2
0.25 0.0046
0.00115 mol
n3
0.00115 mol
n4
= volume sample
C NaOH unreacted
X unreacted
X reacted
0.00115
0.05
0.023 M
0.023
0.1
0.368
1X unreacted
10.023
0.77
0.77 100 = 77
18
19
77.0
of NaOH is reacted
k=
v0
X
V TFR C AO 1X
V0
0.6 L/min
V TFR
=
C AO
k=
4L
0.1 M
0.77
0.6
0.632
(0.4)(0.1) 10.632
4) Rate of Reaction,
r A
r A
k ( C A 0 )2 ( 1X )2
r A
L
min
20
DISCUSSION
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.
As seen in Figure 1, the solution in the tube is treated as a series of layers of volume
segments that are unmixed with the segment before and after it. Like a series of plugs,
stacked together in a pipe. In this particular experiment, the solutions used are NaOH and
Et(Ac). These two solutions react together in the PFR to complete saponification reaction.
The main objective of this particular experiment is to study the effect of residence time on
the performance of this reactor, the PFR. To do that, of course, residence times have to be
manipulated throughout the experiment and the effects of each one is studied. Residence
time, in this particular experiment, is varied by the means of changing the flow rates of the
feed solutions. This is shown in equation (6).
From the equation (6), it can best seen as 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. From the raw
data obtained, a series of calculations were made, as seen in the 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 3. The reason for plotting a graph consists of 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.
21
By analysing Figure 3, it can be clearly seen that the conversion of the reaction fluctuates
with the increasing residence time from residence time of 6.6667 to 20 minutes. Then begin
to increase linearly from residence time of 20 to 40 minutes. To put it simply, as conversion
increases, residence time increases. Therefore, one can postulate that residence time is a
factor for reaction conversion, as far as plug flow reactors are concerned.
The experiment also aims to evaluate the reaction rate constants and rate of reaction values
of the reaction. Both of these properties have been tabulated in Table 2 in the Result section.
Other than that, there are some errors occurred during the experiment thus there are some
recommendations for future students that will be conducting the experiment. First, all valves
should be properly placed before the experiment started. Then, flow rates should be
constantly monitored so that it remains constant throughout the reaction, as needed. After
that, titration should be immediately stopped when the indicator turned pink. Lastly, pumps
should never be run dry. By doing all these recommendations, readings will be more
accurate and thus improve the results.
22
CONCLUSION
The experiment is conducted with several objectives. 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 are flowed into the reactor, mixed
and let to react for a certain period of time. By doing that, saponification process is
completed. The experiment also targets to determine the reaction rate of this particular
reaction. This is done by calculating the reaction rate as seen in the Calculation section and
the data is tabulated in Table 2 in Results section. Lastly, the main objective of this
experiment is to study the relationship between the residence time and the conversion of the
reactants. By analysing Figure 3, it can be clearly seen that the conversion of the reaction
fluctuates with the increasing residence time from residence time of 6.6667 to 20 minutes.
Then begin to increase linearly from residence time of 20 to 40 minutes. To put it simply, as
conversion increases, residence time increases. Therefore, one can postulate that residence
time is a factor for reaction conversion, as far as plug flow reactors are concerned. This
relationship was successfully studied and graphed in Result section. The experiment was
successfully conducted.
Other than that, there are some errors occurred during the experiment thus there are some
recommendations for future students that will be conducting the experiment. First, all valves
should be properly placed before the experiment started. Then, flow rates should be
constantly monitored so that it remains constant throughout the reaction, as needed. After
that, titration should be immediately stopped when the indicator turned pink. Lastly, pumps
should never be run dry. By doing all these recommendations, readings will be more
accurate and thus improve the results.
23
RECOMMENDATIONS
1) All valves should be properly placed before the experiment started.
2) Flow rates should be constantly monitored so that it remains constant throughout the
reaction, as needed.
3) Titration should be immediately stopped when the indicator turned pink.
4) Pumps should never be run dry.
REFERENCE
24
APPENDICES
Specifications
Bench-mounted apparatus designed to demonstrate tubular reactor behaviour comprising
two 20 litre feed tanks; non-corrosive feed pumps and flow meters. It includes a temperature
controlled water jacket, a preheating coils and 0.4 litres reactor volume.
1) Reactor:
Water Jacket: 10 L; borosilicate glass; stainless steel top and bottom plate
Cooling System: 3/8" stainless steel tube with connections for cooling water
Heating System: 2 x 1 kW immersion heaters; temperature sensor; temperature
controller
Tubular Reactor: Coiled tubing; 0.4 L
Pre-heating: 2.5 L stainless steel vessel with coils and circulation pump
2) Stirrer System:
Speed Range: 50 to 2000 rpm; with speed controller and digital indicator
Electrical: 240VAC/1-phase/50-60Hz
Impellers: 2" diameters; stainless steel
3) Feed Tanks:
Capacity: 20 litres (cylindrical)
Material: Stainless steel
4) Product Tanks:
Capacity: 50 litres (rectangular)
Material: Stainless steel
5) Feed Pumps:
Capacity: 1 LPM
Electrical: 240VAC/1-phase/50-60Hz
6) Flow Control:
Liquid Flow meter: up to 500 ml/min; electronic
Flow Control: needle valves
7) Instrumentations:
The unit is fitted with all necessary sensors and digital indicators for measurements
of temperature, flow rate and conductivity. All sensors are of electronic type to ensure
compatibility with data acquisition system.
Requirements
Electrical supply: 240VAC/1-phase/50-60Hz.
Water supply: Laboratory mains supply with drainage points
Working area: ventilated; approx. 10 m2
Chemicals: ethyl acetate and caustic soda are suggested Analytical Equipment
Overall Dimensions
Height: 1.68 m
Width: 1.22 m
Depth: 0.91 m