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CONTENT

PAGE

Abstract

Introduction

Objective

Theory

Apparatus

Procedure

Result

Sample calculation

Discussion

Conclusion

Recommendation

References

Appendix

ABSTRACT
This experiment is carry out to examine the effect of pulse input and step change in
tubular reactor as well as to construct a residence time distribution (RTD) function for the
tubular flow reactor. First of all, the equipment is set up before we run the experiment.
After that, we set up the flowrate to 700mL/min. After the conductivity for inlet and
outlet we collected are reaching to a constant value, the experiment is stopped. For the
first experiment, the conductivity for inlet and outlet are 0.1mS/cm and 0.1mS/cm while
for the second experiment are 5.7mS/cm and 3.5 mS/cm. The outlet conductivity, C(t) is
calculated and we get 4.4 for the first experiment and 7.15 for the second experiment.
Then, we are able to determine the distribution of exit time, E(t) for each 30 seconds. The
sum of E(t) we get is 1.00 which is the residence time distribution for both of the
experiment. The mean residence time, tm for this experiment are 0.9912 minute and
0.6275 minutes respectively. The variance, 2 and the skewness, s3 are also then
calculated. The value we get for 2 is 0.7459 and for the s3 is 1.6147 for the first
experiment. Meanwhile, the value of 2 is 1.0026 and for the s3 is 2.8707 for the second
experiment. Graphs for outlet conductivity, C(t) against time and distribution of exit time,
E(t) against time is plotted. The graphs we get from this experiment are just the same
with the graphs in the theory. The value of E(t) is depends on the value of C(t).
This experiment is carry out to examine the effect of pulse input and step change in
tubular reactor as well as to construct a residence time distribution (RTD) function for the
tubular flow reactor. First of all, the equipment is set up before we run the experiment.
After that, we set up the flowrate to 700mL/min. After the conductivity for inlet and
outlet we collected are reaching to a constant value, the experiment is stopped. For the
first experiment, the conductivity for inlet and outlet are 0.1mS/cm and 0.1mS/cm while
for the second experiment are 5.7mS/cm and 3.5 mS/cm. The outlet conductivity, C(t) is
calculated and we get 4.4 for the first experiment and 7.15 for the second experiment.
Then, we are able to determine the distribution of exit time, E(t) for each 30 seconds. The
sum of E(t) we get is 1.00 which is the residence time distribution for both of the
experiment. The mean residence time, tm for this experiment are 0.9912 minute and
0.6275 minutes respectively. The variance, 2 and the skewness, s3 are also then
2

calculated. The value we get for 2 is 0.7459 and for the s3 is 1.6147 for the first
experiment. Meanwhile, the value of 2 is 1.0026 and for the s3 is 2.8707 for the second
experiment. Graphs for outlet conductivity, C(t) against time and distribution of exit time,
E(t) against time is plotted. The graphs we get from this experiment are just the same
with the graphs in the theory. The value of E (t) depends on the value of C (t).

INTRODUCTION
The reactants are continually consumed as they flow down the length of the reactor in the
tubular reactor. Flow in tubular reactor can be laminar or turbulent. 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 conveniently long reactors or may require unacceptable high
feed rates.
However, many tubular reactors that are used to carry out a reaction do not fully conform
to this idealized flow concept. A pulse of tracer injected at the inlet would not undergo
any dispersion as it passed through the reactor and would appear as a pulse at the outlet in
an ideal plug flow reactor. The degree of dispersion that occurs in a real reactor can be
measured by following the concentration of tracer versus time at the exit. This procedure
is known as the stimulus-response technique. The nature of the tracer peak gives an
indication of the non-ideal that would be characteristic of the reactor.
It is impossible for the reaction to proceed to 100% completion for most chemical
reactions. The percent completion increases as the rate of reaction decreases until the
point where the system reaches dynamic equilibrium. The equilibrium point for most
systems is less than 100% complete. For this reason in order to separate any remaining
reagents from the desired product, a separation process often follows a chemical reactor.
These reagents may sometimes be reused at the beginning of the process.
Residence Time Distribution (RTD) analysis can be used to inspect the malfunction of
chemical reactors. It can also be very useful in the estimation of effluent properties and in
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modeling reactor behavior. This technique is extremely important in teaching reaction


