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CBB2074

REACTION ENGINEERING




EXPERIMENT 4: RTD IN PACKED BED REACTOR

GROUP: B9





MOHD SHAZNI BIN AB LATIF 13596
SRINIVASAN A/L SIVARAMAN 13396
MUHAMMAD MUKHLIS BIN AHMAD KAMAL 13727
NUR AINNA EMIRA BT EZANI 13897
EBTEHAL EISA RAGHEB 13456

DATE OF EXPERIMENT: 17
TH
JULY 2012

1

TABLE OF CONTENTS

Contents Page
_______________________________________________________________________

1.0 ABSTRACT . . . . . . . 2
2.0 OBJECTIVE . . . . . . . 3
3.0 INTRODUCTION AND THEORY . . . . . 3
4.0 METHODOLOGY . . . . . . . 6
4.1 Experiment A: The effect of step change input . . 6
4.2 Experiment B: The effect of pulse input . . . 7
5.0 RESULTS AND CALCULATIONS . . . . . 9
5.1 Results . . . . . . . 9
5.2 Calculations . . . . . . . 15
5.3 Sample Calculations . . . . . . 15
6.0 DISCUSSION AND ERROR ANALYSIS . . . . 16
6.1 Discussion . . . . . . . 16
6.2 Error Analysis . . . . . . 19
7.0 CONCLUSION . . . . . . . 21
8.0 REFERENCES . . . . . . . 21








2

1.0 ABSTRACT
In the majority of industrial chemical processes, a reactor is the key item of
equipment in which raw materials undergo a chemical change to form desired products. The
design and operation of chemical reactors is thus crucial to the whole success of the industrial
operation. Reactors can take a widely varying form, depending on the nature of the feed
materials and the products. Understanding non-steady behaviour of process equipment is
necessary for the design and operation of automatic control systems. Continuous flow
reactors are almost always operated at steady state. Examples of continuous reactors are
continuous stirred tank reactor (CSTR), tubular reactor or plug flow reactor (PFR), packed
bed reactor (PBR), and etc.
One particular type of process equipment is the tubular reactor. In this reactor, it is
important to determine the system response to a change in concentration. This response of
concentration versus time is an indication of the ideality of the system. The RTD in Packed
Bed has been designed for students experiment on residence time distribution (RTD) in a
tubular reactor. The unit consists of mainly a vertical glass column packed with glass Raschig
rings. Sump tanks and circulation pumps are provided as well as instruments to measure
concentration of the tracer passing through the column. Students may select either step
change input or pulse input to the reactor and then will continuously monitor the responses in
the reactor at suitable intervals.







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2.0 OBJECTIVE
1. To study the dynamic behavior of packed bed reactor due to step change and pulse input
for co-current and counter current mode of liquid and gas feed.
2. To determine the effect of liquid (L) and gas (G) feed rate on the mean residence time and
degree (intensity) of liquid-phase axial dispersion.


3.0 INTRODUCTION AND THEORY
Packed bed reactor is a tubular reactor packed with solid catalyst particles. It is most
often used to catalyze gas reactions. The reaction rate is based on the amount of the solid
catalyst rather than the volume of the reactor. Packed bed reactors have high conversion per
unit mass of catalyst and the operating cost is low. However, packed bed reactors have poor
temperature control. Channelling may occur during the operation. The fluid, flows past the
catalyst pellets, on which the reaction takes place. Due to the heat of reaction, the temperature
can vary and in the case of an exothermic reaction, the temperature increases. The energy is
removed at the wall. Energy released near the wall is easily removed, but energy released in
the centre of the cylinder must get their way to the wall, using essentially two pathways. One
pathway is by heat conduction through the fluid and solid, and another is due to mixing, as
the flow around adjacent pellets combines downstream. This mechanism is called dispersion.
The rate of reaction depends on temperature. If the temperature rise is very small, then
the temperature is the same at different radial positions in the bed. If no mass is removed at
the wall, then there is no mechanism to create concentration variations in the radial direction,
provided the concentration is uniform upstream. In that case, a radial dispersion model is not
needed. If the temperature rise is large, however, then the temperature will be different at the
centre and wall of the cylinder, highest at the centre for exothermic reactors. In that case, the
rate of reaction will also vary in the radial direction, and a radial dispersion model is needed.
The model described here is a two phase model that is derived by averaging the concentration
and temperature in a small region, over both the fluid and solid.

