CHE331: Unit Operations and Process Control

Laboratory
Experiment No. 03

Name of the Experiment Plug Flow Reactor

Date of the Experiment 14/09/24

Date of Submission 03/09/24

Group No. 2

Students’ Details Name Roll No.

Ajay Singh 220090

Adarsh Pal 220054

Abhishek Maurya 220047

Akansha Ratnakar 220093

Kaushalendra Singh 220511

Objective:
1. To study the reaction between ethyl acetate and sodium hydroxide in a tubular reactor.
2. To study the effect of axial dispersion on the conversion in a tubular reactor.

Theory:
The reaction between ethyl acetate and sodium hydroxide is represented as (assuming second
order, irreversible reaction)

Plug flow reactor design equation:

The residence time τ is also:

Now the flow through the reactor may be either (a) Laminar or (b) turbulent, according to
whether the Reynolds number, NRe

is less or greater than approximately 2000, where ρ and μ are the density and viscosity of the
solution (essentially water) flowing through the reactor, dt is the internal diameter of the tube and
u is the mean velocity in the tube.
A graph between NRe and conversion of reactant can be plotted.

(a) For Laminar Flow, the velocity profile is parabolic in shape; the mean exit conversion of
NaOH is given by

Where,

ā1 = Mean outlet molal concentration of NaOH

a1 = Outlet molal concentration of NaOH

(b) For Turbulent flow, the velocity profile is not too for removed from being flat in shape
(i.e. Plug flow). The Exit concentration of NaOH is given by

where, a1 = Outlet molal concentration of NaOH

Equations (9) and (10) assume a second order irreversible constant volume reaction. Provided
plug flow exists and there is no radial or longitudinal diffusion of reactants in the liquid and the two
reactant inlet flow rates are always in a constant ratio to each other, it may also be shown
that

Dispersion Model:

Where CAp is the concentration of the plug flow reactor with the same τ or L as the real reactor.
Levenspiel and Bischoff have given the graphical solution for second order reactions having equal
concentration. In this graph, conversion based on the dispersion model is a function of dispersion
number.
Line Diagram:

Equipment/ Apparatus:
● Coil type tubular reactor (0.5 cm ID) and 0.9 meter long
● Constant Temperature Bath
● Rotameters for flow measurement of ethyl acetate and sodium hydroxide solutions.
● Sodium Hydroxide and ethyl acetate solutions (0.05N)
● Conductivity Meter
5. 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 enter
the reactor.
3. The density of ethyl acetate is 0.898 gm/ml at 25oC and its Molecular Weight is 88.
Hence 10 ml of ethyl acetate added to 2030 ml of distilled water produces a 0.05 N
solution.
4. Collect product samples in a flask when the steady state is reached.
5. Analyze the samples and find the concentration of reactant by analyzing the sample by
titration.
6. Repeat the run at 3 different temperatures (40oC, 50oC and 60oC)
7. Repeat for other flow rates at a given temperature. This will generate data of Reynolds
no. vs conversion.
8. After the last run, pipette out the reactor contents and allow distilled water to flow
through the rotameters and reactor for a few minutes.

Observations:

Conversion, XA = (CO - Ct)/(CO - CINF)

Temperature Flow Conductivity (in mS/cm)

Rate (in Ct avg (in XA
L/h) mS/cm)
t = 10 t = 12 t = 14
mins mins mins
60 oC 5+5 3.8 3.82 3.78 3.8 0.882

10 + 10 4.82 4.69 4.70 4.74 0.768

50 oC 5+5 4 4.02 4.12 4.05 0.852

10 + 10 4.96 4.75 4.9 4.87 0.751

40 oC 5+5 4.76 4.7 4.7 4.72 0.770

10 + 10 4.9 5 4.58 4.83 0..757

Sample Calculation:

Inner Diameter of Reactor: 0.5 cm

Length of the Reactor: 0.9 m
 𝑫𝟐
Now, Volume of the Reactor: 𝝅 ∗ 𝟒
∗ 𝒉 = 𝟎. 𝟎𝟏𝟕𝟔 𝒍
@ Temperature = 600C
Using the PFR equation
𝒙𝑨
𝒅𝒙𝑨
𝝉 = 𝑪𝑨𝑶 ∫ 𝟐 (𝟏
𝟎 𝒌𝑪𝑨𝑶 − 𝒙𝑨 )𝟐
Also,
CAO = 11mS/cm, and CINF = 2.84 mS/cm
Now, conversion (XA)
𝟏𝟏 − 𝑪
𝑿𝑨 =
𝟏𝟏 − 𝟐. 𝟖𝟒

