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Title
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Marks
(%) CHE HASNAN
NAME
: NURUL SYAHEERAH BINTI
STUDENT NO.
: 2015230056
GROUP
: GROUP 1 / EH2205G
EXPERIMENT
: TUBULAR FLOW REACTOR
DATE PERFORMED : 19 OCTOBER 2016 (WEDNESDAY)
SEMESTER
:5
PROGRAMME / CODE : EH220
SUBMIT TO
: MADAM NOR SHARLIZA MOHD SAFAAI
No.
1
2
3
4
5
6
7
8
9
10
11
12
13
Abstract / Summary
Introduction
Aims
Theory
Apparatus
Methodology / Procedure
Results
Calculations
Discussion
Conclusion
Recommendations
Reference
Appendix
TOTAL MARKS
...........................................
Date :
5
5
5
5
5
10
10
10
20
10
5
5
5
100
.
Date :
TABLE OF CONTENTS
Content
Page
ABSTRACT
INTRODUCTION
OBJECTIVES
THEORY
PROCEDURE
10
RESULTS
13
CALCULATIONS
14
DISCUSSION
27
CONCLUSION
29
RECOMMENDATIONS
29
REFERENCES
30
APPENDICES
31
1.0 ABSTRACT
The objective of this experiment is to examine the effect of pulse input and step
change input in a tubular flow diagram. Another objective is to construct a residence
time distribution (RTD) function for the tubular flow reactor. The experiment was run
at constant flow rate of 700 mL/min with de-ionised water in tank 1 and salt solution
in tank 2 as the reactants. Both reactants are mixed in the reactor. Based on the data
tabulated, the highest outlet conductivity for pulse input is at minute 1.0 which is 2.5
mS/cm. However, for step change input, the highest outlet conductivity is at minute
3.0 which is 4.9 mS/cm and it is constant until minute 5.0. The mean residence time,
t m , second moment, variance,
s3
for pulse
input is 2.598, 29.173 and -0.6619 respectively. The value of skewness for pulse
input is negative, and therefore it is said as negative skewness. Meanwhile, for step
change input, the mean residence time, t m , second moment, variance,
third moment, skewness,
s3
and
respectively. The value of skewness for pulse input is positive, and therefore it is said
as positive skewness. All in all, the experiment is completed and succeeds.
2.0 INTRODUCTION
A tubular reactor is a vessel through which flow is continuous, usually at steady state,
and configured so that conversion of the chemicals and other dependent variables are
functions of position within the reactor rather than of time. In the ideal tubular reactor,
the fluids flow as if they were solid plugs or pistons, and reaction time is the same for
all flowing material at any given tube cross section. Tubular reactors resemble batch
reactors in providing initially high driving forces, which diminish as the reactions
progress down the tubes.
Flow in tubular reactors can be laminar, as with viscous fluids in smalldiameter tubes, and greatly deviate from ideal plug-flow behaviour, or turbulent, as
with gases. Turbulent flow generally is preferred to laminar flow, because mixing and
heat transfer are improved. For slow reactions and especially in small laboratory and
pilot-plant reactors, establishing turbulent flow can result in inconveniently long
reactors or may require unacceptably high feed rates.
The residence time distribution (RTD) of a chemical reactor is a probability
distribution function that describes the amount of time a fluid element could spend
inside the reactor. Chemical engineers use the RTD to characterize the mixing and
flow within reactors and to compare the behavior of real reactors to their ideal
models. This is useful, not only for troubleshooting existing reactors, but in estimating
the yield of a given reaction and designing future reactors.
The basic ideas that are used in the distribution of residence times to characterize
and model non-ideal reactions are really few in number. The two major uses of the
residence time distribution to characterize non-ideal reactors are:
1. To diagnose problems of reactors in operation
2. To predict conversion or efuent concentrations in existing/available reactors
when a new reaction is used in the reactor
The idea of using the distribution of residence times in the analysis of chemical
reactor performance.
In an ideal plug-ow reactor, all the atoms of material leaving the reactor have
been inside it for exactly the same amount of time. Similarly, in an ideal batch reactor,
4
all the atoms of materials within the reactor have been inside it for an identical length
of time. The time the atoms have spent in the reactor is called the residence time of
the atoms in the reactor.