4

W
F
A0
F
A
The mole balance for packed bed reactors is as follows:
'
A
A
r
dW
dF
=
}
=
'
A
A
r
dF
W
Residence Time Distribution is used to characterize existing reactors and predict exit
conversions and concentrations when reaction occurs in these reactors. Inject a tracer and the
concentration in the exit is measured, C
T
(t).


From the exit tracer concentration, we can determine:

E(t)dt = Fraction of molecules exiting the reactor that have spent a time between (t) and
(t + dt) in the reactor.
5


Mean Residence Time, t
m















6

4.0 METHODOLOGY
4.1 Experiment A: The effect of step change input
In this experiment a step change input would be introduced and the progression of the tracer
will be monitored via the conductivity measurements.
a) Counter-current Mode
The general start-up procedure is performed.
1. The valves is set appropriately for counter-current mode:
2. Valves V3, V5 and V10 remain closed.
3. Valve V1 is opened and pump P1 is turned on. The column is filled with de-ionized water
to packing height.
4. Valve V1 is adjusted to obtain a liquid flow rate of 500 ml/min.
5. Valve V6 is opened. Valve V8 is opened to obtain a gas flow rate of 1.0 L min-1.
6. The conductivity reading of CT1 is obtained and let it stabilizes at low value.
7. Dosing pump P2 is switched on. Valve V14 is opened and bleed off any air trapped in the
tubing.
8. Valve V14 is closed. Valve V9 is closed and start timer simultaneously. The conductivity
reading CT1 is recorded at 1 min interval.
9. Recording is continued until conductivity reading is constant.
10. The experiment is repeated with gas flow rate of 2.0 L min-1. The system is ensured that it
is flushed with de-ionized water until no traces of salt is detected.
11. The experiment is stopped and all the liquid from the system are drained out.

b) Co-current Mode
The general start-up procedure is performed.
1. The valves is set appropriately for co-current mode:
2. Valves V2, V4 and V9 remain closed. Valves V3 and V5 are opened.
3. Pump P1 is switched. Valve V1 is opened and adjusted to obtain a liquid flow rate of 500
ml/min.
4. Valve V6 is opened. Valve V8 is adjusted to obtain a gas flow rate of 1 Lmin-1.
5. The conductivity reading of CT2 is obtained and let it stabilizes at low value.
7

6. The dosing pump P2 is switched on. Valve V15 is opened and bleed off any air trapped in
the tubing.
7. Valve V15 is closed. The valve V10 is opened and start timer simultaneously. The
conductivity reading CT2 is recorded at 1 min interval.
8. The recording is continued until conductivity reading is constant.
9. The experiment is repeated with gas flow rate of 2.0 L min-1. The system is ensured that it
is flushed with de-ionized water until no traces of salt is detected.
10. The experiment is stopped and all the liquid from the system are drained out.

4.2 Experiment B: The effect of pulse input.
In this experiment a pulse input would be introduced and the progression of the tracer will be
monitored via the conductivity measurements.
a) Counter-current Mode
The general start-up procedure is performed.
1. The valves is set appropriately for counter-current mode:
2. Valves V3, V5 and V10 remain closed.
3. Valve V1 is opened and switch on pump P1. The column is filled up with de-ionized water
to packing height.
4. Valve V1 is adjusted to obtain a liquid flow rate of 500 ml/min
5. Valve V6 is closed. Open valve V8 to obtain a gas flow rate of 1.0 L min-1.
6. The conductivity reading of CT1 is observed and let it stabilizes at low value.
7. The dosing pump P2 is switched on. Valve V14 is opened and bleed off any air trapped in
the tubing.
8. The valve V14 is close. Valve V9 is opened and start timer simultaneously. The
conductivity reading CT1 is obtained at 1 min interval.
9. The dosing pump P2 is let run for 2 minutes. Close valve V9 and stop pump P2.
10. The recording is continued until conductivity reading is constant.
11. The experiment is repeated with gas flow rate of 2.0 L min-1. The system is ensured to be
flushed with de-ionized water until no traces of salt is detected.
12. The experiment is stopped and all the liquid from the system are drained out.

