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1.

0 ABSTRACT

This experiment is to carry out by determine the suitable methodology of experiment


by using Tubular Flow Reactor model BP: 101, to examine the effect of a pulse input and
step change input in a tubular flow reactor and to construct a residence time distribution
(RTD) function for the tubular flow reactor. In this experiment sodium hydroxide and ethyl
acetate react in Tubular Flow Reactor. So from the Graph 1 is conductivity vs conversion
conductivity smooth. . From the experiment , the outlet conductivity, C(t) that had been
calculated for step change is 46.55. The distribution of exit time, E (t) is calculated for each
30 second until 5 minutes interval. The sum of E (t) for pulse input and step change are
2.6036 and 1.0000 respectively. The mean residence time, t m for pulse input is 6.0939
minutes. The variance, 2 and skewness, s3 are also calculated. For pulse input are 45.8578
and -11.4477 while for step change are 0.33492 and 1.41875. Graph for outlet conductivity,
C (t) against time and distribution of exit time, E (t) against time are plotted. The objectives
have been achieved and related to the theory and the experiment is success.

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2.0 INTRODUCTIONS

Tubular Flow Reactor (Model: BP 101) has been designed to introduce as a plug
flow reactor by studying the second order reaction between dilute caustic soda and ethyl
acetate. A tubular reactor is a vessel which flow is continuous and at steady state, so that
conversion of the chemicals and other dependent variables are functions of position within
the reactor. Whereas, in the ideal tubular reactor, the fluids flow as if they were solid plugs
and reaction time is the same for all flowing material at any given tube cross section.

Moreover, flow in tubular reactors can be laminar, as with viscous fluids in small-
diameter 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. In addition to that, for slow reactions and especially in small
laboratory and pilot-plant reactors, establishing turbulent flow can result in inconveniently
long reactors.

Tubular flow reactors applications which are:

Large-scale reactions

Fast reactions

Homogeneous or heterogeneous reactions

Continuous production

High-temperature reactions

In an ideal tubular flow rector, 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.
Also, the degree of dispersion that occurs in a real reactor can be assessed by following the

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concentration of tracer versus time at the exit. This procedure is called the stimulus-
response technique.

A distribution of residence time of a tubular reactor that is used, didactically, in the


Chemical Engineering Laboratory. Residence time distributions are measured by introducing
a non-reactive tracer into the system at the inlet. The tracer of concentration is changed
according to a known function and the response is found by measuring the concentration of
the tracer at the outlet. The selected tracer should not modify the physical characteristics of
the fluid and the introduction of the tracer should not modify the hydrodynamic conditions.

3.0 AIMS AND OBJECTIVES

The main purpose of conducting the experiment is

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

4.0 THEORY

Tubular reactors in which homogeneous reactions are conducted can be empty or


packed conduits of various cross-sectional shape. Pipes, as example tubular vessels of
cylindrical shape, dominate. The flow can be turbulent or laminar. The questions arise as to
how to interpret the performance of tubular reactors and how to measure their departure
from plug flow behaviour. As the volume of tubular flow reactor :

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As steady state, the general mole balance is reduced to :

rA is an indirect function of y. That is, rA is a function of reactant concentration, which


is a function of the position, y down the reactor. The volume, is the product of the cross-
sectional area, A of the reactor and the reactor length , y.

Above expression substitute into the following equation:

The RTD is determined experimentally by injecting an inert chemical, molecule, or


atom, called a tracer, into the reactor at some time T= 0 and then measuring the tracer
concentration, C, 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.

Then, we choose an increment of time of time t, sufciently small that the


concentration of tracer, C (t), exiting between time t and t + t is essentially the same. The
amount of tracer material N leaving reactor between time t and t + t is then

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If we now divide by the total amount of material that was injected into the reactor, N0,
we obtain:

Which represents the fraction of material that has a residence time in the reactor
between time t and t + t. For pulse injection we dene:

Writing the equation as :

Integrating we obtain :

The volumetric flow rate v is usually constant, so we can define E(t) as

5.0 APPARATUS AND MATERIALS

1. SOLTEQ Tubular Reactor (Model: BP 101)


2. Conical flask
3. Calibration meter
4. Sodium hydroxide, NaOH (0.1M)
5. Sodium Acetate, Na(Ac) (0.1M)
6. Deionised water, H2O

