Professional Documents
Culture Documents
April 2023
instructor: -Defre
date of experiment 16 April 2023
date of submission
Table of Contents
Experiment 1 ......................................................................................................... 1
Title ................................................................................................................... 1
Objective ........................................................................................................... 1
Theory and literature review ............................................................................. 1
Experimental procedure .................................................................................... 5
Data collected .................................................................................................... 6
Graph Analysis .................................................................................................. 8
Experiment 2 ..................................................................................................... 16
Title ................................................................................................................. 16
Objective ......................................................................................................... 16
Theory ............................................................................................................. 16
Design equation of CSTR ........................................................................... 16
Reagent preparation ........................................................................................ 17
Procedure ........................................................................................................ 18
Data/Result ...................................................................................................... 19
Graphical analysis ........................................................................................... 20
Experiment 3 ....................................................................................................... 24
Title ................................................................................................................. 24
Objective ......................................................................................................... 24
Theory and literature review ........................................................................... 24
Material and chemical ..................................................................................... 27
Procedure ........................................................................................................ 27
Data or result ................................................................................................... 28
Graphical analysis ........................................................................................... 29
Experiment-4 ....................................................................................................... 39
Title ................................................................................................................. 39
Objective: - ..................................................................................................... 39
Theory ............................................................................................................. 39
Design equation for PFR ............................................................................. 39
Procedure ........................................................................................................ 42
Result/Data ...................................................................................................... 43
Graph Analysis ................................................................................................ 44
Conclusions ..................................................................................................... 49
Experiment 1
Title isothermal saponification reaction in batch reactor
Objective
To determine the order and value of the rate constant for the liquid
reaction of caustic soda and ethyl acetate in a batch reactor:
information regarding:
1
operating the batch reactor, the correct stability conditions can be
found for each reaction and thus a runaway of the reaction on the
operation of a continuous reactor can be avoided. Batch reactor is
normally used in small scale industry set-ups to study the kinetics of
chemical reaction.
Simple in construction.
Small instrumentation and cost.
Flexibility of operation.
r = kCACB..............................(2)
The stoichiometric equations in terms of fractional conversion X are: -
But when CA,o = CB,o and CA,oXA, = CB,oXB,o, then CB is also equal
to CA,o(1 − XA) and the rate equation become:
𝑑𝑑𝑑𝑑𝑑𝑑 𝑑𝑑𝑑𝑑𝑑𝑑
= 𝐶𝐶𝐶𝐶 …………………(8)
𝑑𝑑𝑑𝑑 𝑑𝑑𝑑𝑑
3
4
From the conductivity values the percentage conversion of the reactant S can be calculated as:
The temperature dependence of the reaction rate constant could be correlated by the Arrhenius
equation: -
Experimental procedure
The batch reactor was attached to the trainer above the collecting tray and then opened.
It was ensured that all lower-level switches on the CE 310 main unit are switched off.
The Switch was switched on the unit CE 310 only at the master was switched on.
In a glass beaker a solution containing 400ml of distilled water and 1.6g 0.1M Sodium Hydroxide was
prepared. We Measured by using the measuring sensor, the conductivity and temperature of the solution.
Again, in another glass beaker a solution containing 400ml of distilled water and 4ml 0.1M Ethyl
Acetate was prepared and then measured by using the measuring sensor, the conduction and temperature
of the solution.
5
The conductivity measuring sensor in the measuring opening on the lid was inserted and connected to
the stirrer
The stirrer to a medium speed was adjusted.
The rubber bung of the lid was removed.
Both solutions were quickly poured into the reaction tank with the help of the funnel
through the hole.
The hole in the lid with rubber was closed and switched on the stirrer.
Continuously the conductivity and temperature values were taken until the steady
condition was reached within the gap of 3 minutes.
The data was recorded in the table form.
