1.

ABSTRACT/SUMMARY
A tubular reactor is a vessel through which flow is continuous, usually at steady state,

and configures so that conversion of the chemicals and other dependent variables are
functions of position within the reactor rather than of time. The objectives of this experiment
are to examine the effect of pulse input and step change input in a tubular flow reactor .
Furthermore, the purpose is to construct a residence time distribution (RTD) function for the
tubular flow reactor. First of all, the general set up is run before the experiment begin. After
that, the flowrate 700mL/min is set up. After the conductivity for inlet and outlet collected
are reaching to three times constant value, the experiment is stopped. For the first experiment
which is pulse input, the conductivity for inlet and outlet after 5 minutes are 0.0mS/cm and
0.0mS/cm while the second experiment is 2.9mS/cm and 3.3 Ms/cm respectively. The outlet
conductivity, C(t) then is calculated and the value is...for the first experiment andfor
the second experiment. Then, the distribution of exit time, E(t) are able to determine. The
E(t) is calculated for each 30 seconds. For the first experiment, the sum of E(t) is while
the second experiment iswhich is the residence time distribution. The mean
residence time, tm for the first experiment is . minute and minute for second
experiment. The variance, 2 and the skewness, s3 are also then calculated. The value get for
2 is and for the s3 is ... in the first experiment while the value 2 in the second
experiment is. and s3 is Graphs for outlet conductivity, C(t) against time
and distribution of exit time, E(t) against time is plotted. The graphs 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).

2.0

INTRODUCTION

2.1 The Flow Concept of Tubular Reactor

In the tubular reactor, the reactants are continually consumed as they flow down the
length of the reactor. Flow in tubular reactor 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 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. 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. The nature of the tracer peak gives an indication of
the non-ideal that would be characteristic of the reactor.
For most chemical reactions, it is impossible for the reaction to proceed to 100%
completion. The rate of reaction decreases as the percent completion increases until the point
where the system reaches dynamic equilibrium (no net reaction, or change in chemical
species occurs). The equilibrium point for most systems is less than 100% complete. For this
reason a separation process, such as distillation, often follows a chemical reactor in order to
separate any remaining reagents or by products from the desired product. These reagents may
sometimes be reused at the beginning of the process, such as in the Haber process.

2.2

The Application of Tubular Flow Reactor

Tubular flow reactors are usually used for this application which are large scale
reactions,fast reactions, homogeneous or heterogeneous reactions, continuous production and
high temperature reactions.

Residence Time Distribution (RTD) analysis is a very efficient diagnosis tool that can be
used to inspect the malfunction of chemical reactors. It can also be very useful in modelling
reactor behaviour and in the estimation of effluent properties. This technique is, thus, also
extremely important in teaching reaction engineering, in particular when the non-ideal
reactors become the issue. The work involves determining RTDs, both by impulse and step
tracer injection techniques, and applying them to the modelling of the reactor flow and to the
estimation of the behaviour 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).
The concept of using a tracer species to measure the mixing characteristics is not
limited to chemical reactors. In the area of pharmacokinetics, the time course of renal
excretion of species originating from intravenous injections in many ways resembles the
input of a pulse of tracer into a chemical reactor. Normally, a radioactive labelled ( 2H, 14C, 32P,
etc.) version of a drug is used to follow the pharmacokinetics of the drug in animals and
human.
Another important field of RTD applications lies in the prediction of the real reactor
performance, since the known project equations for ideal reactor are no longer valid. Now the
concepts of macro and micro mixing are fundamental. For each macro mixing level,
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.

3.0

OBJECTIVES/AIMS

For the experiment one, the purpose of the experiment is to examine the effect of a pulse
input in a tubular flow reactor and to construct a residence time distribution (RTD) function
for the tubular flow reactor. In experiment two, the objective is to examine the effect of a step
change input in a tubular flow reactor and to construct a residence time distribution (RTD)
function for the tubular flow reactor.

4.0

THEORY
In a tubular flow 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. It is often not
necessary to know details of the entire flow fluid but rather only how long fluid elements
reside in the reactor (i.e. the distribution of residence times). This information can be used as
a diagnostic tool to ascertain flow characteristics of a particular reactor. 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.

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 age of a fluid element is defined as the time it has resided within the reactor. The
concept of a fluid element being a small volume relative to the size of the reactor yet
sufficiently large to exhibit continuous properties such as density and concentration was first
put forth by Danckwerts in 1953.
In order to analyze the residence time distribution of the fluid in a reactor the following
relationships have been developed. Fluid elements may require differing lengths of time to
travel through the reactor. The distribution of the exit times, defined as the E(t) curve, is the
RTD of the fluid. The outlet conductivity of a tracer species C(t) can be used to define E(t).
That is:
E (t)

Ctout (t )

C tout ( t ) dt
0

Based on the data collected, a graph of conductivity versus time could be draw to obtain the
C(t) curve and data of the integral C(t) could be calculate.

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

Figure 4.1: Theory of graph with its formula area under the graph

Other things that are needs to be determined in this experiment are:

Mean Residence Time

t E(t).dt

= tiEi(t)

Second moment Variance, 2 =

(t - tm)2 E(t).dt = (t - tm)2 E(t)

Third Moment Skewness, s3 =

(t - tm)3 E(t).dt = (t - tm)3 E(t)

If the RTD function, E(t), is very broad, however, it may be difficult to inject an amount
of tracer that is sufficiently large so as to keep the outlet concentration sufficiently high to be
measured accurately.