8

b) Co-current Mode
The general start-up procedure is performed.
1. The valves is set appropriately for co-current mode:
2. Valves V2, V4 and V9 remain closed. Valves V3 and V5 are opened.
3. The pump P1 I switched on. Open and adjust valve V1 to obtain a liquid flowrate of 500
ml/min.
4. Valve V6 is opened. Valve V8 is adjusted to obtain a gas flowrate of 10.
5. The conductivity reading of CT2 is observed and let it stabilizes at low value.
6. The dosing pump P2 is switched on. Valve V15 is opened and bleed off any air trapped in
the tubing.
7. Valve V15 is closed. Valve V10 is opened and start timer simultaneously. The
conductivity reading CT1 is recorded at 1 min interval.
8. Dosing pump P2 is let to run for 2 minutes. Valve V10 is closed and stop pump P2.
9. The recording is continued until conductivity reading is constant.
10. The experiment is stopped and all the liquid from the system are drained out.














9

5.0 RESULTS AND CALCULATIONS
5.1 Results
Experiment A: The effect of step change input.

Liquid Flow rate : 0.5 L min
-1

Air Flow rate : 2.0 L min
-1

Time (min) Conductivity CT1 (s/cm) E(t) (min
-1
)
1 345.8 0.000000
2 343.0 -0.004049
3 354.0 0.007904
4 399.3 0.038678
5 586.9 0.139445
6 944.1 0.288365
7 1402.1 0.436379
8 1914.4 0.567019
9 2314.9 0.632704
10 2654.3 0.667582
11 2964.1 0.688338
12 3205.4 0.689127
13 3347.3 0.667683
14 3469.4 0.645212
15 3584.3 0.624349
16 3660.6 0.599118
17 3708.1 0.571956
18 3746.0 0.546270
19 3782.4 0.523059
20 3805.2 0.500202
21 3818.3 0.478187
22 3823.4 0.457122
23 3829.9 0.438064
24 3839.2 0.420932
25 3845.6 0.404835
26 3843.1 0.388987
27 3855.8 0.375940
28 3853.6 0.362286
29 3864.6 0.350890
30 3862.9 0.339030
Table1: Effect of step change input in counter-current mode




10

Liquid Flow rate : 0.5 L min
-1

Air Flow rate : 2.0 L min
-1

Time (min) Conductivity CT2 (s/cm) E(t) (min
-1
)
1 227.4 0.000000
2 214.8 -0.027704
3 196.1 -0.045881
4 196.7 -0.033751
5 243.8 0.014424
6 334.6 0.078569
7 414.2 0.117351
8 603.7 0.206849
9 796.1 0.277876
10 1023.3 0.350000
11 1297.9 0.427960
12 1417.9 0.436272
13 1525.1 0.438976
14 1570.6 0.421912
15 1869.1 0.481296
16 1876.7 0.453304
17 2007.2 0.460396
18 2152.5 0.470317
19 2256.8 0.469703
20 2171.0 0.427353
21 2311.3 0.436382
22 2278.5 0.409990
23 2387.3 0.412967
24 2425.7 0.402796
25 2458.2 0.392401
26 2363.6 0.361308
27 2569.8 0.381511
28 2523.1 0.360551
29 2589.6 0.358202
30 2603.5 0.348300
Table2: Effect of step change input in co-current mode





11


Figure 1: Graph of conductivity vs time for counter-current and co-current mode in the effect of
step change input


Figure 2: Graph of E(t) vs time for counter-current and co-current mode in the effect of step
change input
0
500
1000
1500
2000
2500
3000
3500
4000
4500
0 5 10 15 20 25 30 35
Conductivity
(s/cm)
Time (min)
Graph of Conductivity , CT versus Time, t
counter
-current
co-
current
-0.100000
0.000000
0.100000
0.200000
0.300000
0.400000
0.500000
0.600000
0.700000
0.800000
0 5 10 15 20 25 30 35
E(t)
(1/min)
Time (min)
Graph of Residence-time distribution function, E(t) versus Time, t
counter
-current
co-
current
12

Experiment B: The effect of pulse input.