Data collected
time con tem 1/T XA CA K lnK rA lnCA CA^2 1/CA
(sec d p
) (Z) (0C)
0 20. 30 0.0333 0 0.1 #DIV/ #DIV/ #DIV/ - 0.01 10
1 33 0! 0! 0! 2.302
59
30 9.1 24.9 0.0401 0.7236 0.0276 0.8730 - 0.0006 - 0.0007 36.190
61 84 32 16 0.1358 67 3.588 64 48
8
60 8.5 25.7 0.0389 0.7631 0.0236 0.5370 - 0.0003 - 0.0005 42.222
11 58 84 37 0.6216 01 3.742 61 22
9 95
90 8 26.6 0.0375 0.7960 0.0203 0.4336 - 0.0001 - 0.0004 49.032
94 53 95 92 0.8354 8 3.892 16 26
2 48
120 7.5 27.4 0.0364 0.8289 0.0171 0.4038 - 0.0001 - 0.0002 58.461
96 47 05 46 0.9067 18 4.068 93 54
2 37
150 7.1 28.1 0.0355 0.8552 0.0144 0.3939 - 8.25E- - 0.0002 69.090
87 63 74 39 0.9315 05 4.235 09 91
6 42
180 6.8 28.6 0.0349 0.875 0.0125 0.3888 - 6.08E- - 0.0001 80
65 89 0.9444 05 4.382 56
6 03
210 6.5 29 0.0344 0.8947 0.0105 0.4047 - 4.48E- - 0.0001 95
83 37 26 62 0.9044 05 4.553 11
6 88
240 6.3 29.3 0.0341 0.9078 0.0092 0.4107 - 3.48E- - 8.48E- 108.57
3 95 11 14 0.8898 05 4.687 05 14
6
6 41
270 6.1 29.6 0.0337 0.9210 0.0078 0.4320 - 2.69E- - 6.23E- 126.66
84 53 95 99 0.8391 05 4.841 05 67
56
300 6 29.8 0.0335 0.9276 0.0072 0.4272 - 2.24E- - 5.24E- 138.18
57 32 37 73 0.8503 05 4.928 05 18
3 57
330 5.8 30 0.0333 0.9407 0.0059 0.4814 - 1.69E- - 3.51E- 168.88
33 89 21 81 0.7308 05 5.129 05 89
9 24
360 5.7 30.1 0.0332 0.9473 0.0052 0.5 - 1.39E- - 2.77E- 190
23 68 63 0.6931 05 5.247 05
5 02
390 5.6 30.2 0.0331 0.9539 0.0046 0.5311 - 1.13E- - 2.12E- 217.14
13 47 05 36 0.6327 05 5.380 05 29
4 56
420 5.5 30.3 0.0330 0.9605 0.0039 0.5793 - 9.03E- - 1.56E- 253.33
03 26 47 65 0.5458 06 5.534 05 33
2 71
450 5.4 30.4 0.0328 0.9671 0.0032 0.6533 - 7.07E- - 1.08E- 304
95 05 89 33 0.4256 06 5.717 05
7 03
480 5.3 30.5 0.0327 0.9736 0.0026 0.7708 - 5.34E- - 6.93E- 380
87 84 32 33 0.2602 06 5.940 06
8 17
510 5.2 30.5 0.0327 0.9802 0.0019 0.9738 - 3.79E- - 3.9E- 506.66
87 63 74 56 0.0264 06 6.227 06 67
9 85
540 5.2 30.6 0.0326 0.9802 0.0019 0.9197 - 3.58E- - 3.9E- 506.66
8 63 74 53 0.0836 06 6.227 06 67
5 85
570 5.1 30.6 0.0326 0.9868 0.0013 1.3157 0.2744 2.28E- - 1.73E- 760
8 42 16 89 37 06 6.633 06
32
600 5 30.7 0.0325 0.9934 0.0006 2.5166 0.9229 1.09E- - 4.33E- 1520
73 21 58 67 35 06 7.326 07
47
630 5 30.7 0.0325 0.9934 0.0006 2.3968 0.8741 1.04E- - 4.33E- 1520
73 21 58 25 45 06 7.326 07
47
660 4.9 30.7 0.0325 1 -2.2E- - #NU -3.4E- #NU 4.93E- -
73 17 6.8E+ M! 20 M! 34 4.5E+
7
13 16
690 4.9 30.7 0.0325 1 -2.2E- - #NU -3.2E- #NU 4.93E- -
73 17 6.5E+ M! 20 M! 34 4.5E+
13 16
720 4.9 30.8 0.0324 1 -2.2E- - #NU -3.1E- #NU 4.93E- -
68 17 6.3E+ M! 20 M! 34 4.5E+
13 16
Graph Analysis
The following graph shows the analysis of the data obtained for the batch reactor. The graphs
are taken randomly from the calculated data.
time vs concentration
0.12
0.1
0.08
0.06
0.04
0.02
0
0 5 10 15 20 25 30
-0.02
8
Time Vs conductivity
25
20
15
conductivity
10
0
0 5 10 15 20 25 30
time
Time Vs convertion
1.2
0.8
conductivity
0.6
0.4
0.2
0
0 5 10 15 20 25 30
-0.2
time
30
25
TEMPRATURE)
20
15
10
0
0 5 10 15 20 25 30
TIME
0
0 5 10 15 20 25 30
-1E+13
-2E+13
RATE CONSTANT
-3E+13
-4E+13
-5E+13
-6E+13
-7E+13
-8E+13
TIME
0.0007
0.0006
0.0005
0.0004
0.0003
0.0002
0.0001
0
0 5 10 15 20 25 30
-0.0001
TIME
0.1
0.08
concentration
0.06
0.04
0.02
0
0 5 10 15 20 25 30
-0.02
conversion
11
As we observe the graph, the conversion and the concentration have inversely relationship due
to the effect of temperature.
