UNIVERSITI TEKNOLOGI MARA

FAKULTY OF CHEMICAL ENGINEERING

CHEMICAL ENGINEERING LABORATORY III (CHE574)
NAME
MATRIX NO
GROUP
EXPERIMENT
DATE
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SUBMIT TO
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MUHAMMAD AMIRUL BIN HASHIM

2014207844
EH2204A (G4)
LAB 5 : CSTR 40L
8 MARCH 2016
EH220
PUAN NURHASHIMAH BT ALIAS
Title
Allocated Marks
(%)
Abstract
5
Introduction
5
Objectives
5
Theory
5
Procedures/Methodology
10
Apparatus
5
Results
10
Calculation
10
Discussion
20
Conclusion
10
Recommendations
5
References
5
Appendices
5
TOTAL
100

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Rechecked by:

Date:

Date:

ABSTRACT

Marks

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, t m 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 s 3 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, t m for this experiment are 0.9912 minute and

0.6275 minutes respectively. The variance, 2 and the skewness, s 3 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 s 3 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

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. 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. 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.
There are tubular flow reactors applications which are:

Large-scale reactions

Fast reactions

Homogeneous or heterogeneous reactions

Continuous production

High-temperature reactions
In an ideal plug flow reactor, 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. The degree of dispersion that occurs in a real reactor can be assessed by
following the concentration of tracer versus time at the exit. This procedure is called the
stimulus-response technique.

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 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.

The residence time distribution of a real reactor deviated 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
curve arrives earlier than the expected time

it indicates that there is stagnant

fluid within the vessel. If the residence time distribution curve shows more than one
main peak it may indicate channeling, parallel paths to the exit, or strong internal
circulation.

OBJECTIVES
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

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 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.
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.

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. 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 into the reactor R1 at approximately 700 ml/min at Fl-01.
4. Let the de-ionized water to continue flowing through the reactor until the inlet (Ql01) and outlet (Ql-02) conductivity values are stable at low levels. Both
conductivities values are recorded.
5. Valve V9 is closed and pump P1 is switch off.
6. Valve V11 is opened and Pump P2 is switch on. The timer is started
simultaneously.
7. 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.
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. 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 into the reactor R1 at approximately 700 ml/min at Fl-01.
4. Let the de-ionized water to continue flowing through the reactor until the inlet (Ql01) and outlet (Ql-02) conductivity values are stable at low levels. Both
conductivities values are recorded.
5. Valve V9 is closed and pump P1 is switch off.
6. Valve V11 is opened and Pump P2 is switch on. The timer is started
simultaneously.
7. Both the inlet (Ql-01) and outlet (Ql-02) conductivity a value at regular intervals of
30 seconds is start recorded.
8. The conductivity values is continue recording until all readings are almost
constant.

A P P AR ATU S AN D M ATE R I AL S

Tubular flow reactor

Deionized

water
S o d i u m h yd r o x i d e
E t h yl a c e t a t e

RESULTS

Time (min)

Conductivity (mS/cm)
Inlet
Outlet
0.0
0.0
0.0
0.5
0.0
1.6
1.0
0.0
2.2
1.5
0.0
2.9
2.0
0.0
2.3
2.5
0.0
0.8
3.0
0.0
0.3
3.5
0.0
0.1
4.0
0.0
0.0
Experiment 1: Pulse input in Tubular Flow Reactor
Flow rate : 700mL/min
Input type : Pulse input

Outlet Conductivity versus Time

3.5
3
2.5
2
OUTLET CONDUCTIVITY (mS/cm)

1.5
1
0.5
0
0

0.5

1.5

2.5

TIME (min)

3.5