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4.

0 THEORY

A tubular flow reactor (TFR) is a tube or pipe through which reactants flow and are converted
into product. Several of TFR arrange in parallel or series, both horizontal and vertical
orientations are common. The TFR reactor may have a varying diameter along the flow path and
has continuous gradient of concentration in the direction flow [1]. In these reactors, conditions of
temperature, pressure, and gas fluid residence time can be carefully controlled [2]. Chemical
reactions take place in a stream of gas that carries reactants from the inlet to the outlet. Presence
of catalyst in tubes uniform loading is ensured by using special equipment that charges same
amount of catalyst to each tube at a definite rate.

Tubular flow reactors resemble batch reactors in providing initially high driving forces,
which decrease as the reaction progress down the tubes. In TFR, the flow can be laminar as with
viscous fluids in small-diameter tubes and greatly deviate from ideal plug-flow behavior, or
turbulent, as with gases [1]. Laminar flow are more prefer in tubular flow as the mixing and heat
transfer are improved. For small scale reaction such as in small laboratory and in pilot plant
reactor, establishing turbulent flow can result in inconveniently long reactors or may require
unacceptably high feed rates . The tubular flow 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 reactant to product.

The residence-time distribution (RTD) of a reactor is a characteristic of the mixing that


occurs in the chemical reactor. The RTD which is synonymic with the exit age distribution
density function E(t) is a probability distribution function that describes the amount of time a
fluid element spends inside a reactor [3]. Two method used to determine RTD are used methods
of injection are pulse input and step input. In a pulse input, an amount of tracer N 0 is suddenly
injected in one shot into the feed stream entering the reactor in as short a time as possible. The
outlet concentration is then measured as a function of time [4].

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 effluent stream as a function of time. Then E(t) representing the probability for a tracer
element to have a residence time between the time interval (t, t+dt) and is defined as follows [3]:
Ci(t ) ∞

Ei (t) = , such that ∫ Ei (t ) dt =1
∫ Ci ( t ) dt ' 0
0

Figure 1: RTD measurement.

Other things can be determined:

Mean Residence Time ∞

= ∫ t E (t ) . dt = Σ tiEi (t)
0

Second moment Variance, σ 2 ∞


= ∫ (t−t m)2 E(t). dt = Σ (t−t m)2 E(t)
0

Third Moment Skewness, s3 ∞


=∫ ¿ ¿) 3 E(t). dt = Σ (t−t m)3 E(t)
0
5.0 APPARATUS AND MATERIALS

Figure 2: SOLTEQ Tubular Flow Reactor (BP101-B)

Apparatus:

a) SOLTEQ Tubular Flow Reactor (BP101-B)


b) Stopwatch

Materials:

a) 0.025M Sodium Chloride


b) 0.025M Deionized water
6.0 PROCEDURE

6.1 General Start-Up Procedure:

a) All valves are ensured closed except for valve V7.


b) The following solution were prepared: Tank B1: Deionized water and Tank B2: 0.05M
sodium chloride solution (NACl).
c) The power for control panel was turned on.
d) Water jacket B4 and pre-heater B5 was filled with clean water. Valves V13 and V8 were
opened. Pump P3 was switched on to circulate the water through pre-heater B5.
e) Stirrer motor M1 was switched on the speed was set to about 200 rpm.
f) Valves V2 and V10 were opened. Pump P1 was switched on. P1 was adjusted to flow rate of
700mL/min at flow meter FI-01. Valve V10 was closed and pump P1 was switched off.
g) Valves V6 and V12 were opened. Pump P2 was switched on and was adjusted to flow rate of
100 mol /min at flow meter FI-02. Valve V12 was closed and pump P2 was switched off.
h) The unit was ready for experiment.

6.2 Experimental Procedure:

6.2.1 Experiment 1: Pulse Input in a Tubular Flow Reactor

a) General stat-up procedure was performed as in 6.1


b) Valve V9 was opened and pump P1 was switched on.
c) Pump P1 flow controller was adjusted to give a constant flow rate of deionized water into
reactor R1 at approximately 700 mL/min at FI-01.
d) The deionized water continued to flow through the reactor until the inlet (QI-01) and outlet
(QI-02) conductivity values were stable at low levels. Both conductivity values were
recorded.
e) Valve V9 was closed and Pump P1 was switched off.
f) Valve V11 was opened and pump P2 was switched on. The timer was set simultaneously.
g) Pump P2 was flow controller was adjusted to give a constant flow rate of salt solution into
the reactor R1 at 700 mL/min at FI-02.
h) The salt solution was allowed to flow for 1 minutes and the timer was reset and restarted.
i) Valve V11 was closed and pump P2 was switched off. Valve V9 was quickly opened and
pump P1 was switched on.
j) The deionized water flow rate was made sure always maintained at 700 mL/min by adjusting
P1 flow controller.
k) Both the inlet (QI-01) and outlet (QI-02) conductivity values were recorded at regular
intervals of 30 seconds.
l) Conductivity values were recorded until all readings were constant and approach stable low
level values.

6.2.2 Experiment 2: Step Change Input in a Tubular Flow Reactor

a) General stat-up procedure was performed as in 6.1


b) Valve V9 was opened and Pump P1 was switched on.
c) Pump P1 flow controller was adjusted to give constant flow rate of deionized water into the
reactor R1 at approximately 700 mL/min at FI-01.
d) 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.
Valve V9 was closed and pump P1 was switched off.
e) Valve V11 was opened and pump P2 was switched on. The timer was set simultaneously.
f) Both the inlet (QI-01) and outlet (QI-02) conductivity values were recorded at regular
intervals of 30 seconds.
g) The conductivity values were taken down until all readings are almost constant.

6.3 General Shut-Down Procedure:

a) Both pumps P1 and P2 were switched off. Valves V2 and V6 were closed.
b) The heaters were switched off.
c) Cooling water was kept to circulate through the reactor while the stirrer motor was switched
on to allow the water jacket to cool down to room temperature.
d) The power for the control panel was switched off.
11.0 RECOMMENDATIONS

There are several factor that can be fix and take into consideration for the experiment run
smoothly and get accurate result. First recommendation is ensure all the equipment is properly
calibrated, functioning, clean and ready to use. Equipment that are malfunction can affected the
result as it influence measurement of mass and volume. Secondly, student must follow the
procedure given carefully. Open and close the valve correctly according to the procedure,
perform general start up and general shut down procedure to run the experiment smoothly. Start
the experiment after 1 minutes to stable the conductivity for inlet and outlet. Next, make sure
flow rate remain constant throughout the experiment. Next, check the storage tank all the time
during experiment to make sure there are enough solution for experiment. Lastly, take each
measurement multiple times and take an average reading in order to get more accurate and
precise results.
References:

[1] Nasir, H. (2015). Types of Chemical reactors. Production and Operation Engineer, pp 81.

Retrieved from: http://appliedchem.unideb.hu/Unit%20Operation

%203/Reactors/reactortypes.pdf

[2] https://link.springer.com/chapter/10.1007/978-1-4471-5307-8_9

[3]https://www.researchgate.net/publication/308797261_RESIDENCE_TIME_DISTRIBUTION

_RTD_IN_OPERATING_PLANT_A_REVIEW

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

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