0.0005
0.0004
0.0003
0.0002
0.0001
0
-0.0001 0 5 10 15 20 25 30
conersion
0.8
rate constant
0.6
0.4
0.2
0
0 5 10 15 20 25 30
time
12
Concentration vs. rate reaction
0.12
0.1
0.08
0.06
0.04
0.02
0
0 5 10 15 20 25 30
-0.02
0.0006
0.0005
0.0004
Axis Title
0.0003
0.0002
0.0001
0
0 5 10 15 20 25 30
-0.0001
Axis Title
Series2
13
Figure 12 Temperature vs. rate constant
Looking from the graph, as temperature increase rate constant increase parabolic ally until some
interval then it immediately decrease down to null.
14
Observing the graph, it shows that at the start when the temperature increases the rate of
reaction is high (well mixed) but, as we keep increasing the temperature, the reactant will lose
the ability to react and this leads the decrement of the rate of reaction.
15
Experiment 2
Title: - Single Continuous Stir Tank Reactor (CSTR)
Objective
Determination of the kinetics parameter of the saponification reaction between 0.1 M sodium hydroxide and
0.1M ethyl acetate in CSTR at (25-45) (°c).
Theory
A continuous stirred tank reactor (CSTR) is a reaction vessel in which reagents, reactants and often solvents
flow into the reactor while the product of the reaction concurrently exit the vessel. In this manner the tank
reactor is considered to be a valuable tool for continuous chemical processing.
The behavior of a CSTR is often approximated or modeled by that of an ideal CSTR, which assumes perfect
mixing In a perfectly mixed reactor, reagent is instantaneously and uniformly mixed throughout the reactor
upon entry. Consequently, the output composition is identical to composition of the material inside the reactor,
which is a function of residence time and reaction rate.
. It is normally operated at steady state and is assumed to be perfectly mixed; consequently, there is no time
dependence or position dependence of the temperature, concentration, or reaction rate inside the CSTR. That is,
every variable is the same at every point inside the reactor. Because the temperature and concentration are
identical everywhere within the reaction vessel, they are the same at the exit point as they are elsewhere in the
tank. Thus, the temperature and concentration in the exit stream are modeled as being the same as those inside
the reactor. In systems where mixing is highly nonideal, the well-mixed model is inadequate, and we must resort
to other modeling techniques, such as residence time distributions, to obtain meaningful results.
Design equation of CSTR
Assumption
16
• Measuring cylinder
• Volumetric flask
• Funnel
• Pipette
• Beaker
• Magnetic stirrer
Chemical used
• Ethyl acetate
• Sodium hydroxide
Reagent preparation
17
Procedure
First, we attached the single continuous stirrer tank reactor to the system unit then Connect the water hoses
from the heating system to the connections on the base of the tank and to the switch housing. Connect the
chemical hoses from the pumps to the tank using the rapid action connectors. Insert the conductivity-
measuring sensor in the measuring opening on the lid and connect the stirrer. Adjust the overflow on the tank
such that the measuring sensor is immersed approximately 50 mm in the liquid with the tank filled. Ensure
that all subordinate switches on the main unit are switched off and then switch on the unit at the master switch.
Set the required water temperature for the heating regulator to [28, 32, 36,400C] and switch on the heater.
Switch on the chemical pumps and adjust both to the same flow rate of approximately 40%. When the liquid
level reaches the overflow, switch on the stirrer and adjust to a medium speed. At regular intervals of
approximately 20-30 seconds, the conductivity and reaction temperature indicated on the measuring unit until
stable values are reached Then reduce the flow rate of both chemical pumps to the same value of approx. 40%.