We get XA = 0.882, as C = CAVG = = (3.8 + 3.78 + 3.82)/ 3 =3.8 mS/cm

Also,
𝑽 0.0001 0.9 𝟎. 𝟐𝟏𝟐
𝝉= = 3.14 ∗ 0.5 ∗ 0.5 ∗ ∗ ∗ 60 = = 𝟎. 𝟏𝟎𝟔 𝒎𝒊𝒏
𝑽𝒐 4 5 𝟐

Now, using PFR equation

𝑿𝑨
𝒌= = 𝟐𝟑. 𝟓𝟗 𝑳𝒎𝒐𝒍−𝟏 𝒔𝒆𝒄−𝟏
(𝟏 − 𝑿𝑨 ) ∗ 𝑪𝑨𝑶 ∗ 𝝉

Now, calculating NRE

𝒅 0.9 0.01
𝑵𝑹𝑬 = 𝝆 ∗ 𝒗 ∗ = 898 ∗ ∗ 0.5 ∗ = 𝟔𝟕𝟗. 𝟕𝟎𝟖
𝝁 0.212 0.000935
Here, I have used the expression
𝑳
𝒗=
𝝉

Now, since NRE < 2000, we have the laminar flow

Now, used the above equation to calculate k (real) on calculation we get using the MATLAB
code attached at the bottom.
k(real) = 16.25 Lmol-1sec-1

Now, below are the attached figures, at temperature = 333 kelvin

Arrhenius Plot
 ln(k) VS 1/T
3.4

3.3

3.2

3.1
ln(k)

2.9

2.8
y = -2386.4x + 10.474
2.7 R² = 0.8259
0.00295 0.003 0.00305 0.0031 0.00315 0.0032 0.00325
1/T

Fig.1

Now, from the above figure we can say that,

𝑬𝑨
= 𝟐𝟑𝟖𝟔. 𝟒, 𝑡ℎ𝑒𝑟𝑒𝑓𝑜𝑟𝑒
𝑹
𝒌𝑱
𝑬𝑨 = 𝟏𝟗. 𝟖𝟒𝟎
𝒎𝒐𝒍𝒆
Now, pre-exponential factor ko = exp(10.474) Lmol-1sec-1 = 35.383 Lmol-1sec-1

X vs Conductivity

X(conversion)
0.900
0.880
0.860
X(conversion)

0.840
0.820
0.800
0.780
0.760
y = -0.1225x + 1.348
0.740
0 1 2 3 4 5 6
Conductivity
 Fig.2

Fig.3

Questions:
● What are the assumptions involved in the derivation of the dispersion model?

1. Steady-State Operation: The system is considered to operate in steady-state,

meaning concentration and flow profiles do not change with time.

2. Negligible Axial Dispersion: Axial mixing is assumed to be minimal, allowing the

fluid elements to travel distinctly through the reactor.

3. Perfect Radial Mixing: Complete mixing occurs in the radial direction, ensuring
uniform concentration across the reactor's cross-section.

4. Constant Physical Properties: Properties like density and viscosity are assumed to
remain constant throughout the reactor.

5. Negligible Mass Transfer Resistance: External mass transfer limitations are

considered insignificant, focusing solely on internal reactor dynamics.

6. Defined Reaction Kinetics: Reactions typically follow second-order kinetics, though

other forms can be used as applicable.

● Why dispersion model is important to study the performance of the Plug Flow Reactor?
Accounts for Non-Ideal Flow: It models deviations from ideal plug flow by considering axial
dispersion, leading to more realistic predictions.

• Improves Conversion Predictions: Incorporating dispersion helps in accurately predicting

reactant conversion rates under non-ideal conditions.

• Optimizes Reactor Design: It aids in refining reactor design for better efficiency and
performance by understanding flow dynamics.

• Crucial for Scale-Up: The model ensures reliable scaling up from laboratory to industrial
reactors by addressing flow irregularities.

• Enhances Process Safety: Understanding dispersion contributes to safer reactor operation by

allowing better control over reaction conditions.

