Plug Flow Reactor Report
Aim and Objective
1. To study the saponification reaction between Ethyl Acetate and Sodium Hydroxide in a helical
tubular reactor.
2. To obtain reaction kinetics parameters of Saponification reaction at different temperatures.
3. To observe the effect of flow rate and Temperature on the conversion of saponification
reaction.
Materials:
0.08 M NaOH solution, 0.08 M Ethyl Acetate solution, 0.1 N HCl solution
Utilities:
Conductivity meter, Coil type tubular reactor, Hot water bath, Rotameters, Temperature sensors,
Stopwatch, Measuring beaker.
Theory:
The saponification reaction can be represented by the following chemical reaction:
Neglecting the backwards reaction and considering equimolar reactant feed, the rate equation
for this second-order reaction reduces to the following form:
The design equation of a PFR then becomes:
Which on integrating further simplifies to:
Arrhenius equation for the rate constant:
Kinetics of saponification reaction:
The kinetics study of this experiment consists of the following:
(i) Determination of the rate constant at T = 40°C, 50°C, and 60°C
(ii) Determination of the activation energy
(iii) Determination of the frequency factor or (pre-exponential) factor
By applying the performance equations of an ideal CSTR to the experimental data, the above
parameters can be determined. Temperature affects the rate through the Arrhenius equation.
Experimental Procedure
1. Set at desired temperature the constant temperature bath.
2. Adjust the rotameter readings so that an equal molar flow rate of both reactants enters
the reactor.
3. 196 mL of ethyl acetate added to 20 L of distilled water produces a 0.1 N solution, and
80 g of NaOH pellets added to 20 L of distilled water produces a 0.1 N solution.
4. Collect product samples in a flask when the steady state is reached.
5. Dip the probe in the flask and measure the conductivity of the solution and its actual
temperature.
6. Repeat the run at 3 different temperatures (40°C, 50°C, and 60°C).
7. Repeat for other flow rates at a given temperature. This will generate data of Reynolds
number vs. conversion.
8. After the last run, pipette out the reactor contents and allow distilled water to flow
through the rotameter and reactor for a few minutes.
Description:
The helical tubular reactor is kept in a constant temperature bath where the temperature is
maintained through a heater and controller setup. The feeds are pumped through rotameters
and a mixing Tee. There is also a stirrer in the hot water bath to maintain a uniform temperature
throughout. The product sample is collected from the outlet.
Analysis Methodology and Sample Calculation
Conductivity Method:
Normality of the NaOH in the fresh feed = 0.06 N
Normality of CH₃COONa in the fresh feed = 0.06 N
Since both of the feed was taken in equal volumetric flow rate:
Normality of NaOH in the reactant stream = 0.06 N / 2 = 0.03 N
Normality of CH₃COONa in the reactant stream = 0.06 N / 2 = 0.03 N
Now, the experiment has been performed at 40 °C, 50 °C and 60 °C but calibration data in the
lab is available for 31 °C, 42 °C and 52 °C. Reference I states that in our relevant range
conductivity varies linearly with temperature and concentration (for low concentration). We also
find that the conductivity of NaOH (0.1 N) and CH₃COONa (0.1 N) varies linearly with
temperature with the following relation:
Where ttt is the temperature in °C. Similarly, conductivity of the NaOH (0.03 N) and CH₃COONa
(0.03 N) at a given temperature ttt can be estimated in the following way:
For example, let's consider the case of 55 °C:
The conversion of the reaction can be related with the conductivity of the sample using the
following relation:
Observation Table
Sample Calculation for K:
For 60 C,
Slope = 6.02, i.e. (1/KCo)= 6.02
K = 1/(6.02 •0.04•60) = 0.092
Similarly, at 50° C, K = 0.0208 and at 40° C, K = 0.0418
Activation Energy Calculation
Slope = E/R = 3996.26 => Activation energy, E= 3996.26*8.314 J/mol = 33.224 kJ/mol
-ln(A) = -15.2569 => Pre exponential factor, A = 4.22*10^7
Scaling laws
● −ln (k) vs 1/T scales in such a way that on increasing temperature, k (rate constant) will
decrease.
● Keeping the flow rate fixed, X (conversion) increases with an increase in temperature.
● Keeping the temperature fixed, X (conversion) decreases with an increase in flow rate.
● Electrical conductivity decreases with an increase in temperature at a fixed flow rate.
● The concentration of the reactant decreases with time as the product is formed.
● As the volumetric flow rate increases, the residence time decreases, and theoretically,
conversion should decrease and the concentration of NaOH inthe sample should
increase. Hence, conductivity values are expected to increase for a given temperature
with an increase in flow rate, which is observed.
Summary:
At three different temperatures (40°C, 50°C and 60°C), rate constants k were estimated as:
0.6034, 0.1337 and 0.0877 L/(mol·s), respectively.
The activation energy for the saponification reaction of ethyl acetate: 33.224 kJ/mol.
The rate equation is
Sources of Error:
1. Since the conductivity meter reading continuously changed whenever it was dipped in a
sample solution. The reasons could be (a) deviation from reactor temperature outside the
reactor where reading is taken, and (b) insufficient time given to the conductivity meter to reach
a stable value. (c)Reaction proceeds towards completion once outside the reactor.
2. Since conductivity readings were taken outside the reactor at room temperature. 1he
temperature of the solution might change, impacting the expected conductivity values.
Moreover, the reaction will proceed when the solution is taken outside the reactor. Hence,
conductance values do not truly represent the concentration inside the reactor.
3. Conductivity meter takes time to show a stable reading, but given the instructions. It could not
be allowed to achieve stable reading.
4. The set level of the rotameter reading frequently deviated, and it had to be adjusted.