Check whether the hot water temperature has reached [28, 32, 36,400C] and switch on the hot water pump. The
conductivity and reaction temperature indicated on the measuring unit at regular intervals of approximately 20-
30 seconds until stable values are reached. Then increase the flow rate of both chemical pumps back to the
same value of approximately 80% . Again log the conductivity and reaction temperature indicated on the
measuring unit at regular intervals of approximately 20-30 seconds until stable values are reached. When
finished switch off chemical pumps, heater, hot water pump and stirrer. Export the measured data and save it if
you are done by computer or record your data in table if you work manually.
18
Data/Result
Initial Conductivity of 0.2M NaOH ...mS/cm
Initial Conductivity of 0.2M ethyl Acetate ... . .mS/cm
t
Pump λ(mS/cm T(OC) xa CA K lnk 1/T rA ater
(sec.)
Bat
0 20.1 30 0 0.1 #DIV/0! #DIV/0! 0.03333333 #DIV/0!
h
30 8.9 27.1 0.95726 0.00427 7.46667 2.01045 0.03690037 0.03111
tem
80% 60 8.7 27.7 0.97436 0.00256 6.33333 1.84583 0.03610108 0.01583
pera
90 8.6 28.2 0.98291 0.00171 6.38889 1.85456 0.03546099 0.01065
ture
120 8.5 28.5 0.99145 0.00085 9.66667 2.26868 0.03508772 0.00806 inlet
150 8.4 28.7 1 -2E-17 -3E+14 #NUM! 0.03484321 0.0065 for
180 8.1 29.3 0 0.1 0 #NUM! 0.03412969 0 heat
210 8 29.5 0.04348 0.09565 0.00216 -6.1356 0.03389831 0.00159 exc
40% 240 7.9 29.6 0.08696 0.0913 0.00397 -5.5294 0.03378378 0.00278 han
270 7.8 29.78 0.13043 0.08696 0.00556 -5.193 0.03357958 0.0037 ge
300 7.8 29.7 0.13043 0.08696 0.005 -5.2983 0.03367003 0.00333
330 7.9 29.4 0 0.1 0 #NUM! 0.03401361 0.00202
360 8 29.3 0.5 0.05 0.02778 -3.5835 0.03412969 0.00093
80% 390 8.1 29.2 1 3.6E-16 7.2E+12 29.6075 0.03424658 0.00154
420 8.1 29.2 1 3.6E-16 6.7E+12 29.5334 0.03424658 0.00135
450 8.1 29.2 1 3.6E-16 6.3E+12 29.4644 0.03424658 0.0022
19
Graphical analysis
25
20
conductivity
15
10
0
0 50 100 150 200 250 300 350 400 450 500
time
Conductivity vs time
0.12
0.1
0.08
0.06
ca
0.04
0.02
0
0 50 100 150 200 250 300 350 400 450 500
-0.02
TIME
Concentration vs time
20
1.2
0.8
0.6
xa
0.4
0.2
0
0 50 100 150 200 250 300 350 400 450 500
t
Conversion vs time
25
20
15
cond
10
0
-0.02 0 0.02 0.04 0.06 0.08 0.1 0.12
ca
Conductivity vs concentration
21
1.2
0.8
0.6
xa
0.4
0.2
0
-0.02 0 0.02 0.04 0.06 0.08 0.1 0.12
ca
Conversion vs concentration
0.035
0.03
0.025
0.02
0.015
rA
0.01
0.005
0
26.5 27 27.5 28 28.5 29 29.5 30 30.5
-0.005
T
22
8E+13
7E+13
6E+13
5E+13
4E+13
1/T
3E+13
2E+13
1E+13
0
-10 -5 0 5 10 15 20 25 30 35 40
-1E+13
LNK
1/T vs lnK
0.12
0.1
0.08
0.06
CA
0.04
0.02
0
-0.005 0 0.005 0.01 0.015 0.02 0.025 0.03 0.035
-0.02
RA
23
Experiment 3
Title continuous stirred tank reactor in serious (CSTR in serious)
Objective: - to determination of the reaction rate constants[k], conversion and efficiency of
CSTR in series.
• Determination of steady operating points depending on the retention time.
• Comparison of different reactor types
The mass balance expression for any control volume analysis can be expresses as:
In − out − Loss + Generation = Accumulation (Eq. 2)
Where in = mass of constituent entering system
Out = mass of constituent leaving system
Loss = mass of constituent disappearing
Generation = mass of constituent appearing within system due to reaction
Accumulation = mass of constituent accumulating in system
Because the tracer is added as a pulse input (single event), the influent concentration could be assumed as zero
after the initial injection of the tracer. At the same time, because the tracer substance is considered as
24
conservative (no reaction occurs during the experiment), the generation term could be assumed as zero too.