engineering, in particular when the non-ideal reactors become the issue. By impulse and
step tracer injection techniques can determine RTDs, and applying them to the modeling
of the reactor flow and to the estimation of the behavior of a nonlinear chemical
transformation. The RTD technique has also been used for the experimental
characterization of flow pattern of a packed bed and a tubular reactor that exhibit,
respectively, axially dispersed plug flow and laminar flow patterns (FEUP).
Another important field of RTD applications lies in the prediction of the real reactor
performance. Nowadays, the concepts of macro and micro mixing are fundamental. Each
macro mixing level is expressed in the form of a specific RTD. There is a given micro
mixing level, which lies between two limiting cases, complete segregation and perfect
micro mixing.

OBJECTIVE
1. To examine the effect of pulse input in tubular flow reactor.
2. To examine the effect of a step change input in a tubular flow reactor
3. To construct a residence time distribution (RTD) function for the tubular flow
reactor

THEORY
In a 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 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.
In the ideal tubular reactor, which is called the plug flow reactor, specific assumptions
are made about the extent of mixing:
1. no mixing in the axial direction, i.e., the direction of flow
2. complete mixing in the radial direction
3. a uniform velocity profile across the radius.
The absence of longitudinal mixing is the special characteristics of this type of reactor. It
is an assumption at the opposite extreme from the complete mixing assumption of the
ideal stirred tank reactor.
The validity of the assumptions will depend on the geometry of the reactor and the flow
conditions.
Deviations, which are frequent but not always important, are of two kinds:
1. mixing in longitudinal direction due to vortices and turbulence
2. incomplete mixing in radial direction in laminar flow conditions
Mass Balance
For a time element t and a volume element V, the mass balance for species i is given
by the following equation:
QA CA v t- QA CAv+v t - rAVt = 0
Where QA : volumetric flow rate of reactant A to the reactor, L/s
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(10.1.1)

CA : concentration of reactant A, mol/L


rA : rate of disappearance of reactant A, mol/Ls

The conversion, X, is defined as:


X = (initial concentration - final concentration) / (initial concentration)

Since the system is at steady state, the accumulation term in Equation (10.1.1) is zero.

Equation (10.1.1) can be written as:


-QA CA - rAV = 0

(10.1.2)

Dividing by V and taking limit as V 0


dCA/dV = -rA/QA

(10.1.3)

This is the relationship between concentration and size of reactor for the plug flow
reactor. Here rate is a variable, but varies with longitudinal position (volume in the
reactor, rather than with time).
Integrating,
-dV/ QA = dCA/rA

At the entrance:

V=0
CA = CA0

At the exit:

V = VR (total reactor volume)


6

(10.1.4)

CA = CA (exit conversion)

VR = dCA
QA

rA

APPARATUS
1. SOLTEC Tubular Flow Reactor Instrument.
2. Clock watch
3. De-ionized water and 0.025M Sodium Chloride solution.

PROCEDURE
Experiment 1 :
1. Perform the general start-up as in section 4.1
2. Open valve V9 and switch on pump P1
3. Adjust P1 floe controller to give a constant flow rate f de-ionized water into the reactor
R1 at approximately 700ml/min at F1-01
4. Let the de-ionized water to continue flowing through the reactor until the inlet (Q1-01)
and the outlet (Q1-02) conductivity values are stable a low levels. Record both
conductivity values.
5. Close valve V9 and switch off pump P1
6. Open valve V11 and switch on pump P2. Start the timer simultaneously
7. Adjust pump P2 flow controller to give a constant flow rate of salt solution into the
reactor R1 at 700ml/min at F1-02
8. Let the salt solution to flow for 1 minute, then reset and restart the timer. This will start
the time at the average pulse input.
9. Close valve V9 and switch off pump P2. Then, quickly open valve V9 and switch on
pump P1.
10. Make sure the de-ionized water flow rate is always maintained at 700ml/min by adjusting
P1 flow controller