The RTD is determined experimentally by injecting an inert chemical, molecule,
or atom, called a tracer into the reactor at some time and then measuring the tracer
concentration, in the efuent stream as a function of time. In addition to being a
nonreactive species that is easily detectable, the tracer should have physical properties
similar to those of the reacting mixture and be completely soluble in the mixture. It
also should not adsorb on the walls or other surfaces in the reactor. The latter
requirements are needed so that the tracers behaviours will honestly reect that of the
material owing through the reactor. Coloured and radioactive materials along with
inert gases are the most common types of tracers. The two most used methods of
injection are pulse input and step input.
In a pulse input, an amount of tracer is suddenly injected in one shot into the feed
stream entering the reactor in as short a time as possible. The outlet concentration is
then measured as a function of time.
3.0 OBJECTIVES
i.
ii.
To examine effect of pulse input and step change input in tubular flow reactor.
Construct a residence time distribution (RTD) function of the tubular flow reactor.
4.0 THEORY
A tubular reactor is a vessel through which flow is continuous, usually at steady state,
and configured so that conversion of the chemicals and other dependent variables are
functions of position within the reactor rather than of time. In the ideal tubular reactor,
the fluids flow as if they were solid plugs or pistons, and reaction time is the same for
all flowing material at any given tube cross section. Tubular reactors resemble batch
reactors in providing initially high driving forces, which diminish as the reactions
progress down the tubes. Tubular reactor are often used when continuous operation is
required but without back-mixing of products and reactants.
Flow in tubular reactors can be laminar, as with viscous fluids in smalldiameter tubes, and greatly deviate from ideal plug-flow behaviour, or turbulent, as
with gases. Turbulent flow generally is preferred to laminar flow, because mixing and
heat transfer are improved. For slow reactions and especially in small laboratory and
pilot-plant reactors, establishing turbulent flow can result in inconveniently long
reactors or may require unacceptably high feed rates.
Tubular reactor is specially designed to allow detailed study of important
process. The tubular reactor is one of three reactor types which are interchangeable on
the reactor service unit. The reactions are monitored by conductivity probe as the
conductivity of the solution changes with conversion of the reactant to product. This
means that the inaccurate and inconvenient process of titration, which was formally
used to monitor the reaction progress, is no longer necessary.
The residence-time of an element of fluid leaving a reactor is the length of
time spent by that element within the reactor. For a tubular reactor, under plug-flow
conditions, the residence-time is the same for all elements of the effluent fluid. (K. G.
Denbigh).
RT
P
1+x
1x
V P
1
=
=
mf RT
k
( )
Mf
From experiment, it should be able to draw a curve of against xout, the slope of
which according to the first equation, should be
1+ x out
1x out
d
1 RT
=
d x out k P
n1
( )
RT
P
1+ x out
1(
n1 ] +n ln(
)
k
1xout
d
(
)=ln
d x out
ln
So, n and k can be obtained from the intercept and slope of the appropriate log-log
plot. This experiment is approaching to be isothermal (k and T outside the integral in
the first equation). If the reactor is not isothermal, then the first equation must be
written as
R
P
1+ x
1x
Tn
k
V
P
1
=
=
mf R T T
( )
Therefore, when the effect of wall heat transfer and of velocity gradient
operates simultaneously they might, under rather special circumstance, give rise to a
more complex kind of temperature profile. However, the most commonly observed
8
profiles obtained with exothermic reactions in externally cooled reactors. The reason
why the elementary design method is erroneous when the transverse gradients are
appreciable arises from the extreme sensitivity of reaction rate to changes of
temperature.
5.0 APPARATUS
i.
Material
i.
ii.
iii.
Deionize water
Sodium hydroxide
Ethyl acetate
10
6.0 PROCEDURE
GENERAL START-UP PROCEDURE
1. All valves were ensured initially closed except valve V7.
2. 20 litre of salt solution was prepared. For example, sodium chloride,
NaCl(0.025M).
3. The food tank B2 was filled with the NaCl solution.
4. The power for the control panel was turned up.
5. The water deionizer was connected to the laboratory water supply. Valve V3
was opened and feed tank B1 was filled up with the deionized water. Valve V3
was closed.