Then equation (2) becomes:
25
Third reactor in the series
For this third reactor, the generation term (in equation (2)) is still assumed as null, but the influent concentration
changes with time and is equal to the effluent concentration from the second CSTR in the series, thus:
26
Advantages
Conversion of reactant to product per volume of reactor is small compared to other flow reactors
Dead zones, where no mixing occurs, can develop
Reactants can bypass if outlet placed improperly
Procedure
1. Attach the continuous stirrer tank reactor in series to the system unit.
2. addition equipment is there for only CSTR that measure four [series] conductivity and temperature.so attach
this part to system unit.
3. Insert the conductivity measuring sensor in the measuring opening on the lid and connect the stirrer. Connect
the chemical hoses from the pumps to the tank using the rapid action connectors.
4. Adjust the overflow on the tank such that the measuring sensor is immersed approximately 50 mm in the liquid
with the tank filled.
27
5. Ensure that all subordinate switches on the main unit are switched off and then switch on the unit at the master
switch.
6. Switch on the chemical pumps and adjust both to the same flow rate of approximately 400/0.
7. When the liquid level reaches the overflow, switch on the stirrer and adjust to a medium speed.
8. At regular intervals of approximately 20-30 seconds, the conductivity and reaction temperature indicated on the
measuring unit until stable values are reached
9. Then reduce the flow rate of both chemical pumps to the same value of approx. 40%.
10.Then the conductivity and reaction temperature indicated on the measuring unit at regular intervals of
approximately 20- 30 seconds until stable values are reached.
11.The conductivity and reaction temperature indicated on the measuring unit at regular intervals of approximately
20-30 seconds until stable values are reached.
12.Then increase the flow rate of both chemical pumps back to the same value of approximately 80%.
13.Again, log the conductivity and reaction temperature indicated on the measuring unit at regular intervals of
approximately 20-30 seconds until stable values are reached.
14.When finished switch off chemical pumps and stirrer.
Export the measured data and save it if you are done by computer or record your data in table if you work
manually.
Data or result
Pu Ti Cond
CA
mp me Tem 1
1& p1 XA rA K XA (%) CA2 lnK 1/CA
(ms/ (Mol/L
2 (s) ( C)
o
cm) )
(%)
#NU
0 30 20.5 0 0.1 0 0 0 0.01 10
M!
0.8356 0.0164 0.0835 309.23 83.561 0.000 5.734 60.83
30 24.5 8.3
1644 3836 6164 6111 6438 27 105 333
80 0.8356 0.0164 0.0835 309.23 83.561 0.000 5.734 60.83
60 24.5 8.3
1644 3836 6164 6111 6438 27 105 333
0.8356 0.0164 0.0835 309.23 83.561 0.000 5.734 60.83
90 24.5 8.3
1644 3836 6164 6111 6438 27 105 333
12 0.8356 0.0164 0.0835 309.23 83.561 0.000 5.734 60.83
24.8 8.3
0 1644 3836 6164 6111 6438 27 105 333
28
15 0.8424 0.0157 0.0842 339.47 84.246 0.000 5.827 63.47
24.5 8.2
0 6575 5342 4658 0699 5753 248 388 826
Graphical analysis
converstion vs rate of rxn
0.09
0.08
0.07 y = 0.1x - 6E-11
R² = 1
0.06
0.05
rate of rxn
0.04
0.03
0.02
0.01
0
-0.01 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
converstion
conductivity vs concentration
0.12
0.1
concentration
0.04
0.02
0
0 5 10 15 20 25
conductivity
0.0059
0.00585
0.0058
0.00575
0.0057
0.869 0.87 0.871 0.872 0.873 0.874 0.875 0.876 0.877 0.878
Conversion
Conductivity vs concentration
0.0131
0.013
0.0129
y = 0.0068x - 0.0404
concentration
0.0128
R² = 1
0.0127
0.0126
0.0125
0.0124
0.0123
0.0122
7.68 7.7 7.72 7.74 7.76 7.78 7.8 7.82
Conductivity
30