11. Start recording both the inlet (Q1-01) and outlet (Q1-02) conductivity values at regular
intervals of 30 seconds.
12. Continue recording the conductivity values until all readings are almost constant and
approach the stable low level values.

Experiment 2 :
1. Perform the general start-up as in section 4.1
2. Open valve V9 and switch on pump P1
3. Adjust P1 floe controller to give a constant flow rate f de-ionized water into the reactor
R1 at approximately 700ml/min at F1-01
4. Let the de-ionized water to continue flowing through the reactor until the inlet (Q1-01)
and the outlet (Q1-02) conductivity values are stable a low levels. Record both
conductivity values.
5. Close valve V9 and switch off pump P1
6. Open valve V11 and switch on pump P2. Start the timer simultaneously
7. Record both the inlet (Q1-01) and outlet (Q1-02) conductivity values at regular intervals
30 seconds
8. Continue recording the conductivity values until all readings are almost constant.

RESULTS
Experiment 1: Pulse Input in a Turbular Flow Reactor
Flow rate
= 700 mL/min
Input type
= De-ionized Water
Time
(min)

0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5

Conductivity
(mS/cm)

C(t)

E(t)

tm

s3

Inlet

Outlet

Cit

Ci(t)
Ci(t)

t*E(t)/

(t - tm) 2 *
E(t)/

(t - tm) 3 *
E(t)/

0.0
0.0
0.0
0.0
0.0
0.1
0.2
0.1

0.0
0.0
0.0
0.0
0.0
0.1
0.0
0.0

0.00
0.00
0.00
0.00
0.00
0.05
0.00
0.00

0.0000
0.0000
0.0000
0.0000
0.0000
0.0213
0.0000
0.0000

0.0000
0.0000
0.0000
0.0000
0.0000
0.0227
0.0000
0.0000

0.0000
0.0000
0.0000
0.0000
0.0000
0.0556
0.0000
0.0000

0.0000
0.0000
0.0000
0.0000
0.0000
0.1378
0.0000
0.0000

4.0
4.5
5.0
5.5
6.0

0.1
1.4
0.0
2.0
0.0
1.0
0.0
0.2
0.0
0.0
SUMMATION

0.70
1.00
0.50
0.10
0.00
2.35

0.2979
0.4255
0.2127
0.0426
0.0000
1.0000
Table 1

0.5071
0.8148
0.4526
0.0997
0.0000
1.8969

Graph 1: outlet conductivity against time

1.5466
2.4589
1.8717
0.5287
0.0000
6.4615

5.4021
9.0618
8.5112
2.8549
0.0000
25.9678

Graph 2: distribution of exit time, E(t) against time

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Experiment 2: Step Change Input in a Turbular Flow Reactor


Flow rate
= 700 mL/min
Input type
= De-ionized Water
Time
(min)

0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0
7.5
8.0
8.5
9.0
9.5
10.0
10.5
11.0
11.5
12.0
12.5
13.0
13.5
14.0

Conductivity
(mS/cm)

C(t)

E(t)

tm

s3

Inlet

Outlet

Cit

Ci(t)
Ci(t)

t*E(t)/

(t - tm) 2 *
E(t)/

(t - tm) 3 *
E(t)/

0.0
3.5
3.6
3.6
3.6
3.6
3.6
3.6
3.7
3.6
3.6
3.6
3.6
3.7
3.7
3.6
3.7
3.7
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6
3.6

