Republic of the Philippines

EASTERN VISAYAS STATE UNIVERSITY

Tacloban City

Laboratory Report in ChE 512L

CHEMICAL ENGINEERING LABORATORY II

by

CABIDOG, Vergel B.

PAGARAO, Alyssa Isabel D.

PROGELLA, Marygrace S.

RABI, Chadine E..

BSChE-5A

Submitted to:

ENGR. JOAN R. ALIGANTE – TOLEDO

ChE Faculty

December 2019
 Experiment No. 3
REACTION KINETICS EXPERIMENT USING TUBULAR FLOW REACTOR

Introduction

Chemical Reaction Engineering is an area where Chemical Engineers are very much
needed and will play important roles in the design, operation and maintenance of industrial
plants that involved chemical reactors. There are many type of reactors, depending on the
phases involved, batch or continuous operation. Among the continuous reactors that are
commonly used in the industry are constant stirred tank reactors (CSTR) and tubular or plug
flow tubular reactors (PFTR). The Plug Flow Reactor is an ideal steady-state reactor. Here, the
flow of fluid through the reactor involves no overtaking or mixing with other elements or
behind. Although there maybe lateral mixing of fluid, it does not involve mixing or diffusion
along the flow path. In this experiment, the students tested a laboratory size plug flow reactor to
determine the design parameters associated with the kinetics of a liquid phase second order
reaction at different operating temperatures [ CITATION Ola151 \l 13321 ].

Figure 1. Plug Flow Reactor

Analysis of the performance of the PFTR by making material balance for a component A,
Levenspiel (1999) presents the following:

Input=Output + Disappearnace+ Accumulation

Where:

Input of A (moles /time)=F A

Output of A moles /time¿ ¿=F A + D F A

Disappearance of A moles/time ¿ ¿=(−r A ) dV

Substituting these values,

F A=( F A + D F A ) + (−r A ) dV
Objective

1. To determine the reaction rate constant and the reaction rate at a given temperature
using a plug flow reactor.

2. To determine the activation energy of a reaction.

3. To determine the order of a reaction using experimental data gathered from a tubular
flow reactor.

Materials and Equipment

(a) 20 liters 0.05 M Ethyl Acetate - working reactant

(b) 20 liters 0.05 M Caustic Soda
(c) 2 liters 0.05 M Hydrochloric Acid
(d) 1 liter 0.02 M NaOH Titrant
(e) Phenolphthalein indicator – used in titration
(f) Distilled water – used to prepare solutions
(g) 1 L glass flask and stopper – container for the working reactants
(h) 2-10 mL pipette – used for titration
(i) 2-50 mL burette – used for titration
(j) 2 pcs titration flask – used for titration
(k) ARMFIELD Plug Flow Tubular Reactor Module
(l) Timer

Procedure

1. At the outset, all the chemicals used in the experiment as feed, titrant or indicators were
prepared based on the specified concentrations in the Materials and Equipment section.
For the feeds, 99 ml of pure ethyl acetate and 40 grams of pure sodium hydroxide were
separately dissolved in 20 liters of de-ionized water to attain 0.05 molarities for both. The
two-liter 0.05 M hydrochloric acid quench was prepared by diluting 30.63 ml of pure
HCl to de-ionized water. Similarly, to prepare the one-liter 0.02 sodium hydroxide
titrant, two grams of sodium hydroxide pellets were dissolved in water.

2. With the aid of a laboratory technician, the titration set-up was established and the
general start-up procedures for the experiment were performed. With all exiting valves
closed, the reactor tank was filled with NaOH and Et(Ac) solutions, with both their flow
rates initially adjusted to 30 ml/min. Both solutions were allowed to flow through the
reactor and overflow into the waste tank. Then, the stirrer motor was switched on, with
 the speed set to around 200 rpm to ensure homogenous water jacket temperature. The
system was allowed to reach steady-state conditions before the sampling was done.

3. For trial 1, samples were taken from the sampling point of the equipment about every
five minutes by measuring 10mL of the product and they were added to the flask
containing 10mL of HCl solution to quench the saponification reaction. A few drops of
pH indicator were added into the mixture. The mixture with NaOH solution was
titrated from the burette until the mixture was neutralized or became slightly pink. The
amount of NaOH titrated was recorded. The sample collection was continued until
steady state condition was attained.

4. For trial 2, the flow rate of ethyl acetate was adjusted to 50 ml/min, while keeping the
flow rate of sodium hydroxide the same. The sampling procedures were repeated until
steady state condition was obtained.

5. For trial 3, the flow rate of the NaOH was now adjusted to 50 ml/min while the flow rate
of ethyl acetate was brought to its original lower value. The sampling procedures were
repeated.

6. For the last trial, which was done to meet the second objective of this experiment, the
system was operated at two different temperatures in order to get two values of reaction
constants at two different temperatures. The flow rates were set back to the values in
trial 1 and the collection of samples continued at the same interval of time.

7. After the experiment, before the spent solution was drained, it was first properly
neutralized to avoid environmental contamination.