Figure 2 conductivity vs concentration
Table 3 The data recorded for reactor 1 at 80 % flow rate (second trial)
Pu Ti Con
mp me Te d1 CA
1& mp
XA rA K XA (%) CA2 lnK 1/CA
2 1 (ms/ (Mol/L
(% (s) (oC) cm) )
)
33 24. 0.8561 0.0143 0.0856 413.83 85.616 0.0002 6.0254 69.523
8
0 8 6438 8356 1644 22 4384 0689 6058 8095
36 24. 0.8493 0.0150 0.0849 374.04 84.931 0.0002 5.9243 66.363
8.1
80 0 7 1507 6849 3151 9587 5068 2706 8837 6364
39 24. 0.8424 0.0157 0.0842 339.47 84.246 0.0002 5.8273 63.478
8.2
0 7 6575 5342 4658 0699 5753 4817 8764 2609
42 24. 0.8424 0.0157 0.0842 339.47 84.246 0.0002 5.8273 63.478
8.2
0 8 6575 5342 4658 0699 5753 4817 8764 2609
0.0848
0.0846
0.0844
0.0842
0.084
0.84 0.842 0.844 0.846 0.848 0.85 0.852 0.854 0.856 0.858
conversion
31
conductivity vs concentration
0.016
0.0158
0.0156 y = 0.0068x - 0.0404
R² = 1
concentration
0.0154
0.0152
0.015
0.0148
0.0146
0.0144
0.0142
7.95 8 8.05 8.1 8.15 8.2 8.25
conductivity
32
Conversion vs rate of rxn
0.1
0.04
0.02
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
-0.02
Conversion
Conductivity vs concentration
0.12
0.08
0.06
0.04
0.02
0
0 5 10 15 20 25
Conductivity
R² = 1
0.0938
0.0936
0.0934
0.0932
0.093
0.93 0.932 0.934 0.936 0.938 0.94 0.942 0.944 0.946
conversion
Conductivity vs concentration
0.008
0.007
0.006
concentration
0.005
0.004
0.003 y = 0.0068x - 0.0404
R² = 1
0.002
0.001
0
6.65 6.7 6.75 6.8 6.85 6.9 6.95
conductivity
34
1& 2
(ms/ (Mol/L
2 (s) (o C
cm) )
(%) )
2.298
33 24. 0.9520 0.0047 0.0952 4141.6 95.205 8.3288 208.57
6.6 7E-
0 8 5479 9452 0548 3265 4795 453 1429
05
36 24. 0.9383 0.0061 0.0938 2469.3 93.835 3.8E- 7.8117 162.22
6.8
80 0 9 5616 6438 3562 8272 6164 05 235 2222
3.002
39 24. 0.9452 0.0054 0.0945 3148.1 94.520 8.0545
6.7 4E- 182.5
0 9 0548 7945 2055 25 5479 623
05
42 24. 0.9383 0.0061 0.0938 2469.3 93.835 3.8E- 7.8117 162.22
6.8
0 9 5616 6438 3562 8272 6164 05 235 2222
conversion vs rate of rxn
0.0954
0.0952
y = 0.1x - 4E-13
0.095
R² = 1
0.0948
0.0946
rate
0.0944
0.0942
0.094
0.0938
0.0936
0.936 0.938 0.94 0.942 0.944 0.946 0.948 0.95 0.952 0.954
conversion
Conductivity vs concentration
0.007
0.006
0.005
concentration
0.004
0.003
0.002 y = 0.0068x - 0.0404
R² = 1
0.001
0
6.55 6.6 6.65 6.7 6.75 6.8 6.85
Conductivity
35
Table 7 The recorded data for reactor 3 at 80 % flow rate (first trial)
Pu Ti Te Cond
CA
mp me mp 3
XA
1& 3 XA rA K CA2 lnK 1/CA
(ms/c (%)
2 (s) (o C (Mol/L)
m)
(%) )
0.0 #NU
0 30 20.5 0 0.1 0 0 0 10
1 M!
3.8
24. 0.93835 0.00616 0.09383 2469.38 93.83 7.811 162.2
30 6.8 E-
7 616 438 562 272 562 723 222
05
24. 0.94520 0.00547 0.09452 3148.12 94.52 3E- 8.054
60 6.7 182.5
7 548 945 055 5 055 05 562
80 2.3
24. 0.95205 0.00479 0.09520 4141.63 95.20 8.328 208.5
90 6.6 E-
7 479 452 548 265 548 845 714
05
2.3
12 24. 0.95205 0.00479 0.09520 4141.63 95.20 8.328 208.5
6.6 E-
0 8 479 452 548 265 548 845 714
05
2.3
15 24. 0.95205 0.00479 0.09520 4141.63 95.20 8.328 208.5
6.6 E-
0 9 479 452 548 265 548 845 714
05
0.02
0.01
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Conversion
36
Conversion vs rate of rxn
0.1
0.09
0.08 y = 0.1x
0.07 R² = 1
0.06
0.05
0.04
0.03
rate
0.02
0.01
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Conversion
0.097
0.0965
0.096
37
0.0955
0.955 0.96 0.965 0.97 0.975 0.98 0.985
conversion
Figure 2 Conversion vs rate of rxn
conduction vs concentration
0.0045
0.004 y = 0.0068x - 0.0404
0.0035 R² = 1
concentration
0.003
0.0025
0.002
0.0015
0.001
0.0005
0
6.15 6.2 6.25 6.3 6.35 6.4 6.45 6.5 6.55
conduction
38
Experiment-4
Title: - Plug Flow Reactor [PFR]
Objective: -
To determine the rate constant for the liquid reaction of caustic soda and ethyl acetate in a PFR.
