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Abstract

This experiment has been conducted on 30th March 2015 at Pilot Plant Laboratory, UiTM
Shah Alam. The experiment is conducted to achieve the objective that has been considered
which is to examine the effect of pulse input and step change input in tubular flow reactor and
to construct the residence time distribution function by using tubular machine. Based on the
experiment, two experiment were conducted which is pulse input experiment and step change
input experiment. In the pulse input experiment, the flow rate was set up at 700 m3 s-1 and let
it for one minute before reading taken every 30 seconds until the conductivity reading is 0.0.
in the other hand, the step change input experiment, the conductivity were observe every 30
seconds until the reading at Q2 is constant for 3 times

Introduction

The experiment that was carried out involved the tubular flow reactor. Tubular reactor is a
vessel through which flow is continous, usually at steady state, and configured so that
conversion of the chemicals and other dependent variables are functions of position within
the reactor rather then of time. In the ideal tubular reactor, the fluid flow as if the were solid
plugs or pistons, and reaction time is the same for all flowing material at any given tube cross
section. Tubular reactors resembles batch reactors in providing initially driving forces, which
diminish as the reaction progress down the tubes.
Flow in tubular reactors can be laminar as with viscous fluids in small diameter tubes, and
greatly deviate from ideal plug flow reactor behavior, 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 igh
feed rates.

OBJECTIVES
Experiment 1
-

To examine the effect of a pulse input in a tubular flow reactor.


To construct a residence time distribution (RTD) function for the tubular flow reactor.

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

THEORY
2

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 backmixing of products and reactants.
Flow in tubular reactors can be laminar, as with viscous fluids in small-diameter
tubes, and greatly deviate from ideal plug-flow behavior, 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)
The procedure would be to carried out experiments with tubular reactor at varying feed rates,
measuring the extent of reaction of the stream leaving the reactor. One possible method might
to add inert gas to the acetaldehyde vapour in such quantity that the change in density
between entry and exit of the reactor could be neglected. In that case, the batch reactor time
and the residence-time would both be equal to the space-time.

Using the result of experiment, apply equation below to determine n and k ( wil bw
known from the stoichiometry).

Mf=various values of feed rate


= space-time
from experiment, it should be able to draw a curve of against xout, the slope of which
according to the first equation, should be

Taking the logarithm of both sides of equation, we can obtain

So, n and k can be obtain from the intercept and slope of the appropriate log-log plot.
This approach that the experiments 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

Where Tin is the temperature of the feed into the reactor


Therefore, when the effect of wall heat transfer and of velocity gradient operate
simultaneously they might, under rather special circumstance, give rise to a more complex
kind of temperature profile. However, the most commonly observed 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.

PROCEDURE
Experiment 1: Pulse Input in a Tubular Flow Reactor
1
2
3

The general start-up procedures as in Section 4.1 is performed.


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


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

5
6
7

values are recorded.


Valve V9 is closed and pump P1 is switch off.
Valve V11 is opened and Pump P2 is switch on. The timer is started simultaneously.
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.


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.


Valve V11 is closed and pump P2 is switch off. Then, open valve V9 quickly and

pump P1 is switch on.


10 Make sure that the de-ionized water flow rate is always maintained at 700 ml/min by
adjusting P1 flow controller.
11 Both the inlet (Ql-01) and outlet (Ql-02) conductivity a value at regular intervals of 30
seconds is start recorded.
12 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 The general start-up procedures as in Section 4.1 is performed.
2 Valve V9 is opened and pump P1 is switch on.
3 Pump P1 flow controller is adjusted to give a constant flow rate of de-ionized water
4

into the reactor R1 at approximately 700 ml/min at Fl-01.


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

5
6
7

values are recorded.


Valve V9 is closed and pump P1 is switch off.
Valve V11 is opened and Pump P2 is switch on. The timer is started simultaneously.
Both the inlet (Ql-01) and outlet (Ql-02) conductivity a value at regular intervals of 30

seconds is start recorded.


The conductivity values is continue recording until all readings are almost constant.

APPARATUS AND MATERIALS

Tubular flow reactor


Deionized water
Sodium hydroxide
Ethyl acetate

RESULT
Experiment 1: Pulse Input in a Turbular Flow Reactor

Flow rate

= 700 mL/min

Input type

= Pulse input

Time

Conductivity (mS/cm)

C(t)

E(t)

tm

s3

Inlet

Cit

Ci(t)

t*E(t)/

(t - tm) 2 *

(t - tm) 3 *

E(t)/

E(t)/

(min)
Outlet

Ci(t)