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6.0 PROCEDURES

GENERAL START-UP PROCEDURE:

1. The valves have been ensure that are initially closed except valves V7
2. The solutions have been prepared for each experiment

Tank Experiments 1 & 2 Experiments 3 & 4


B1 Deionized water 0.1M NaOH solution
B2 0.05M NaCl solution 0.1M Et(Ac) Solution
*Connect the water de-ionizer to the laboratory water supply

3. The power are turned on at control panel


4. The water jacket B4 are filled and pre-heater B5 with clean water. Open valves V13
and V8. Pump P3 has been switched on to circulate water through pre-heater B5.
5. The stirrer on motor M1 have been switched on and the speed about 200 rpm are
being set.
6. The valves V6 and V12 are open. Pump P1 are switched on. P1 are adjusted to flow
rate of 700 ml/min at flow meter F1-01. V10 valves are closed and switched off pump
P1.
7. The valves V6 and V12 are open. Pump P2 are switched on. P2 are adjusted to flow
rate of 700 ml/min at flow meter F1-02. V12 valves are closed and switched off pump
P2.
8. For experiment 4, perform the following additional steps:
a) The heaters are switched on
b) Open valves V17 to let cooling water flowing through the cooling tubes.
c) The temperature are set to set point TIC-01 to the desired temperature.
9. The units are now ready for experiments.

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EXPERIMENTAL PROCEDURES

Experiment 1: Pulse Input in a Tubular Flow Reactor

1. Valve V9 is opened and pump P1 is switch on.


2. Pump P1 flow controller is adjusted to give a constant flow rate of de-ionized
water into the reactor R1 at approximately 700 ml/min at Fl-01.
3. Let the de-ionized water to continue flowing through the reactor until the inlet
(Ql-01) and outlet (Ql-02) conductivity values are stable at low levels. Both
conductivities values are recorded.
4. Valve V9 is closed and pump P1 is switch off.
5. Valve V11 is opened and Pump P2 is switch on. The timer is started
simultaneously.
6. Pump P2 flow controller is adjusted to give a constant flow rate of salt solution
into the reactor R1 at 700 ml/min at Fl-02.
7. 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.
8. Valve V11 is closed and pump P2 is switch off. Then, open valve V9 quickly
and pump P1 is switch on.
9. Make sure that the de-ionized water flow rate is always maintained at 700
ml/min by adjusting P1 flow controller.
10. Both the inlet (Ql-01) and outlet (Ql-02) conductivity a value at regular
intervals of 30 seconds is start recorded.
11. The conductivity values is continue recording until all readings are almost
constant and approach the stable low level values.

Experiment 2: Step Change Input in a Tubular Flow Reactor

1. Valve V9 is opened and pump P1 is switch on.


2. Pump P1 flow controller is adjusted to give a constant flow rate of de-ionized
water into the reactor R1 at approximately 700 ml/min at Fl-01.
3. Let the de-ionized water to continue flowing through the reactor until the inlet
(Ql-01) and outlet (Ql-02) conductivity values are stable at low levels. Both
conductivities values are recorded.
4. Valve V9 is closed and pump P1 is switch off.
5. Valve V11 is opened and Pump P2 is switch on. The timer is started
simultaneously.
6. Both the inlet (Ql-01) and outlet (Ql-02) conductivity a value at regular
intervals of 30 seconds is start recorded.
7. The conductivity values is continue recording until all readings are almost
constant.

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GENERAL SHUT DOWNBPROCEDURE:

1. Switched off both pumps P1 and P2 and P3. The valves V2 and V6 are closed.
2. Switched off the heaters.
3. The cooling water are kept circulated through the reactor while stirrer motor is
running to allowed water jacket to cool down to room temperature.
4. If the experiment are not going to be used for long period of time , drawn all the liquid
from the unit by opening valves V1 to V16.The feed tank are rinsed with clean water.
5. Turn off the power for the control panel.