• Improves Operation Control: It helps fine-tune operating parameters to minimize the

negative effects of dispersion on reactor performance...

● What are the sources of error in evaluation of dispersion number and conversion?
• Inaccurate Measurement Techniques: Errors in conductivity or concentration measurements
can lead to incorrect conversion and dispersion values.
 • Non-Ideal Flow Conditions: Deviations from ideal plug flow, such as channeling or stagnant
zones, can distort dispersion assessments.

• Temperature and Flow Rate Fluctuations: Variations in temperature or flow rates affect
reaction rates and dispersion, causing inaccurate results.

• Incorrect Kinetic Assumptions: Assuming incorrect reaction kinetics can lead to errors in
conversion predictions.

• Human Errors: Mistakes in titration, data recording, or experimental setup can introduce
significant inaccuracies.

• Sampling Errors: Improper sampling techniques may result in unrepresentative data,

affecting both conversion and dispersion evaluations.

Nomenclature:
● a0 = Inlet molal concentration of NaOH
● a1 = Outlet molal concentration of NaOH
● ā1 = Mean outlet molal concentration of NaOH
● CA = Molar Concentration of NaOH
● CA0 = Molar concentration of NaOH at initial conditions
● CB = Molar Concentration of Ethyl Acetate
● dt = Diameter of Tube
● D = Axial dispersion coefficient for flowing fluid (m²/s)
● DAB = Diffusivity of ethyl acetate in water, (m²/s)
● FA0 = Initial molar flow rate of A (moles/s)
● k = Arrhenius Constant
● L = Reactor Length (m)
● MB = Molecular weight of the solvent, kg/kmol
● NRe = Reynolds Number
● NSc = Schmidt Number
● n0 = Inlet molal flow rate of either reactant
● n1 = Exit molal flow rate of ethyl acetate
● rA = Rate of reaction (moles/m³s)
● T = Temperature (K)
● u = Velocity of Fluid (m/s)
● Q = Volumetric flow rate (m³/s)
● V = Volume of reactor (m³)
● XA = Conversion of reactant A
Matlab Code

% Given parameters

X_avg = (0.750+.757)/2; % Example value for conversion (X bar)

a0 = 0.05; % Example value for initial concentration (mol/L)

tau = 0.212*60; % Example value for residence time (s)

% Define the function for the equation to solve for k

f = @(k) X_avg - (k*a0*tau - (k^2 * a0^2 * tau^2 / 2) * log((2 + k*a0*tau) / (k*a0*tau)));

% Use fsolve to find the root of the equation (k)

k_initial_guess = 2.0; % Initial guess for k

k = fsolve(f, k_initial_guess);

% Display the result

disp(['The value of k is: ', num2str(k)]);

For Dispersion coefficient and Raynold’s number

%% Clear previous data

clc;
clear all;

%% Constants
tube_diameter = 0.5 * 10^(-2); % Diameter of the tube in meters
tube_length = 0.9; % Length of the tube in meters
density_fluid = 0.898 * 10^3; % Density of fluid in kg/m^3
viscosity_60C = 0.935 * 10^(-3); % Viscosity at 52°C in Pa.s
viscosity_50C = 0.683 * 10^(-3); % Viscosity at 42°C in Pa.s
viscosity_40C = 0.3668 * 10^(-3); % Viscosity at 32°C in Pa.s
initial_conc_A = 0.05; % Initial solute concentration

%% Flow rates and velocities

flow_rate_5lph = (10 * 10^(-3)) / 3600; % Convert 5+5 L/h to m^3/s
flow_rate_10lph = (20 * 10^(-3)) / 3600; % Convert 10+10 L/h to m^3/s

% Velocity for 5+5 L/h and 10+10 L/h

velocity_5lph = flow_rate_5lph / ((pi * tube_diameter^2) / 4); % Velocity at 5+5 L/h
velocity_10lph = flow_rate_10lph / ((pi * tube_diameter^2) / 4); % Velocity at 10+10
L/h
%% Reynolds number calculation for each temperature
% For 60°C
Reynolds_60_5lph = (density_fluid * velocity_5lph * tube_diameter) / viscosity_60C;
Reynolds_60_10lph = (density_fluid * velocity_10lph * tube_diameter) / viscosity_60C;

% For 50°C
Reynolds_50_5lph = (density_fluid * velocity_5lph * tube_diameter) / viscosity_50C;
Reynolds_50_10lph = (density_fluid * velocity_10lph * tube_diameter) / viscosity_50C;