C i t

C i t

C i t

0.0

0.0

0.0

0.00

0.0000

0.0000

0.0000

0.0000

0.5

4.1

0.0

0.00

0.0000

0.0000

0.0000

0.0000

1.0

4.3

0.0

0.00

0.0000

0.0000

0.0000

0.0000

1.5

4.4

0.3

0.15

0.0117

0.0014

0.0021

0.0031

2.0

4.5

2.4

1.20

0.0938

0.0015

0.0293

0.0584

2.5

4.5

2.6

1.30

0.1016

0.0198

0.0488

0.1211

3.0

4.5

2.8

1.40

0.1094

0.0256

0.0756

0.2249

3.5

4.5

2.9

1.45

0.1133

0.0310

0.1065

0.3695

4.0

4.5

3.0

1.50

0.1172

0.0366

0.1438

0.5701

4.5

4.5

3.2

1.60

0.1250

0.0439

0.1939

0.8641

5.0

0.3

3.4

1.70

0.1328

0.0519

0.2540

1.2569

5.5

0.1

3.5

1.75

0.1367

0.0587

0.3162

1.7205

6.0

0.0

1.4

0.70

0.0547

0.0256

0.1525

0.9113

6.5

0.0

0.1

0.05

0.0039

0.0254

0.0128

0.0827

7.0

0.0

0.0

0.00

0.0000

0.0000

0.0000

0.0000

12.80

1.0001

0.3214

1.3355

6.1826

SUMMATION

Table 1

outlet conductivity vs time


4
3.5
3
2.5
outlet conductivity

2
1.5
1
0.5
0
0

time

Graph of outlet conductivity against time

E(t) vs time
0.16
0.14
0.12
E
(
t
)

0.1
0.08
0.06
0.04
0.02
0
0

time

Experiment 2: Step Change Input in a Turbular Flow Reactor

Flow rate

= 700 mL/min

Input type

= Step Change

Time

Conductivity (mS/cm)

C(t)

E(t)

tm

s3

Inlet

Cit

Ci(t)

t*E(t)/

(t tm) 2 *

(t tm) 3 *

E(t)/

E(t)/

(min)
Outlet

Ci(t)

C i t

C i t

C i t

0.0

0.0

0.0

0.00

0.0000

0.0000

0.0000

0.0000

0.5

4.1

0.0

0.00

0.0000

0.0000

0.0000

0.0000

1.0

4.3

0.0

0.00

0.0000

0.0000

0.0000

0.0000

1.5

4.4

0.3

0.15

0.0094

0.0009

0.0013

0.0020

2.0

4.5

2.4

1.20

0.0752

0.0094

0.0187

0.0037

2.5

4.5

2.6

1.30

0.0815

0.0128

0.0316

0.0121

3.0

4.5

2.8

1.40

0.0878

0.0165

0.0490

0.1462

3.5

4.5

2.8

1.40

0.0878

0.0193

0.0667

0.2321

4.0

4.5

2.8

1.40

0.0878

0.0220

0.0871

0.3465

4.5

4.5

2.9

1.45

0.0909

0.0256

0.1141

0.5105

5.0

4.5

3.0

1.50

0.0940

0.0295

0.1456

0.7237

5.5

4.5

3.0

1.50

0.0940

0.0324

0.1762

0.9633

6.0

4.5

3.0

1.50

0.0940

0.0354

0.2097

1.2506

6.5

4.5

3.1

1.55

0.0972

0.0396

0.2543

1.6432

7.0

4.5

3.2

1.60

0.1003

0.0440

0.3043

2.1165

15.95

0.9999

0.2874

1.4586

8.0593

SUMMATION

Table 2

10

outlet conductivity vs time


3.5
3
2.5
2
1.5
1
0.5
0
0

E(t) vs time
0.12
0.1
0.08
0.06
0.04
0.02
0
0

SAMPLE CALCULATIONS

11

C ( t ) dt
0

Area = (

= Area under the graph

t1

t2

f ( t 1 ) + f (t 2)
2

For time (1.0-1.5) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

= (1.5 1.0)

0.2+1.8
2

= 0.5 g .min

= (2.0 1.5)

1.8+2.1
2

= 0.975 g .min

= (2.5 2.0)

2.1+1.1
2

= 0.8 g .min

m3

= (3.0 2.5)

1.1+0.1
2

= 0.3 g .min

m3

m3

For time (1.5 2.0) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

m3
For time (2.0 2.5) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

For time (2.5 3.0) minutes

Area = ( t 2 t 1

E (t 1+t 2)
2

So the total area or

C ( t ) dt
0

= ( 0.5+ 0.975 + 0.8 + 0.3) = 2.575

g.min/m3

12

E (t)=

C (t)