0.0
0.0
0.0
0.0
0.4
1.7
2.0
2.1
2.1
2.1
2.1
2.2
2.2
2.2
2.3
2.3
2.3
2.4
2.4
2.5
2.5
2.6
2.6
2.7
2.8
2.8
2.9
2.9
3.0

0.00
0.00
0.00
0.00
0.20
0.85
1.00
1.05
1.05
1.05
1.05
1.10
1.10
1.10
1.15
1.15
1.15
1.20
1.20
1.25
1.25
1.30
1.30
1.35
1.40
1.40
1.45
1.45
1.50

0.0000
0.0000
0.0000
0.0000
0.0033
0.0140
0.0165
0.0173
0.0173
0.0173
0.0173
0.0182
0.0182
0.0182
0.0190
0.0190
0.0190
0.0198
0.0198
0.0206
0.0206
0.0215
0.0215
0.0223
0.0231
0.0231
0.0239
0.0239
0.0248

0.0000
0.0000
0.0000
0.0000
0.0001
0.0006
0.0008
0.0010
0.0011
0.0013
0.0014
0.0017
0.0018
0.0020
0.0022
0.0024
0.0025
0.0028
0.0029
0.0032
0.0034
0.0037
0.0039
0.0042
0.0046
0.0048
0.0051
0.0053
0.0057

0.0000
0.0000
0.0000
0.0000
0.0002
0.0014
0.0024
0.0035
0.0046
0.0058
0.0071
0.0091
0.0108
0.0127
0.0154
0.0176
0.0201
0.0236
0.0264
0.0307
0.0340
0.0391
0.0429
0.0486
0.0548
0.0595
0.0666
0.0718
0.0801

0.0000
0.0000
0.0000
0.0000
0.0004
0.0036
0.0073
0.0122
0.0183
0.0260
0.0357
0.0499
0.0648
0.0824
0.1074
0.1321
0.1604
0.2005
0.2380
0.2912
0.3396
0.4103
0.4717
0.5590
0.6579
0.7437
0.8655
0.9692
1.1216

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14.5
15.0
15.5
16.0
16.5
17.0
17.5
18.0
18.5
19.0
19.5
20.0
20.5
21.0
21.5
22.0
22.5
23.0
23.5

3.6
3.1
3.6
3.1
3.6
3.1
3.6
3.1
3.7
3.2
3.6
3.2
3.6
3.2
3.6
3.2
3.6
3.3
3.6
3.4
3.6
3.4
3.6
3.4
3.6
3.4
3.6
3.5
3.6
3.5
3.6
3.5
3.6
3.5
3.6
3.5
3.6
3.5
SUMMATION

1.55
1.55
1.55
1.55
1.60
1.60
1.60
1.60
1.65
1.70
1.70
1.70
1.70
1.75
1.75
1.75
1.75
1.75
1.75
60.6

0.0256
0.0256
0.0256
0.0256
0.0264
0.0264
0.0264
0.0264
0.0272
0.0281
0.0281
0.0281
0.0281
0.0289
0.0289
0.0289
0.0289
0.0289
0.0289
1.0005

12

0.0061
0.0063
0.0065
0.0068
0.0072
0.0074
0.0076
0.0078
0.0083
0.0088
0.0090
0.0093
0.0095
0.0100
0.0103
0.0105
0.0107
0.0110
0.0112
0.2328

0.0887
0.0950
0.1014
0.1081
0.1185
0.1258
0.1333
0.1410
0.1535
0.1672
0.1762
0.1853
0.1947
0.2101
0.2202
0.2306
0.2412
0.2520
0.2631
3.8945

1.2862
1.4239
1.5711
1.7281
1.9544
2.1375
2.3317
2.5374
2.8381
3.1761
3.4335
3.7044
3.9893
4.4102
4.7328
5.0707
5.4244
5.7941
6.1803
71.2929