Figure 4.2: Example of graph when distribution exit time is very abroad

5.0

APPARATUS AND MATERIAL

Apparatus and
material
SOLTEQ Tubular
Flow Reactor
Clock watch

1. 0.1M of Sodium
Hydroxide
2. 0.1M of Sodium
Acetate
3. 0.1M of
Deionised water

Purpose
The main instrument to read the conductivity,
open and close the valve and the pump and etc.
To record every 30 second for reading of
conductivity until it constant about three times
and then stop.
The materials used to prepare the standard
solution before the experiment run.

Figure 5.1 : Soltec Tubular Flow Reactor instrument

6.0

EXPERIMENTAL PROCEDURES
6.1

General Start-up Procedure

For the general start-up procedure, initially all the valves are closed except valve 7.
Then, 20Liters of salt solution is prepared. Next, the feed tank B2 is filled with the sodium
chloride solution. After that, the power button is turn on. The water De-ionizer is connected
to the laboratory water supply. Valve V3 is opened and the feed tank B1 is allowed to feed
with the water. Valve V3 is closed as the water level reached the tank mark.
Valve V2 and V10 then is opened and pump P1 is switched on. From observing the
flow meter F1-01 value, The P1 pump is adjusted by controlling the flow controller to obtain
a flow rate of approximately 700mL/min. Next, valve V6 and V12 are opened and pump 2
P2 is switched on. From observing the flow meter F1-02 value, The P2 pump is adjusted by

controlling the flow controller to obtain a flow rate of approximately 700mL/min. Then the
valve V12 is closed and pump P2 is turn off. The experiment can now be carried out.

6.2
Experiment One : Pulse input in a Tubular Flow
Reactor.
For the experiment one, the valve V9 initailly is opened and pump P1 is switched on.
The P1 pump is adjusted by controlling the flow controller to obtain a flow rate of
approximately 700mL/min of de-ionized water into the reactor R1. Then, the de-ionized
water is allowed to continue flowing through the reactor until the inlet (Q1-01) and outlet
(Q1-02) conductivity values are stable at low levels. Both conductivity values is recorded.
After that, the valve V9 is closed and pump P1 is switched off. Valve V11 is opened
and pump P2 is switched on. The timer is simultaneously started. Pump P2 flow controller is
adjusted to give a constant flow rate of salt solution into the reactor R1 at 700mL/min at F102. The salt solution is allowed to flow for 1minute, the timer is reset and restarted. This will
start the time at the average pulse input. Valve V11 is closed and pump P2 is switched off.
Valve V9 is quickly opened and pump P1 is switch on.

By adjusting pump P1 flow

controller, the de-ionized water flow rate is always maintained at 700mL/min. The inlet (Q101) and outlet (Q1-02) conductivity values are recorded at regular interval of 30 seconds.
The conductivity values are recorded until all readings are almost constant and approach
stable low level values.

6.3 Experiment Two: Step Change Input in a Tubular Flow

Reactor
For the second experiment on step change input, the general start-up procedure was
performed again as in 6.1. Valve V9 was opened and pump P1 was switched on. Pump P1
flow controller was adjusted to give a constant flow rate of deionized water into the reactor
R1 at approximately 700 mL/min at FI-01. The deionized water was allowed to flow through
the reactor until the inlet (QI-01) and outlet (QI-02) conductivity values are stable at low
levels. Both conductivity values were recorded. Then, valve V9 was closed and pump P1
was switched off. Valve V11 was opened and pump P2 was switched on. The timer was set
simultaneously. Both the inlet (QI-01) and outlet (QI-02) conductivity values were recorded

at regular intervals of 30 seconds.

The conductivity values were taken down until all

readings are almost constant.

6.4

General Shut-Down Procedure

For the general shut- down procedure, both pumps P1 and P2 were switched off. After
that, the valves V2 and V6 were closed. The heaters were switched off. Cooling water was
kept to circulate through the reactor while the stirrer motor is switched on to allow the water
jacket to cool down to room temperature. Finally, the power for the control panel was
switched off.

7.0

RESULTS

7.1 Experiment One: Pulse input in Tubular Flow Reactor

Flow rate : 700mL/min
Input type : Pulse input

Time (min)
0.0
0.5
1.0
1.5
2.0
2.5

Conductivity (mS/cm)
Inlet
Outlet
0.0
0.1
0.3
2.2
0.1
2.3
0.1
2.4
0.0
2.4
0.0
0.8

3.0
3.5
4.0
4.5
5.0

0.0
0.0
0.0
0.0
0.0

0.3
0.1
0.0
0.0
0.0

Table 7.1 : Table conductivity of pulse input

Experiment Two: Step Change Input in a Turbular Flow Reactor

Flow rate

= 700 mL/min

Input type : Step change

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

Conductivity (mS/cm)
Inlet
outlet
0.0
0.0
2.7
0.0
2.8
0.0
2.8
0.0
2.8
0.0
2.7
1.3
2.7
1.6
2.6
1.6
2.6
1.6
2.8
2.5
2.9
2.6
2.9
2.7
2.9
2.9
2.9
3.1
2.9
3.3
2.9
3.3
2.9
3.3