C ( t ) dt
0

For t = 0, C(t) = 0.0


E(t)=0/2.575=0
For t = 0.5, C(t) = 0.0
E(t)=0.0/2.575=0

For t = 1.0, C(t) = 0.2


E(t)=0.2/2.575=0.07767
For t = 1.5, C(t) = 1.8
E(t)=1.8/2.575=0.69903

For t = 2.0, C(t) = 2.1


E(t)=2.1/2.575=0.81553
For t = 2.5, C(t) = 1.1
E(t)=1.1/2.575=0.42718

For t = 3.0, C(t) = 0.1


E(t)=0.1/2.575=0.038833
For t = 3.5, C(t) = 0.0
E(t)=0.0/2.575=0

For t = 4.0, C(t) = 0.0

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

So based on the table, Area is 20.05m2


Example of calculation at t=0.00min
t m=

t E( t)
Area

t m=

2.50 0.16209
20.05

t m=0.02021

2=

2
( tt m ) E(t)

Area

( 2.500.02021 )2 0.16209
=
20.05
2

2=0.049713

s=

s 3=

3
( t t m ) E(t )

Area

( 2.500.02021 )3 0.16209
20.05

s 3=0.12328

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DISCUSSION

Firstly, the objective that need to be achieve for this tubular reactor experiment is to examine
the effect of a pulse input and step change in a tubular reactor and also to construct the
residence time distribution (RTD) function for the tubular flow reactor at the end of the
experiment. The experiment was run at the 700 mL/min of flowrate. While the experiment is
running, the conductivity for the inlet and outlet of the solution had been recorded at the
period of time where until the conductivity of the solution is constant.
For a tubular reactor, the flow that throught the vessel is continuous, usually at the
steady state and also configured thus the conversion of the chemicals and other dependent
variables are functions of position within the reactor rather than of time.
For this experiment, the effects of flow for two types of reaction which are in pulse
input and step change is examined. The flowrate of solution is kept constant at 700 ml/min.
For this types of experiments, the graph of outlet conductivity versus times had been plotted.
Based on graph of pulse input, the outlet conductivity that had been plotted is 2.1 mS/cm at
time of 2 minutes which are the highest value. After that, the conductivity is decrease within
the time and comes to be constant at the time of 3.5 minutes. From the result, it showed that it
result was not differ from the theory that recorded that the conductivity is reaching zero at
time of 4 minutes. Thus, the experiment 1 is succeed.
In addition, for the graph of step change the outlet conductivity is increase within the
time by started at time of 2.0 minutes which it inlet conductivity is 2.8 mS/min and then
undergoes some increament until at minutes 4.0 which the outlet conductivity is 1.6 mS/min.
There are differences between both of the graph where the outlet conductivity for step change
is increase smoothly compare to pulse input where the outlet conductivity is increase at the
some period of times and then it become decrease into the constant value.
Next experiment, to construct the residence time distribution (RTD) function for the
tubular flow reactor for pulse input and also step change. The residence time distribution is
plotted based on exit time (E(t)) versus time from the data that had been recorded in the table.
From the graph plotted, it almost same with the graph that are stated at the theory. From the
15

graph, it can be concluded tha the residence time distribution is depends on the
outlet conductivity.

CONCLUSION

The conductivity for inlet and outlet after 3 minutes for pulse input are 0.00 mS/min
and 0.1 mS/min while for the step change is 2.7 mS/min and 1.6 mS/min respectively. The
outlet conductivity, C(t) that had been calculated for pulse input is 12.8 and for step change is
15.95. The distribution of exit time, E(t) is calculated for each 30 second until 4 minutes
interval. The sum of E (t) for pulse input and step change are 1.0001 and 0.999 respectively.
The mean residence time, tm for pulse input is 0.3214 minutes and step change is 0.2874
minutes.
The variance, 2 and skewness, s3 are also calculated. For pulse input are 1.1355 and
-6.1826 while for step change are 0.4586and 8.0593. graph for outlet conductivity, C (t)
against time and distribution of exit time, E (t) against time are plotted. The graph plotted
almost the same as the theory which stated that exit time, E (t) is depends on the value of C
(t).

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RECOMMENDATIONS

Each experiment we must do the start-up and shut-down experiment first in order to
make sure there are no left over in the chamber.
Open and close the valve carefully according to the procedure given.
The experiment should be conducted at the stable and unshaken place.
Make sure there are no leakages at the equipment.

II
III
IV

REFERENCES

(K. G. Denbigh, Chemical Reactor Theory: An Introduction, 41-45)



(Artin
hatzikioseyian,

Emmanouela

Remoundaki,http://www.metal.ntua.gr/~pkousi/e-learning/bioreactors/page_07.htm
http://www.neduet.edu.pk/Chemical/PDF/CHEMICAL%20REACTION
%20ENGINEERING%20LAB.pdf

Turbular

Reactor.

(n.d.).

Retrieved

April

2013,

from

Scrib:

http://www.scribd.com/doc/95675475/Turbular-Reactor

Wikipedia. (n.d.). Retrieved April 2013, from Plug Flow Reactor Model:
http://en.wikipedia.org/wiki/Plug_flow_reactor_model

http://www.metal.ntua.gr/~pkousi/elearning/bioreactors/page_07.htm

http://en.wikipedia.org/wiki/Residence_time_distribution

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APPENDICES

18

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