Liquid Flow rate : 0.5 L min
-1

Air Flow rate : 2.0 L min
-1

Time (min) Conductivity CT1 (s/cm) E(t) (min
-1
)
1 384.4 0.000000
2 370.0 -0.018730
3 360.8 -0.020465
4 372.5 -0.007739
5 486.7 0.053226
6 672.1 0.124740
7 926.2 0.201353
8 1116.6 0.238098
9 1231.0 0.244710
10 1268.9 0.230099
11 1232.8 0.200643
12 1161.9 0.168553
13 1075.0 0.138197
14 968.9 0.108611
15 865.0 0.083351
16 765.5 0.061963
17 682.6 0.045633
18 605.5 0.031955
19 554.0 0.023221
20 502.1 0.015310
21 472.5 0.010914
22 437.0 0.006220
23 414.6 0.003416
24 392.3 0.000856
25 381.0 -0.000354
26 371.0 -0.001341
27 362.5 -0.002110
28 356.1 -0.002629
29 351.7 -0.002933
30 347.8 -0.003174
Table 3: Effect of pulse input in counter-current mode







13

Liquid Flow rate : 0.5 L min
-1

Air Flow rate : 2.0 L min
-1

Time (min) Conductivity CT2 (s/cm) E(t) (min
-1
)
1 102.7 0.000000
2 60.4 -0.205940
3 52.0 -0.164557
4 46.5 -0.136806
5
76.7
-0.050633
6
130.0
0.044304
7
216.7
0.158576
8 325.3 0.270935
9 390.6 0.311479
10 480.0 0.367381
11 569.6 0.413296
12
497.5
0.320351
13
547.5
0.333159
14 533.1 0.299346
15 509.6 0.264135
16 503.0 0.243610
17 424.1 0.184088
18 436.2 0.180407
19
384.2
0.144263
20
348.4
0.119620
21 311.8 0.096954
22 253.8 0.066876
23 215.2 0.047627
24 211.7 0.044223
25
197.8
0.037040
26
171.1
0.025616
27
137.0
0.012370
28 124.8 0.007685
29 114.7 0.004029
30 118.0 0.004966
Table 4: Effect of pulse input in co-current mode





14


Figure 3: Graph of conductivity vs time for counter-current and co-current mode in the effect of
pulse input

Figure 4: Graph of E(t) vs time for counter-current and co-current mode in the effect of pulse
input
0
200
400
600
800
1000
1200
1400
0 5 10 15 20 25 30 35
Conductivity
(s/cm)
Time (min)
Graph of Conductivity (CT) versus Time (t)
counter
-current
co-
current
-0.300
-0.200
-0.100
0.000
0.100
0.200
0.300
0.400
0.500
0 5 10 15 20 25 30 35
E(t)
(1/min)
Time (min)
Graph of Residence-time distribution function, E(t) versus Time, t
counter-
current
co-
current
15

5.2 Calculations
To calculate the value of residence time distribution function, E(t) for each experiment data,
we use the following formula:
t
C
t C
t E
o
/ 1
) (
) (
(

=
Where:
) (t C is the conductivity of the feed stream at time, t .

o
C is the conductivity of the feed stream at time, 1 = t min.