7.0 RESULTS AND CALCULATIONS

Experiment 1 : Pulse input in Tubular Flow Reactor

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Flow rate : 700mL/min

Input type : Pulse input

Time (min) Conductivity (ms/cm)


Inlet Outlet
0.0 0.4 0.0
0.5 0.2 0.0
1.0 0.2 0.3
1.5 0.1 1.5
2.0 0.0 1.7
2.5 0.0 1.5
3.0 0.0 0.9
3.5 0.0 0.6
4.0 0.0 0.3
4.5 0.0 0.1
5.0 0.0 0.0

Outlet Conductivity (ms/cm) against time (min)

Graph 1 : Outlet Conductivity (ms/cm) against time (min)

C ( t ) dt = Area under the graph


0

Area = ( t 1 - t 2 ) [ f ( t 1 ) + f (t 2)
2 ]

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For time (1.0-1.5) minutes

Area = ( t 2 t 1 [ E (t 1+t 2)
2 ] = (1.5 1.0) [ 0.3+1.5
2 ] = 0.45 g .min m3

For time (1.5 2.0) minutes

Area = ( t 2 t 1 [ E (t 1+t 2)
2 ] = (2.0 1.5) [ 1.5+1.7
2 ] = 0.80 g .min m
3

For time (2.0 2.5) minutes

Area = ( t 2 t 1 [ E (t 1+t 2)
2 ] = (2.5 2.0) [ 1.7+1.5
2 ] = 0.80g .min m3

For time (2.5 3.0) minutes

Area = ( t 2 t 1 [ E (t 1+t 2)
2 ] = (3.0 2.5) [ 0.9+1.5
2 ] = 0.60g .min m
3

So the total area or C ( t ) dt = ( 0.45+ 0.80 + 0.80 + 0.60) = 2.65g.min/m3


0

C (t)
E (t)=
C ( t ) dt
0

For t = 0, C(t) = 0 E(t)=0/2.65=0

For t = 0.5, C(t) = 0 E(t)=0/2.65=0

For t = 1.0, C(t) = 0.3 E ( t ) =0.3/2.65=0.1132

For t = 1.5, C(t) = 1.5 E(t)=1.5/2.65=0.5660

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For t = 2.0, C(t) = 1.7 E(t)=1.7/2.65=0.6415

For t = 2.5, C(t) = 1.5 E(t)=1.5/2.65=0.5660

For t = 3.0, C(t) = 0.9 E(t)=0.9/2.65=0.3396

For t = 3.5, C(t) = 0.6 E(t)=0.6/2.65=0.2264

For t = 4.0, C(t) = 0.3 E(t)=0.3/2.65=0.1132

For t = 4.5, C(t) = 0.1 E(t)=0.1/2.65=0.0377

For t = 5.0 , C(t) = 0 E(t)=0/2.65=0

Residence time distribution (RTD) function for plug flow reactor:

Time (min) Conductivity outlet E(t)


0.0 0.0 0.0000
0.5 0.0 0.0000
1.0 0.3 0.1132
1.5 1.5 0.5660
2.0 1.7 0.6415
2.5 1.5 0.5660
3.0 0.9 0.3396
3.5 0.6 0.2264
4.0 0.3 0.1132
4.5 0.1 0.0377
5.0 0.0 0.0000

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E(t) against Time (min)

Graph 2 : E(t) against Time (min)

