Republic of the Philippines

EASTERN VISAYAS STATE UNIVERSITY

Tacloban City

Laboratory Report in ChE 512L

CHEMICAL ENGINEERING LABORATORY II

by

DANDAN, Kester M.

MACAPAÑAS, Kecie

MANDIA, Fiona N.

SABLAN, Carlo James Q.

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 engineering, when contrasted with other engineering programs, is the lone program
that tackles the course Chemical Reaction Engineering. This is an area where chemical engineers
play important roles, especially in the design, operation, and maintenance of industrial plants
that involve chemical reactors (Olaño, 2000). Apparently, there are many types of reactors, and
one of the most commonly used reactors in industry are plug flow tubular reactors.

A plug flow tubular reactor is a pipe-shaped tank where a chemical reaction takes place, with
walls coated with a catalyst and an inlet flow of pure reactant. It is normally operated at steady
state, as is the CSTR (Morbos et. al, 2016). A simple illustration of a typical plug flow reactor is
shown below:

Figure 3.1. Schematic diagram for a plug flow reactor (Olaño, 2000)

Plug flow tubular reactors are utilized in a huge variety of different applications. This necessitates
for an intensive study on its mechanism and working principles. With the help of this experiment,
students were able to test a laboratory size plug flow tubular reactor to determine the design
parameters associated with the kinetics of a liquid phase second order reaction, particularly the
saponification of ethyl acetate (EtAc) with dilute sodium hydroxide (NaOH), at different
operating flow rates and temperatures.

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

Table 3.1 Calculated Values of Overall Conversion at Varying Residence Times

Flow rate (L/min) Residence Time Overall
Trial
Ethyl acetate Sodium Hydroxide (min) Conversion

1 0.03 0.03 6.666666667 0.33

2 0.03 0.05 5.000 0.288333333
3 0.05 0.05 4.000 0.255
 0.35
0.3
0.25

CONVERSION
0.2
0.15
0.1
0.05
0
0 2 4 6 8
RESIDENCE TIME, MIN

Figure 3.2 Plot of Overall Conversions versus Residence Times

Table 3.2 Reaction Rate Constants and Reaction Rates

Residence Reaction Rate
Temperature Overall Reaction Rate
Trial Time Constant
(K) Conversion (L-mol/min)
(min) (L/mol-min)

1 298.15 6.666666667 0.33 1.47761194 0.00165825

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

Table 3.3 Data for Determination of Activation Energy

Reaction Rate
lnK Temperature (T) 1/T
Constant (K)
1.47761194 0.3904272305 298.15 0.003354016

1.955334988 0.6705615281 313.15 0.003193358

0.8
0.7
0.6
0.5
y = -1743.7x + 6.2387 Plot of lnK versus
lnK

0.4
R² = 1 1/T
0.3
0.2 Linear (Plot of lnK
0.1 versus 1/T)
0
0.003150.00320.003250.00330.003350.0034
1/T

Figure 3.3 Plot of lnK versus 1/T

 Table 3.3 Data for Determination of Activation Energy

Gas Constant Activation Energy

Slope (-E/R)
(J/mol-K) (J/mol)

8.3145 -1743.7 14,497.99

Discussion

The results were outlined based on the suggested chronology of presentation provided in the
Analyses and Calculations sections of the laboratory manual.

Initially, Table 3.1 displays the calculated values of overall conversions at varying residence
times. Varying the residence time was made possible by adjusting the inlet flow rates of the
reactants. It has to be noted that that the overall conversion is the mean of the fractional
conversions computed for each

Calculations

 Residence Time

For flow rates of 30 ml/min:

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

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,
0.4𝐿
Residence Time, 𝜏 = 0.06 𝐿/𝑚𝑖𝑛
= 6.6667 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
V1= 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,

𝑛
CNaOH unreacted = 𝑣𝑜𝑙𝑢𝑚𝑒 4𝑠𝑎𝑚𝑝𝑙𝑒
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= ( )
𝑉𝑇𝐹𝑅 𝐶𝐴𝑂 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. Also, activation energy of the reaction was
calculated, having a value of 14,497.99 J/mol. The reaction is in 2nd order using the data gathered
from the experiment.

Literature Cited

Any information borrowed from another source which is not common knowledge must
be cited within the text but listed (with full citation). It should be on a separate final
page of the report.

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