Graph 1: outlet conductivity against time

Graph 2: distribution of exit time, E(t) against time


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SAMPLE OF CALCULATION

Area = (0.10X0.0)+(0.10X0.5) +(0.20X0.5)+(2.0X0.5)+(1.90X0.5)+


(0.40X0.5)+(0.20X0.5) +(0.10X0.5)+(0.10X0.5)+ (0.10X0.5) +(0.10X0.5)
Area = 2.35

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DISCUSSION
In this experiment, the Tubular Flow Reactor was conducted to examine the effect of a
pulse input and step change in a tubular flow reactor and also to construct a residence
time distribution (RTD) function for the tubular flow reactor. De-ionized water and Salts
solution was used as chemicals to determine the conductivity.
To construct a residence time distribution (RTD) function for the tubular flow
reactor with pulse input, first we find the area under the c curve by using a numerical
evaluation of integrals. After that using formula

, we find the

values of E(t). From that, we plot E(t) as a function of time. This is the residence time
distribution (RTD) function for the plug flow reactor. On the other hand, we use graphical
method to find E(t) for step input. The steps were more complex than the steps use in
finding the area under curve. Besides that, there are high probabilities that some error
may occur while trying to find the differentiation of conductivity when using this method.
The step input is usually easier to carry out than the pulse test. However, step input
involves differentiation of the data when to obtain the RTD. This may lead to large errors
(Forgler, 2006).
When comparing the RTD function plot between experiment 1 and 2, we can see
the different between both graphs.
The two most important parameters that characterize a curve in graph are the
mean time which indicates when the wave of tracer passes the measuring point and the
variances which indicates how much tracer has spread out during the measurement time
(Coulson & Richardson, 1999). As we compare the pulse input and step change input,
pulse input given higher mean time but lower variances. So, we can say that step change
input help the tracer to spread out more amount that pulse input. As we see the time,
pulse input process was faster than step change input.
The advantages of using Tubular Flow Reactor are it has high volumetric unit
conversion, it can run for a long period of time with maintenance and the heat transfer
can be optimized by using tubes in parallel while the disadvantages of using this reactor
15

are the temperatures are difficult to control, variability of products which mean the input
product might be not the same output and high operating cost.
The errors involved during this experiment were:

We must open the valve and pump simultaneously for example valve V11 and

pump P2. To open them simultaneously is a bit difficult for us.


During taken of time by using stopwatch, we cannot stop at accurate time. So, the
data might be not consistent.

CONCLUSION

From the results obtained and the sample calculation done, several graphs were plotted.
For experiment 1, the effect of pulse input in a tubular flow reactor was examined. The
flow rate was kept constant at 700 ml/min and de-ionized water was used. The
summation of C(t) came to a result of 2.35, and the sum of E(t) came to a result of 1.00.
As seen from the graph, both outlet conductivity and E(t) remained constant until minute
3.5, then took a sharp increase in minute 4, and a big decline after. This means that a unit
pulse response was recorded at the outlet stream, indicating a flow of conductivity.
For experiment 2, the effect of a step change input was examined. The flow rate was also
kept constant at 700 ml/min and de-ionized water was also used. The results and
calculations show that the summation of the conductivity was 60.6 and the sum of E(t)
was 1.0005. From the graphs plotted, it is seen that the data increases sharply after some
time, and gradually increases after.
The experiment was considered a success as all objectives were achieved.

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RECOMMENDATIONS
There are a few recommendations for this experiment. Before starting the experiment,
make sure that students read a lab manual and understand how to do. First, make sure all
the apparatus is cleaned before use. Then, make sure the time taken to get the
conductivity is 30 seconds and the flowrate is maintained a 700ml/min.

REFERENCES
http://www.solution.com.my/pdf/BP101(A4).pdf
http://www.google.com.my/search?hl=en&q=tubular+flow+reactor+lab+report&bav=on.
http://smk3ae.files.wordpress.com/2007/10/reaksi-kinetik.pdf

APPENDIX

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