% For 40°C
Reynolds_40_5lph = (density_fluid * velocity_5lph * tube_diameter) / viscosity_40C;
Reynolds_40_10lph = (density_fluid * velocity_10lph * tube_diameter) / viscosity_40C;

%% Mass transfer coefficient calculation

% Using an integral function for mass transfer
mass_transfer_fun = @(x_A) 1./(1 - x_A).^2; % Defining the function for integration

% Dimensionless concentration XA for each case (use the provided data)

Xa_60_5lph = 0.882;
Xa_60_10lph = 0.768;
Xa_50_5lph = 0.852;
Xa_50_10lph = 0.751;
Xa_40_5lph = 0.770;
Xa_40_10lph = 0.757;

% For 60°C and 5+5 L/h

integral_60_5lph = integral(mass_transfer_fun, 0, Xa_60_5lph);
mass_transfer_60_5lph = (integral_60_5lph * Reynolds_60_5lph * viscosity_60C) / ...
(initial_conc_A * density_fluid * tube_diameter * tube_length);

% For 60°C and 10+10 L/h

integral_60_10lph = integral(mass_transfer_fun, 0, Xa_60_10lph);
mass_transfer_60_10lph = (integral_60_10lph * Reynolds_60_10lph * viscosity_60C) /
...
(initial_conc_A * density_fluid * tube_diameter * tube_length);

% For 50°C and 5+5 L/h

integral_50_5lph = integral(mass_transfer_fun, 0, Xa_50_5lph);
mass_transfer_50_5lph = (integral_50_5lph * Reynolds_50_5lph * viscosity_50C) / ...
(initial_conc_A * density_fluid * tube_diameter * tube_length);

% For 50°C and 10+10 L/h

integral_50_10lph = integral(mass_transfer_fun, 0, Xa_50_10lph);
mass_transfer_50_10lph = (integral_50_10lph * Reynolds_50_10lph * viscosity_50C) /
...
(initial_conc_A * density_fluid * tube_diameter * tube_length);

% For 40°C and 5+5 L/h

integral_40_5lph = integral(mass_transfer_fun, 0, Xa_40_5lph);
mass_transfer_40_5lph = (integral_40_5lph * Reynolds_40_5lph * viscosity_40C) / ...
(initial_conc_A * density_fluid * tube_diameter * tube_length);

% For 40°C and 10+10 L/h

integral_40_10lph = integral(mass_transfer_fun, 0, Xa_40_10lph);
mass_transfer_40_10lph = (integral_40_10lph * Reynolds_40_10lph * viscosity_40C) /
...
(initial_conc_A * density_fluid * tube_diameter * tube_length);

%% Dispersion Coefficient Calculation

% Assuming the dispersion coefficient is proportional to mass transfer and flow rate
dispersion_coeff_60_5lph = mass_transfer_60_5lph * velocity_5lph;
dispersion_coeff_60_10lph = mass_transfer_60_10lph * velocity_10lph;
dispersion_coeff_50_5lph = mass_transfer_50_5lph * velocity_5lph;
dispersion_coeff_50_10lph = mass_transfer_50_10lph * velocity_10lph;
dispersion_coeff_40_5lph = mass_transfer_40_5lph * velocity_5lph;
dispersion_coeff_40_10lph = mass_transfer_40_10lph * velocity_10lph;

%% Plotting the Dispersion Coefficient vs Reynolds Number

figure;
Reynolds_numbers = [Reynolds_60_5lph, Reynolds_50_5lph, Reynolds_40_5lph, ...
Reynolds_60_10lph, Reynolds_50_10lph, Reynolds_40_10lph];
dispersion_coeffs = [dispersion_coeff_60_5lph, dispersion_coeff_50_5lph, ...
dispersion_coeff_40_5lph, dispersion_coeff_60_10lph, ...
dispersion_coeff_50_10lph, dispersion_coeff_40_10lph];

plot(Reynolds_numbers, dispersion_coeffs, 'bo-', 'LineWidth', 2, 'DisplayName',

'Dispersion Coefficient');
xlabel('Reynolds Number');
ylabel('Dispersion Coefficient (D_L) [m^2/s]');
title('Dispersion Coefficient vs Reynolds Number');
legend;
grid on;