6. Valves V2 and V10 were opened. Pump P1 was switched on P1 flow
controller was adjusted to obtain a flow rate of approximately 700ml/min at
flow meter F1-01. The conductivity display was observed at low value then a
valve V10was closed and pump P1 was switched off.
7. Valves V6 and V12 were opened. Pump P2 was switched on. P2 flow
controller was adjusted to obtain a flow rate of approximately 700 ml/min at
flow meter F1-02. A valve V12 was closed and pump P2 was switched off.
8. The unit was ready for experiment.
EXPERIMENTAL PROCEDURE
Experiment 1: Pulse Input in a Tubular Flow Reactor
1. The general start-up procedures is performed.
2. Valve V9 is opened and pump P1 is switch on.
11
12
7.1
RESULTS
Conversion
Solution Mixtures
H2O
0.1M
0.1M
NaOH
100 mL
75 mL
50 mL
25 mL
-
0%
25%
50%
75%
100%
Et(Ac)
25 mL
50 mL
75 mL
100 mL
Concentration Conductivity
100 mL
100 mL
100 mL
100 mL
100 mL
of NaOH (M)
(mS/cm)
0.0500
0.0375
0.0250
0.0125
0.0000
5.64
4.25
3.70
3.37
74.2
Time (min)
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
Pulse
Conductivity (mS/cm)
Inlet
Outlet
3.0
0.0
0.3
0.0
0.1
2.5
0.0
2.3
0.0
0.4
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Step Change
Conductivity (mS/cm)
Inlet
Outlet
0.0
0.0
3.3
0.0
3.6
0.0
3.7
0.0
3.7
1.6
3.8
4.4
3.8
4.9
3.9
4.9
3.9
4.9
3.9
4.9
3.9
4.9
8.1 CALCULATIONS
Experiment 1 : Pulse Input in TBR
13
Time (min)
C ( t ) dt
0
14
t
t
Area
f ( 2)
2
f
( t 1t 2 )
( 1)+
= ( t 2t 1 ) [
E ( t 1+t 2 )
2
= (0.5 0.0) [
0.0+0.0
3
= 0.0g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (1.0 0.5) [
0.0+2.5
= 0.625 g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (1.5-1.0) [
2.5+ 2.3
3
= 1.2 g.min/ m
15
= ( t 2t 1 ) [
E ( t 1+t 2 )
2
= (2.0-1.5) [
2.3+ 0.4
3
= 0.675 g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (2.5-2.0) [
0.4+0.0
3
= 0.1 g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (3.0-2.5) [
0.0+0.0
= 0.0 g.min/ m
16
Area
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (3.5-3.0) [
0.0+0.0
= 0.0 g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (4.0-3.5) [
0.0+0.0
3
= 0.0 g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
2
= (4.5-4.0) [
0.0+0.0
= 0.0 g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (5.0-4.5) [
0.0+0.0
2
17
= 0.0 g.min/ m
5.0
C ( t ) dt
0.0
E (t)=
C (t)
C ( t ) dt
0
0.0
2.6
= 0.0
0.0
2.6
= 0.0
18
E(t)
2.5
2.6
= 0.962
2.3
2.6
= 0.885
0.4
2.6
= 0.154
0.0
2.6
= 0.0
0.0
2.6
= 0.0
19
E(t)
0.0
2.6
= 0.0
0.0
2.6
= 0.0
0.0
2.6
= 0.0
For t = 5.0, C(t) = 0.0
E(t)
0.0
2.6
= 0.0
Time (min)
Conductivity outlet
E(t)
0.0
0.0
0.000
0.5
0.0
0.000
1.0
2.5
0.962
1.5
2.3
0.885
2.0
0.4
0.154
2.5
0.0
0.000
3.0
0.0
0.000
3.5
0.0
0.000
4.0
0.0
0.000
4.5
0.0
0.000
5.0
0.0
0.000
20
21
E(t) vs Time
1.2
1
0.8
E(t) 0.6
0.4
0.2
0
Time (min)
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (0.5 0.0) [
0.0+0.0
2
22
= 0.0 g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (1.0-0.5) [
0.0+0.962
= 0.241 g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (1.5-1.0) [
0.962+ 0.885
= 0.462 g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