The objectives of this experiment were to carry out the saponification reaction
between Sodium Hydroxide ( NaOH) And Ethyl Acetate (Et(Ac)), to determine the effect of
residence time to the extent of reaction of conversion and to evaluate the reaction rate constant
of this saponification reaction.
Theory:
A Plug Flow Reactor (PFR) consisted in a long, straight pipe in which the reactive fluid
transits at steady state ( no accumulation). The main assumption of this models is that the
fluid is completely mixed in any cross-section at any point, but it experiences no axial mixing,
i.e., contiguous cross sections cannot exchange mass with each other.
In a plug 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.
1. no mixing in the axial direction
2. complete mixing in the radial direction
3. a uniform velocity profile across the radius.
Tubular reactors are one type of flow reactors. It has continuous inflow and outflow of
materials. In the 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 stirring prevent complete
mixing of the fluid in the tube
Design equation for PFR
Assumption
• Good mixing applies on the small volume element
• No accumulation dn/dt=0.
• Input — Output + Generation = Accumulation
39
FAO - FA + frAdV = dNA/dt, But and dFA=-FA0dX
FAO - FA = rAdV
FAO-FAO+FAOdX=rAdV
FA0dX/ =kdV
vCAO(1 - XA)2
XA
CAO(I - XA)2
Apparatus used
Burette
conical flask
measuring cylinder
ph indicator
beakers
Chemical used:
Dilution formula
41
MIVI=M2V2
Weigh 20g of pure NaOH using analytical balance and add into 2000ml of beakers.
Add around 2000ml of distilled water and mix using stirrer road for at least five minutes.
Then transfer into 2500ml of volumetric flacks and add distilled water until its mark.
Close the volumetric flacks and shake well.
Procedure
First, we attach the tubular flow reactor to the system unit. Then Connect the chemical hoses from the pumps to
the tank using the rapid action connectors. Connect the water hoses from the hot water system to the
connections on the base of the tank and to the switch housing. Ensure that the end of the overflow hose is in the
collecting tray. Ensure that all lower-level switches on the main unit are switched off and then switch on the
unit at the master switch. Ensure that all lower-level switches on the main unit are switched off and then switch
on the unit at the master switch. Set the required water temperature for the heating regulator to [28, 32,
36,400C] and switch on the heater. Switch on the chemical pumps and adjust both to the same flow rate of
approximately 40%. When the liquid level reaches the overflow, switch on the stirrer and adjust to a medium
speed. At regular intervals of approximately 20-30 seconds, the conductivity and reaction temperature indicated
on the measuring unit until stable values are reached. Then reduce the flow rate of both chemical pumps to the
same value of approx. 40%. Then the conductivity and reaction temperature indicated on the measuring unit at
regular intervals of approximately 20- 30 seconds until stable values are reached. Check whether the hot water
temperature has reached [28, 32, 36,400C] and switch on the hot water pump. The conductivity and reaction
temperature indicated on the measuring unit at regular intervals of approximately 20-30 seconds until stable
42
values are reached. Then increase the flow rate of both chemical pumps back to the same value of
approximately 80% Again log the conductivity and reaction temperature indicated on the measuring unit at
regular intervals of approximately 20-30 seconds until stable values are reached. When finished switch off
chemical pumps, heater, hot water pump and stirrer. Export the measured data and save it if you are done by
computer or record your data in table if you work manually
Result/Data
• Initial Conductivity of 0.1M NaOH .mS/cm
43
720 30.2 7.5 0.95588235 0.004412 0.09558824 4911.111 95.5882353 1.95E-05 8.499255 226.6667
720 30.2 7.5 0.95588235 0.004412 0.09558824 4911.111 95.5882353 1.95E-05 8.499255 226.6667
Graph Analysis
The following graph shows the analysis of the data obtained for the batch reactor. The graphs
are taken randomly from the calculated data.