For time (0 0.5)minutes = 0

For time (0.5 -1.0)minutes

Area = ( t 2 t 1 [ E (t 1+t 2)
2 ] = (1 0.5) [ 0.1132+ 0
2 ] = 0.0283m2

For time (1 1.5) minutes

Area = ( t 2 t 1 [ E (t 1+t 2)
2 ] = (1.5 1) [ 0.5660+0.1132
2 ] = 0.1698m2

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For time (1.5 2.0 )minutes

Area = ( t 2 t 1 [ E (t 1+t 2)
2 ] = (2 1.5) [ 0.6415+0.5660
2 ] = 0.3019m2

For time (2.0 2.5) minutes

Area = ( t 2 t 1 [ E (t 1+t 2)
2 ] = (2.5 2) [ 0.6415+0.5660
2 ] = 0.3019m2

For time (2.5 -3.0) minutes

Area = ( t 2 t 1 [ E ( t 1 +t 2 )
2 ] = (3 2.5) [ 0.3396+ 0.5660
2 ]
= 0.2264m2

For time (3 -3.5) minutes

Area = ( t 2 t 1 [ E (t 1+t 2)
2 ] = (3.5- 3) [ 0.3396+0.2264
2 ] = 0.1415m2

For time (4.0-3.5) minutes

Area = ( t 2 t 1 [ E (t 1+t 2)
2 ] = (4.0- 3.5) [ 0.2264+0.1132
2 ] = 0.0849m2

For time (4.0-4.5) minutes

Area = ( t 2 t 1 [ E (t 1+t 2)
2 ] = (4.5- 4.0) [ 0.0377+ 0.1132
2 ] = 0.0377m2

E ( t ) dt = Total area under the graph = (0.0283 + 0.1698 +0.3019 +0.3019+


0

0.2264+0.1415+0.0849+0.0377)= 1.2924m2


Residencetime , t m= tE ( t ) dt = 5.0 (1.2924) =6.462
0

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time (min) Outlet E(t) tE(t)
conductivity (t-tm)2E(t)dt (t-tm)3E(t)dt
(mS/cm)
0.0 0.0 0.0000 0.0000 0.0000 0.0000
0.5 0.0 0.0000 0.0000 0.0000 0.0000
1.0 0.3 0.1132 0.1132 3.3771 -18.4460
1.5 1.5 0.5660 0.8490 13.9357 -69.1491
2.0 1.7 0.6415 1.2830 12.7719 -56.9882
2.5 1.5 0.5660 1.4150 8.8848 -35.2014
3.0 0.9 0.3396 1.0188 4.0702 -14.0912
3.5 0.6 0.2264 0.7924 1.9863 -5.8834
4.0 0.3 0.1132 0.4528 0.6861 -1.6893
4.5 0.1 0.0377 0.1697 0.1451 -0.2847
5.0 0.0 0.0000 0.0000 0.0000 0.0000

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=2.6036 =6.0939 =45.8578 =-201.7333

Mean residence time, t m= tE ( t ) dt= 6.0939


0

Second moment, variance ,


2
= (ttm )2 E(t) dt
0

= 45.8578
3 1
s=
Third moment, skewness, 3
2
(ttm )3 E(t) dt
0

1
3
= 2 -201.7333) = -11.4477
(6.7718)

Experiment 2: Step Change Input in a Turbular Flow Reactor

Flow rate = 700 mL/min

Input type : Step change

Time (min) Conductivity (mS/cm)


Inlet outlet
0.0 3.0 0.0
0.5 3.2 0.0
1.0 3.3 0.0
1.5 3.3 0.2
2.0 3.4 1.2
2.5 3.4 1.8
3.0 3.4 1.9
3.5 3.4 1.9

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4.0 34 2.0
4.5 3.5 2.0
5.0 3.5 2.0

Outlet Conductivity (ms/cm) against Time (min)

Graph 3: Graph outlet conductivity (mS/cm) against time (min)

Time Conductivity C(t) E(t) tm 2 s3


(min) (mS/cm)

Inlet Outlet Cit Ci(t)/Ci(t) t*E(t)/ (t - tm) 2 * (t - tm) 3 *

C i t E(t)/ E(t)/

C i t C i t

0.00 3.0 0.0 0.000 0.00000 0.00000 0.00000 0.00000

0.50 3.2 0.0 0.000 0.00000 0.00000 0.00000 0.00000

1.00 3.3 0.0 0.000 0.00000 0.00000 0.00000 0.00000

1.50 3.3 0.2 0.300 0.00644 0.00021 0.00031 0.00047

2.00 3.4 1.2 2.400 0.05156 0.00222 0.00442 0.00883

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2.50 3.4 1.8 4.500 0.09667 0.00519 0.01293 0.03225

3.00 3.4 1.9 5.700 0.12245 0.00789 0.02355 0.07046

3.50 3.4 1.9 6.650 0.14286 0.01074 0.03736 0.13037

4.00 34 2.0 8.000 0.17186 0.01477 0.05864 0.23367

4.5 3.5 2.0 9.000 0.19334 0.01869 0.08341 0.37378

5.0 3.5 2.0 10.000 0.21482 0.02307 0.11431 0.56891

=46.55 =1.0000 =0.08278 = 0.33492 =1.41875

Residence time distribution (RTD) function for plug flow reactor

E(t) against Time (min)

Graph 4 : E(t) against Time (min)