= (2.0-1.5) [
0.885+ 0.154
= 0.260 g.min/ m
23
= ( t 2t 1 ) [
E ( t 1+t 2 )
2
= (2.5-2.0) [
0.154+0.0
3
= 0.0385 g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (3.0-2.5) [
0.0+0.0
3
= 0.0 g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
= (3.5-3.0) [
0.0+0.0
= 0.0 g.min/ m
24
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (4.0-3.5) [
0.0+0.0
3
= 0.0 g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (4.5-4.0) [
0.0+0.0
3
= 0.0 g.min/ m
= ( t 2t 1 ) [
E ( t 1+t 2 )
]
2
= (5.0-4.5) [
0.0+0.0
3
= 0.0 g.min/ m
25
5.0
E ( t ) dt
0.0
5.0
tE ( t ) dt
Residence time, t m =
0.0
= 5.0(1.0015)
=5.0075
2
( tt m ) E ( t ) dt
3
( tt m ) E ( t ) dt
0.000
0.000
0.000
0.000
0.000
0.000
0.000
2.5
0.962
0.962
15.449
-61.915
1.5
2.3
0.885
1.328
10.888
-38.189
2.0
0.4
0.154
0.308
2.786
-4.189
2.5
0.0
0.000
0.000
0.000
0.000
3.0
0.0
0.000
0.000
0.000
0.000
3.5
0.0
0.000
0.000
0.000
0.000
4.0
0.0
0.000
0.000
0.000
0.000
4.5
0.0
0.000
0.000
0.000
0.000
5.0
0.0
0.000
0.000
0.000
0.000
= 2.001
= 2.598
= 29.173
= -104.293
Time
Outlet
E(t)
tE(t)
(min)
conductivity
0.0
(mS/cm)
0.0
0.000
0.5
0.0
1.0
Table 4: Table for mean residence time, variance and third moment
tE ( t ) dt
0
26
= 2.598
( tt m )2 E ( t ) dt
0
= 29.173
29.173
3
2
( tt m )3 E ( t ) dt
3
2 0
(104.293)
= -0.6619
Time (min)
27
C(t)
E(t)
tm
s3
(mS/cm)
0.0
0.00
0.000
0.00000
0.00000
0.00000
0.5
0.0
0.00
0.000
0.00000
0.00000
0.00000
1.0
0.0
0.00
0.000
0.00000
0.00000
0.00000
1.5
0.0
0.00
0.000
0.00000
0.00000
0.00000
2.0
1.6
3.20
0.029
0.00052
0.00103
0.00206
2.5
4.4
11.00
0.098
0.00218
0.00545
0.01361
3.0
4.9
14.70
0.131
0.00350
0.01048
0.03141
3.5
4.9
17.15
0.153
0.00477
0.01666
0.05823
4.0
4.9
19.60
0.175
0.00624
0.02488
0.09936
4.5
4.9
22.05
0.197
0.00790
0.03543
0.15916
5.0
4.9
24.50
0.218
0.00971
0.04839
0.24146
= 112.2
= 1.001
= 0.03264
= 0.14232
= 0.60529
Time
Outlet
(min)
conductivity
0.0
Table 5: Table for mean residence time, variance and third moment
28
C(t)
Ci t
E(t)
Ci ( t)/ Ci ( t )
tm
= tE(t )/ Ci t
= (tt m) E(t)/ C i t
s3
= (tt m) E(t)/ C i t
E(t) vs Time
0.25
0.2
0.15
E(t)
0.1
0.05
0
Time (min)
29
tE ( t ) dt
0
= 0.2710
( tt m )2 E ( t ) dt
0
= 1.054
95.930
3
2
( tt m )3 E ( t ) dt
3
2 0
(376.1077)
= 4.144
30
9.0
DISCUSSION
The objective of this experiment is to examine the effect of a pulse input and
step change input in a tubular flow rector. The experiment was run at constant flow
rate of 700 mL/min with de-ionised water in tank 1 and salt solution in tank 2 as the
reactants. Both reactants are mixed in the reactor.
For the first part of the experiment, the effect of pulse input has been
examined. Both inlet and outlet conductivity have been recorded for 5 minutes with
30 seconds interval. The result of this experiment then has been tabulated into Table 2.
Also, a graph of outlet conductivity against times has been plotted as shown in Figure
2. Based on the Figure 2, the highest conductivity of this experiment is at minute 1.0
which is 2.5 mS/cm. the conductivity then dropped to 1.3 mS/cm at minutes 1.5.