First Trial of 80 %
Conversion vs Concentration
1.2
y = -0.0735x + 1.5074
1
R² = 1
Concentration
0.8
0.6
0.4
0.2
0
0 5 10 15 20 25
Conversion
Conversion Vs Concentration
0.12
0.1
y = -0.1x + 0.1
Concentration
0.08 R² = 1
0.06
0.04
0.02
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Conversion
44
Figure for Conversion Vs Concentration
This plot shows the relationship between the conversion and the concentration. In theory, the
above-mentioned two parameters are expected to have an inverse relationship. As you can see
from the graph below, as the reaction proceeds, the reactant concentration decreases, i.e., the
reactants begin to convert to the product, while the conversion of this reactant increases.
However, our calculation shows a negative value. The reason for this is that there is an error in
the lab experiment. These errors can be personal errors or instrumental errors.
0.97
0.96
0.95
0.94
7 7.1 7.2 7.3 7.4 7.5 7.6 7.7
Conductivity
0.004
0.002
45
0
0.945 0.95 0.955 0.96 0.965 0.97 0.975 0.98 0.985 0.99
Conversion
Theoretically we expect inverse relationship between the above two parameters. As expected
the graph shows that as the reaction is going on, the concentration of the reactant decreases i.e.
the reactants start to convert to product and at the same time the conversion of the reactant is
increased. But there is a negative value in our calculation. This is due to the error occurred
during lab experiment. The errors may be personal or instrumental. The other thing we have to
discuss here is the effect of flow rate. Theoretically the decrement in the flow rate leads to
increment in conversion and decrement in concentration. As we have seen, our calculation and
graph also realized this theory practically.
2nd trial
The graph for 80 flow rate
Conductivity vs Conversion
1.01 y = -0.0735x + 1.5074
1 R² = 1
0.99
Conversion
0.98
0.97
0.96
0.95
0.94
0.93
6.8 6.9 7 7.1 7.2 7.3 7.4 7.5 7.6 7.7 7.8
Conductivity
46
Figure for Conductivity vs Conversion
This graph shows that the conductivity and conversions are inversely related. i.e As the
conductivity decreases the conversion increases which is what we have expected theoretically.
As the reaction is going on, the Na ion present in the reaction dissolves and become fewer
conductors. At the same time the conversion of the reactant is favored. But here data recorded is
stopped on the 180 second because the solution ends from the tank at this time.
Conversion vs Concentration
0.006
y = -0.1x + 0.1
0.005
R² = 1
Concentration
0.004
0.003
0.002
0.001
0
0.945 0.95 0.955 0.96 0.965 0.97 0.975 0.98 0.985 0.99
Conversion
This plot represents the relationship between conversion and concentration. Theoretically we
expect inverse relationship between the above two parameters. As expected, the graph shows
that as the reaction is going on, the concentration of the reactant decreases i.e. the reactants start
to convert to product and at the same time the conversion of the reactant is increased. But there
is a negative value in our calculation. This is due to the error occurred during lab experiment.
The errors may be personal or instrumental .
47
The graph for 40 flow
Conductivity vs Conversion
0.99
0.98
y = -0.0735x + 1.5074
Conversion
0.97 R² = 1
0.96
0.95
0.94
7 7.1 7.2 7.3 7.4 7.5 7.6 7.7
Conductivity
Conversion vs Concentration
0.006
0.005
y = -0.1x + 0.1
R² = 1
Concentration
0.004
0.003
0.002
0.001
0
0.945 0.95 0.955 0.96 Conversion0.97
0.965 0.975 0.98 0.985 0.99
48
Third trial
Conductivity vs Conversion
y = -0.0735x + 1.5074
0.99 R² = 1
0.98
Conversion
0.97
0.96
0.95
0.94
7 7.1 7.2 7.3 7.4 7.5 7.6 7.7
Conductivity
Conductivity vs Conversion
Conversion vs Concentration
0.006
0.005 y = -0.1x + 0.1
R² = 1
Concentration
0.004
0.003
0.002
0.001
0
0.945 0.95 0.955 0.96 0.965 0.97 0.975 0.98 0.985 0.99
Conversion
Conversion vs Concentration
Conclusions
The objective of this experiment which were to carry out the saponification process between NaOH and
Et(Ac) and the relationship was graphed in figure (1) was conducted in this experiment. The
results that were obtained was not really satisfied the theory of PFR as the increasing of residence time, suppose
the value of conversion of reaction should be almost constant. From this experiment, the value rate of reaction
this particular reaction was also being done by doing some calculation as shown in sample calculation section.
49