5.3 Sample Calculation
We take a sample data from Experiment A for counter-current run of the feed stream;
At time, t = 2 min
t
C
t C
t E
o
/ 1
) (
) (
(

=
2 / 1
8 . 345
0 . 343
) (
(

= t E
= -0.004049






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6.0 DISCUSSION AND ERROR ANALYSIS
6.1 Discussion
Experiment A: The Effect of Step Change Input
The main objective of this experiment is to determine the effect of liquid and gas feed
rates and modes on the mean residence time and degree (intensity) of liquid-phase axial
dispersion in a packed bed reactor. The controlling variable governing both the experiment
(A & B) is the method of injection of the tracer (sodium chloride, NaCl) into the feed stream
entering the reactor, for both the counter-current and co-current of liquid and gas feed modes.
For experiment A, the controlling variable is set to step input of tracer injection for both the
counter-current and co-current of liquid and gas feed modes. Step input of tracer injection
describes that the concentration of tracer (sodium chloride in this experiment) in the feed to
the reactor is kept in a level until the concentration in the effluent is indistinguishable from
that in the feed. In counter-current mode, the liquid stream is flowing downward from top of
the column while the gas stream is flowing upward from bottom of the column. The pulse or
step input tracer is injected at the top of the column. On the other hand, in co-current mode,
both the liquid and gas streams are flowing upward from bottom of the column. The pulse or
step input tracer is injected at the bottom of the column.
In experiment A, from the plot of conductivity versus time for both the counter-current and
co-current mode of liquid and gas feed, it can be generally specified that, the conductivity
increases rapidly against time at the beginning phase of the experiment, but then after 12
minutes the increase in the conductivity of the system slowly decreases as it approaches a
constant value. This produces an F-curve for the plot of conductivity versus time for the step
input of tracer injection. This can be explained though as, at the beginning phase of the
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experiment, the reacting system is mixed well, but however when the reaction proceeds
further, the mixing level decreases until a constant level is achieved.
From the comparison of the plot of conductivity versus time between the counter-current
flow and the co-current flow, we can observe that the conductivity over time for counter-
current flow is higher than the co-current flow. This is because; in counter-current flow of the
gas feed and liquid feed, both these phases are well mixed as the entering concentration of
both the gas and liquid feed at a point is low and the flow of these feed is opposing in
direction. This provides a greater tendency for the reacting system to be well mixed. Unlike
in the co-current mode, the gas feed and liquid feed are not exactly well mixed because the
entering concentration of the reacting substances at a point are low and are in the same
direction. This does not provide an ideal condition for a well mixed phase for the reacting
substances. That is why the conductivity over time for co-current is lower than the counter-
current mode.
The residence time, as determined by the gasliquid RTD measurements, provides
information on the flow pattern of the liquid in the bed. As we can see, from the 4
th
minute,
the residence-time distribution function E(t) drastically increase, then after some time it
gradually decreases. The readings become constant over time.

Experiment B: The Effect of Pulse Input
For experiment B, the controlling variable is set to pulse input of tracer injection. In a
pulse input of tracer injection, an amount of tracer is suddenly injected in one shot into the
feed stream entering the reactor in as short time as possible. The experiment of the effect of
pulse input on the conductivity of the feed stream over time is conducted for both the
counter-current and co-current of liquid and gas feed modes.
18

In experiment B, from the plot of conductivity versus time for both the counter-current and
co-current mode of liquid and gas feed, it can be observed that, the conductivity increases
until a maximum value is attained by the reacting system. After that, the conductivity
gradually decreases over time. This correlation produces a bell-graph as what can be
observed from the plot of conductivity versus time for pulse input of tracer injection. This can
be explained though as, at the beginning phase of the experiment; the reacting system is
mixed well until it reaches a maximum level. As the reaction time proceeds further, the
mixing level of the liquid and gas feed decreases, as the concentration of the tracer is
gradually decreasing with time. This results in a decreasing conductivity of the reacting
system.
A few irregularities could be observed from the plot of conductivity versus time in
experiment B for both counter-current and co-current mode. At the beginning of the
experiment (from t=0 min to t=4 min) the conductivity decreases initially before it increases
up to its maximum value. This might due to the presence of tracer amount initially in the
conductivity sensor from previous experiment runs.
From the comparison of the plot of conductivity versus time between the counter-current
flow and the co-current flow in this experiment, we can observe that the conductivity
measured in the counter-current mode is higher and much evenly distributed compared to the
co-current mode. The maximum conductivity achieved in the counter current mode is 1268.9
s/cm whereas in co-current mode, the maximum conductivity is only about 569.6 s/cm.
From the graph of residence-time distribution function, E(t) versus time, we actually can
determine the residence time distribution function of the reactants in a reactor. It describes in
a quantitative manner on how much is the time difference where fluid elements have spent in
the reactor. As a result of this experiment, we obtain that in the counter-current mode, the
19

