Experiment no.

ISOTHERMAL REACTION IN A PLUG FLOW TUBULAR 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.

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) = 𝐹𝐴
𝑂𝑢𝑡𝑝𝑢𝑡 𝑜𝑓 𝐴 𝑚𝑜𝑙𝑒𝑠⁄𝑡𝑖𝑚𝑒) = 𝐹𝐴 + 𝐷𝐹𝐴
𝐷𝑖𝑠𝑎𝑝𝑝𝑒𝑎𝑟𝑎𝑛𝑐𝑒 𝑜𝑓 𝐴 𝑚𝑜𝑙𝑒𝑠⁄𝑡𝑖𝑚𝑒) = (−𝑟𝐴 )𝑑𝑉

Substituting these values,

𝐹𝐴 = (𝐹𝐴 + 𝐷𝐹𝐴 ) + (−𝑟𝐴 )𝑑𝑉

Objectives

The experiment was conducted to achieve the following objectives:

1. To determine the reaction rate constant at a given temperature using a plug flow
tubular reactor.
2. To determine the activation energy of a reaction.
3. To determine the order of reaction using experimental data from a tubular 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

Part I. Preparation of Feed solutions, blank solution and titrant

1. 0.05M Ethyl Acetate. 20 Liters of 0.05M Ethyl Acetate solution was prepared by
diluting concentrated EtAc to de-ionized or distilled water and then placed to tank
B. Precautionary measures was observed while preparing the solution since the
liquid is very volatile and flammable and should be kept away from naked lights.
2. 0.05M Caustic Soda. 40 grams of Sodium hydroxide flakes was weighed dissolved
in water and then diluted to 20 Liters of de-ionized or distilled water. The solution
was placed in tank A enough for several experiments. Wearing PPE such as googles
and gloves was observed.
3. 0.05M Hydrochloric Acid. 2 Liters of 0.05m HCl solution was prepared by diluting
concentrated HCl to de-ionized water.
4. Preparation of 0.02M NaOH Titrant. 2 grams of NaOH pellets was dissolved in 1
Liter of water.
 5. Standardization of 0.02M NaOH Titrant. Add 1 to 2 drops of phenolphthalein
indicator and titrate with prepared NaOH titrant until a permanent light pink color
appears.

Part II. Varying Flow Rate

1. The equipment was first operated at room temperature. The temperature was
recorded.
2. For Run 1, the rotameter valves was adjusted to make the flowrates of the reactant
equal.
3. Samples of the reaction product was collected about every 5 to 10 min. by measuring
10 mL of the product and immediately adding this to a flask containing a blank of 10
mL of HCl solution whose concentration is high enough to eliminate the NaOH in
the reacting mixture. The mixture was titrated.
4. For Run 2, the flow rate of the other reactant was increased by 50 to 100% and the
sampling procedure was repeated until steady state condition is obtained.
5. For Run 3, the flowrate of the other reactant was increased so as to get the different
residence times compared to the previous runs.

Part III. Determination of Arrhenius Constants

1. The flow rates was set at the same value as Run 1 of Part II.
2. The system was operated at two other temperatures

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

0.35
0.3
0.25
CONVERSION

0.2
0.15
0.1
0.05
0
 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

Table 3.3 Data for Determination of Activation Energy
4 313.15 6.666666667 0.328 1.955334988 0.00222222

Reaction Rate
lnK Temperature (T) 1/T
Constant (K)
1.47761194 0.3904272305 298.15 0.003354016
0.8
1.955334988 0.6705615281 313.15 0.003193358
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

Calculations

Conclusion

Literature Cited