Results

Reactor Volume: 0.400 L

Molarity of NaOH: 0.05 M

Molarity of Ethyl Acetate: 0.05 M

Flow rate (L/min) Residence Time Overall

Trial
Ethyl acetate Sodium Hydroxide (min) Conversion

1 0.03 0.03 6.666666667 0.33

Residence Reaction Rate
2 Temperature
0.03 0.05 Overall 5.000 Reaction Rate
0.288333333
Trial Time Constant
(K) Conversion (L-mol/min)
3 0.05 (min) 0.05 4.000
(L/mol-min) 0.255

1 298.15 6.666666667 0.33 1.47761194 0.00165825

Table 3.1 Calculated Values of Overall Conversion at Varying Residence Times
2 298.15 5.000 0.03 1.620608899 0.00205197

3 298.15 4.000 0.05 1.711409396 0.00237469

4 313.15 6.666666667 0.328 1.955334988 0.00222222

Reaction Rate
lnK Temperature (T) 1/T
Constant (K)
1.47761194 0.3904272305 Constants298.15 0.003354016
TableTable 3.3 Reaction
3.2 Plot of OverallRate and Reaction
Conversions versus Rates
Residence Times
1.955334988 0.6705615281 313.15 0.003193358

Gas Constant Activation Energy

Slope (-E/R)
(J/mol-K) (J/mol)
Table 3.4 Data for Determination of Activation Energy
0.8 8.3145 -1743.7 14,497.99
0.7
0.6 f(x) = 0.28 x − 0.17
R² = 1
0.5
0.4
lnK

0.3
0.2
0.1
0
0.5 1 1.5 2 2.5 3 3.5
1/T

Plot of lnK versus 1/T Linear (Plot of lnK versus 1/T)

Figure 3.1 Plot of lnK versus 1/T

0.35
0.3
0.25
CONVERSION

0.2
0.15
0.1
0.05
0
0.5 1 1.5 2 Residence
2.5 3
Time, 3.5
MIN 4 4.5 5 5.5
 Figure 3.2 Plot of Overall Conversions versus Residence Times

Calculations

 Residence Time

For flow rates of 30 ml/min:

Reactor volume ( L ) ,V
τ=
Residence Time, L
Total flow rate ( )
min
, v0

Total flow rate, Vo = Flow rate of NaOH + Flow rate of Et(Ac)

= 30 mL/min NaOH + 30 mL/min Et(Ac)

= 60 mL/min

= 0.06 L/min

Hence,
0.4 L
Residence Time, τ = = 6.6667 min
0.06 L /min
Other residence times were calculated using the same process.

 Conversion

For flow rates of 30 ml/min:

Moles of reacted NaOH, n1,

n1= Concentration NaOH x Volume of NaOH titrated

= 0.05 M x 0.0031 L

= 0.000155 moles

Moles of unreacted HCl, n2,

Moles of unreacted HCl = Moles of reacted NaOH

 n2 = n1

n2= 0.000155 moles

Volume of unreacted HCl, V1,

n2
V 1=
concentration HCl quench
0.000155
=
0.05
= 0.0031 L

Volume of HCl reacted, V2,

V2= Total volume HCl – V1

= 0.01 – 0.0031

= 0.0069 L

Moles of reacted HCl, n3,

n3= Concentration HCl x V2

= 0.05 x 0.0069

= 0.000345 mole

Moles of unreacted NaOH, n4,

n4 = n3

= 0.000345 mole

Concentration of unreacted NaOH,

n4
CNaOH unreacted =
volume sample
0.000345
=
0.01
= 0.0345 M
Concentration of NaOH unreacted
Xunreacted =
concentration NaOH
0.0345
=
0.05
= 0.69

Xreacted = 1 - Xunreacted
 = 1 - 0.69

= 0.31

Conversion for flow rate 30 mL/min

0.31x 100% = 31 %

Hence, at flow rate 30 mL/min of NaOH in the reactor, about 31% of NaOH is reacted

with Et(Ac). Other conversions were calculated using the same process.

 Reaction Rate Constant, k

v0 X
k= (
V TFR C AO 1−X )
For flow rates of 30 ml/min:

V0 = Total inlet flow rate

= 0.06 L/min

VTFR = Volume for reactor

= 0.4 L

CAO = inlet concentration of NaOH

= 0.05 M

X = 0.31

0.06 0.31
k= (
(0.4)( 0.05) 1−0.31 )
= 1.3478 L/min-mol

Other Reaction Rate Constants were calculated using the same process.

 Rate of Reaction, -rA

-rA = k (CA0)2 (1-X)2

For flow rates of 30 ml/min:

-rA = (1.3478) (0.05)2 (1-0.31)2

= 1.60 x 10-3 mol-L/min

Other Rate of Reactions were calculated using the same process.

Conclusion

From the experiment, students were able to determine reaction rate constant at a given
temperature using a plug flow tubular reactor. The reaction is in 2nd order using the data
gathered from the experiment. Therefore, from the graph that had been plotted, we can say that
the conversion factor is inversely proportional to the residence time at certain point then a small
changes an increase of graph conversion to the residence time .

Literature Cited

Experiments in Chemical Engineering, 2nd Edition by Servillano S.B Olaño, Jr