residence time distribution of the reactants in the reactor is longer compared to that of the co-
current mode. This is because in counter-current mode, the gas and the liquid feed that enter
the packed bed reactor, is from different direction and this allows the particles to have more
collisions and well mixed due to the longer residence time and entering concentration of both
the gas and liquid feed at a point is low. However, in co-current mode, as the reactants enter
the reactor from the same direction, they have shorter time spent to react and well mixed
before exiting the reactor.
In industrial practice, it is most preferable to feed reactants into reactor in counter-current
mode. This is because longer residence time distribution in the reactor allows the reactants to
be evenly mixed and distributed throughout the reactor. This enables the system to achieve its
desired product and in the same time maintaining the quality of product.

6.2 Error Analysis
There are several errors that might have occurred while the experiment is conducted. These
errors might have caused the inaccuracy of the data obtained. They are either caused by the
malfunction or inaccuracy of the instruments used or human error. The possible errors that
might have occurred are discussed further below:
i. The data display on the SOLDAS Data Acquisition System captures up to 1 decimal point
only. This will reduce the accuracy of the data obtained and thus might affect in further
calculations. Hence, it will be better if the data captured are for at least 3 significant
figures for more precise results.
ii. Throughout the experiment, especially for the counter-current flow, the height of the
liquid feed in the packed bed reactor needs to be regulated so that it remains at the packed
bed height in order to obtain an accurate and precise result. However, the water level is not
20

easy to be controlled as the bed is above the human eye level. Thus, it is very possible that
parallax error to occur when we are regulating the flow rate to control the water level. To
reduce this error, student should observe the water level in the reactor at the same eye
level constantly or install a level control system to regulate the flow, in order to obtain a
consistent level of the liquid feed.
iii. The presence of the tracer substance initially from the previous experiment runs might
influence the conductivity measurement of the new experiment run. That is why in
experiment B, the conductivity measurement of the reacting system is higher at the
starting point of the experiment. To avoid this happen, the packed bed reactor needs to be
rinsed for a longer time to remove the tracers effectively.
iv. In addition, even though the liquid flow rate and the gas flow rate is set to be 0.5 L/min
and 2.0 L/min respectively in the beginning of the experiment, but as the reaction
proceeds, the flow rate of these feed fluctuates and is not consistent. This might cause
some inaccuracy in the experiment. Therefore, it is important to constantly regulate the gas
and liquid flow rate and make it consistent at its desired value throughout the experiment.








21

7.0 CONCLUSION
For the experiment A, based on the graph, we can conclude that the residence time for
counter-current mode of liquid and gas feed is higher than the residence time required for the
co-current mode. This is because in co-current, there is a higher resistance of the tracer flow
in the reactor. This resistance forms as the flow of the liquid and gas feed is against each
other. Due to this resistance, the tracer particles are evenly distributed in the reactor column.
In contrast, the resistance in the co-current flow is lower as the gas and liquid feed exits the
reactor column in parallel. This causes the tracer particle for co- current is not evenly
distributed.
For experiment B, the residence time required in counter-current flow is obviously
higher than the co-current flow, which means that, the tracer particles stay longer in time in
the reactor for counter-current flow than the co-current flow. For co-current flow, the
distribution of the tracer particle is not uniform in the reactor column, thus forming dead
zones in the reactor column. In the industry, the counter-current is more preferable to be
applied compared to the co-current. This is because counter-current allows the reactants to
evenly mixed and distributed throughout the reactor due to the longer residence time
distribution in the reactor.

8.0 REFERENCES
1. H. Fogler, Elements of Chemical Reaction Engineering: International Edition, 4th Edition.
2. Octave Levenspiel, Chemical Reaction Engineering: Third Edition.
3. Reaction Engineering Lab Manual; RTD in Packed Bed.