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SAMPLE OF CALCULATION

C (t)dt = C i t=Area
0

So based on the table, Area is 46.55m2

Example of calculation at t=1.50min

t E( t)
t m=
Area

1.50 0.00644
t m=
46.55

t m=0.00021

2
2 ( tt m ) E(t)
=
Area

( 1.50.00021 )2 0.00644
2=
46.55

2=0.00031

3
3 ( t t m ) E(t )
s=
Area

3 ( 1.500.00021 )3 0.00644
s=
46.55

s 3=0.00047

8.0 DISCUSSION

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The objective of tubular flow reactor is to examine the effect of a pulse input and step
change input in a tubular flow reactor and to construct a residence time distribution (RTD)
function for the tubular flow reactor. In this experiment we have run in those 700 mL/min for
flowrate. Where when analyse is running, those conductivity for inlet and outlet of the result
required been recorded at those time of time until the data is consistent.

Based on the result and calculations, the flowrate of arrangement are steady at 700
ml/min. So, the graph of outlet conductivity versus times had been plotted as the result
given. From the graph the outlet conductivity that had been plotted is 1.7 mS/cm at time of 2
minutes which is the most highest value from other timing. Moreover , from the results was
not contrast from the hypothesis that recorded that the conductivity is achieving zero at time
of 5.0 minutes. As conclude from conductivity , the objective are achieved.

Residence time circulation (RTD) function graph has been plotted according to exit
time E(t) against time from the table recorded. Based on the graph plotted, are mostly same
with the conductivity graph where the hypothesis are achieved as conductivity graph. As the
pulse input graph, the residence time distribution calculated is 6.462 minutes. Also, t m , 2
and ,s3 that recorded 6.0939, 45.8578 and -11.4477 respectively.

In addition to that, the step change, the graph are similar to the outlet conductivity
against time which the residence time distribution (RTD) is increase within the time. Where
the data that are been calculated which are tm, 2 and s3 are 0.00021, 0.00031 and 0.00047
respectively. The skewness give a positive value and it called positive skew compare to
pulse input.

9.0 CONCLUSION

Based on the objectives of this experiment are success which is to examine the effect of
a pulse input and step change input in a tubular flow reactor and to construct a residence

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time distribution (RTD) function for the tubular flow reactor. We can conclude that the
experiment are success and there is some error during the experiment.

From the experiment , the outlet conductivity, C(t) that had been calculated for step
change is 46.55. The distribution of exit time, E (t) is calculated for each 30 second until 5
minutes interval. The sum of E (t) for pulse input and step change are 2.6036 and 1.0000
respectively. The mean residence time, tm for pulse input is 6.0939 minutes. The variance, 2
and skewness, s3 are also calculated. For pulse input are 45.8578 and -11.4477 while for
step change are 0.33492 and 1.41875. Graph for outlet conductivity, C (t) against time and
distribution of exit time, E (t) against time are plotted. As for conclusion , the experiment is
successfully achieved.

10.0 RECOMMENDATIONS

1. Make sure the conductivity of the inlet and outlet stable before start the experiment.
2. Make sure there is no leakage at the equipment during the experiment.
3. The flow rate must be kept constant.
4. The valve must be fully open to ensure constant flow.
5. The conductivity value must be taken for three times.
6. Repeat the experiment to get an accurate result.
7. Start the experiment with correct general start up procedure to get a better result.

11.0 REFERENCES

20
(n.d.). Retrieved from Solution: http://www.solution.com.my/pdf/BP101(A4).pdf

Bioreactor. (n.d.). Retrieved from Metal : http://www.metal.ntua.gr/~pkousi/e-


learning/bioreactors/page_07.htmhttp://www.metal.ntua.gr/~pkousi/e-
learning/bioreactors/page_07.htm

(n.d.). Operating & Experiment Manual, Tubular Flow Reactor. UiTM.

Plug Flow Reactor. (n.d.). Retrieved from Umich:


http://www.umich.edu/~elements/5e/asyLearn/bits/pfrfinal/index.htm

Tubular Flow Reactor Residence Time. (n.d.). Retrieved from Umich:


http://www.umich.edu/~essen/html/byconcept/chapter13.pdf

12.0 APPENDICES

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Figure 1 : Tubular Flow Reactor

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