Further dropped has been shown in the graph at minutes 2.0 and it is constant
throughout the minutes 5.0 for which the outlet conductivity is 0 mS/cm.
For the second part of the experiment, the aim is to examine the effect of step
change input in tubular flow reactor. The only difference between the first experiment
and the second experiment is the reactant that flows in the reactor when time is taken.
For the first experiment, time is taken when de-ionised water is flows in the reactor
compared to experiment 2 where salt solution is flows in the reactor. A graph of outlet
conductivity against time is plotted as shown in Figure 4. Based on the graph, the
outlet conductivity started to increase at minute 2.0 with value of 1.6 mS/cm. Then, it
is further rise to 4.4 mS/cm at minute 2.5 and finally constant at 4.9 mS/cm started
from minute 3.0 until minute 5.0.
When compared between both Figure 2 and Figure 4, the outlet conductivity
of Figure 4 keep increasing until it become constant. The pattern is said as rapid
growth. As for Figure 2, the outlet conductivity is increases and reaches highest point
at some time before decreases and finally become constant until the end of the
experiment.
Another objective of this experiment is to construct a residence time
distribution (RTD) function for the tubular flow reactor. Both RTD function for pulse
input and step change input have been plotted as shown in Figure 3 and Figure 5
respectively.
31
For pulse input experiment, as shown in Figure 3, the peak of the graph is at
minute 1.0 where the value of 0.962. The graph start to show decrement starting from
minute 2.0 with E(t) value of 0.154 and finally become constant of 0.00 until the
experiment is finished.
For the pulse input graph, the residence time distribution calculated is 5.0075
minutes. Besides, there are 3 data that had been obtained and calculated which are
mean residence time, t variance (second moment),
moment),
s3
for the pulse input give a negative value and it called negative skew.
Compare to step change input experiment, as shown in Figure 5, the graph
start with 0.00 value of E(t) at minute 0.0 and minute 1.5. The graph has increase at
minute 2.0 with E(t) value of 0.029. The graph constantly shows increment until the
end of the experiment where the highest point is at minute 5.0 with the E(t) value of
0.218. Therefore, it can be concluded that for step change input experiment, the
residence time distribution is depends on the outlet conductivity.
For the step change, the graph almost same to the outlet conductivity versus
time which the residence time distribution (RTD) is increase within the time. For the
step change, the mean residence time distribution that calculated is 0.2710 minutes.
The other 2 data are also need to be calculate which are variance (second moment),
skewness give a positive value and it called positive skew compare to pulse input.
10.0
CONCLUSION
32
The objective of this experiment is to examine the effect of the pulse input and step
change input in a tubular flow reactor. Another objective is to construct the residence
time distribution (RTD) function for the tubular flow reactor. Based on the data
tabulated, the highest outlet conductivity for pulse input is at minute 1.0 which is 2.5
mS/cm. However, for step change input, the highest outlet conductivity is at minute
3.0 which is 4.9 mS/cm and it is constant until minute 5.0. The mean residence time,
t m , second moment, variance,
s3
for pulse
input is 2.598, 29.173 and -0.6619 respectively. The value of skewness for pulse
input is negative, and therefore it is said as negative skewness. Meanwhile, for step
change input, the mean residence time, t m , second moment, variance,
third moment, skewness,
and
respectively. The value of skewness for pulse input is positive, and therefore it is said
as positive skewness. All in all, the experiment is completed and succeeds.
11.0
RECOMMENDATIONS
i.
The general start-up must be done first to check the machine functioning
ii.
well.
Please make sure the solution that filled in the tank is correct solution and the
amount is also correct. Different substance reacts differently and lack of
iii.
iv.
12.0
REFERENCES
33
Bioreactors for Metal Bearing Wastewater Treatment : Tubular Reactor or Pluf Flow
Reactor, Retrieved on 28th October 2016,
http://www.metal.ntua.gr/~pkousi/e-learning/bioreactors/page_07.htm
Chemical Reaction Engineering Lab, Retrieved on 28th October 2016,
www.neduet.edu.pk/Chemical/PDF/CHEMICAL%20REACTION%20
ENGINEERING%20LAB.pdf
34