ABSTRACT

The experiment aims to study the saponification reaction of sodium hydroxide an ethyl acetate in
a Plug Flow REACTOR (PFR) , both sodium hydroxide and ethyl acetate were prepared
according to the given volume and concentration before transferred to the tanks , When the
process starts, the conductivity was recorded in every minute for 20 minutes When the liquid
level in the PFR reached 690ml, the space time as well as conductivity was recorded, Then, all
valves and pumps were closed, and all liquid will be discarded through valve V4 the time goes
once the experiment starts, the conductivity values should gradually close up its value to the
conductivity value of pure product that is determined before the reaction starts. The conversion
should gradually increase as the time goes by the time goes once the experiment starts, the
conductivity values should gradually close up its value to the conductivity value of pure product
that is determined before the reaction starts. The conversion should gradually increase as the
time goes by. The errors and recommendations also were discussed in the discussion section. The
conclusion section concludes all the objectives and calculations on this experiment.

INTRODUCTION

Chemical reactors are integral to a vast array of industrial processes, playing a crucial role in the
synthesis of chemicals, pharmaceuticals, and materials. Among the various types of reactors, the
Plug Flow Reactor (PFR) is particularly significant due to its high efficiency in handling
continuous chemical processes. Unlike other reactors, such as the Continuous Stirred-Tank
Reactor (CSTR), the PFR operates with reactants flowing unidirectional through a cylindrical
pipe without back-mixing. This unique flow pattern ensures that the reactants progress
sequentially, with each infinitesimal volume of the reactor experiencing identical conditions.

Importance of Isothermal Conditions

In the context of chemical reactions, maintaining isothermal conditions—where the temperature

remains constant throughout the reactor—ensures that the reaction kinetics can be studied
without the interference of temperature fluctuations. Temperature plays a pivotal role in
influencing reaction rates, as it directly affects the kinetic energy of molecules. By ensuring a
constant temperature, the kinetic parameters, such as the rate constant (k), can be accurately
determined. This is critical for the design and optimization of industrial reactors, as precise
control over reaction conditions can lead to enhanced efficiency, reduced energy consumption,
and improved product yields.

Reaction Mechanisms
The chemical reaction chosen for this study is the saponification of ethyl acetate with sodium
hydroxide. This reaction is a classic example in chemical engineering education due to its well-
defined kinetics and straightforward reaction mechanism. The saponification reaction can be
represented by the following equation:

NaOH +CH 3 COO C 2 H 5 →CH 3 COONa+C 2 H 5 OH

where sodium hydroxide ( NaOH ) reacts with ethyl acetate (CH3COOC2H5) to produce sodium
acetate (CH3COONa) and ethanol (C2H5OH). This reaction is generally a second-order
reaction, where the rate of reaction depends on the concentration of both reactants. Studying this
reaction in a PFR under isothermal conditions provides valuable insights into the kinetics and
behavior of the reaction, which can be extrapolated to other industrial processes.

Understanding the isothermal operation of a PFR and accurately determining the rate constant
(𝑘) are of paramount importance for optimizing industrial chemical processes. Accurate kinetic
data allows for the design of reactors that maximize efficiency, minimize energy consumption,
and optimize product yields. Furthermore, the insights gained from this study are applicable to a
wide range of chemical reactions and industrial applications, enhancing the overall efficiency
and sustainability of chemical manufacturing processes. The ability to predict and control
reaction outcomes under isothermal conditions is essential for the development of scalable and
economically viable industrial processes. This detailed introduction provides a comprehensive
foundation for the subsequent sections of the report, which will cover the experimental
procedure, results, discussion, and conclusions.

Objectives
 To practically demonstrate the operation of PFR reactor.
 To determine the value of the rate constant using a tubular reactor.

Theory
The rate at which a given chemical reaction proceeds can be expressed in several ways. It can be
expressed either as the rate of disappearance of the reactants, or the rate of formation of products,
In the following reaction:
NaOH +CH 3 COO C 2 H 5 →CH 3 COONa+C 2 H 5 OH
A and B are the reactants, while C and D are the products. a, b, c, d are the stoichiometric
coefficients for the respective species. If species A is considered as the reaction basis, then the
rate of reaction can be represented by the rate of disappearance of A. It is detonated by the
symbol −r A . The numerical value of the rate of reaction −r A is defined as the number of moles
of A reacting per unit time per unit volume, and has the typical unit of mol/dm3.s.

The rate expression can be shown to be −r A k a b

where if ais equal to bthis simplifies to −r A k a 2
The rate constant can be determined using the CET MkII Tubular Reactor.
We can show that:
Xa
kt a μ=
1−X a

To calculate the reaction rate constant (k) for the saponification reaction:
The overall mass balance around the CSTR will be applied:
Input quantity = output quantity + reacted quantity + accumulated quantity
F A 0 = F A 0 (1− X a) + (−r A )V

Rearranging the equation:

F A 0 X a=(−r A )V

Where F A 0 ( molar feed rate )=a 0 v

2
F A 0 X a=k . a tV

V
Remember that τ =space time=
v

Rearranging the last equation:

v a 0−at
k= ( 2 )
V at

where:

v = total volumetric flow rate = v A +v B

V = the volume of the reactor

a 0 = initial concentration of NaOH at input entrance of CSTR

a t= the concentration of NaOH at a certain time (t)

  To calculate the concentration of NaOH and CH 3 COONa at time (t):

a t=( a∞ −a0 )
( ʎ 0 −ʎ t
ʎ 0 −ʎ ∞)+ a0

ʎ 0−ʎ t
c t =c ∞ ( )
ʎ 0−ʎ ∞

a 0−a t
X a=( )
a0

Where X ais conversion of NaOH

 To find the concentration of product c ∞ (CH 3 COONa ):

 If b 0 <a 0 c ∞ =b0
 If b 0 ≥ a0 c ∞ =a0
 To find the concentration of product a ∞ (NaOH):
 If a 0< b 0 a ∞=0
 If a 0 ≥ b 0 a ∞=a 0−b 0

 To calculate the conductivity of the reacted mixture:

ʎ 0=ʎ a 0=0.195 ( 1+0.0184 (T −294 ) ) a 0

ʎ ∞ =ʎ a ∞ + ʎ c ∞

ʎ a ∞ =0.195 ( 1+0.0184 ( T −294 ) ) a∞

ʎ c ∞=0.195 ( 1+ 0.0184 ( T −294 ) ) c ∞

Where:

va
a 0=( )a
vt μ

vb
b 0=( )b
vt μ
Apparatus and materials:

 DESCRIPTION:

In an ideal Plug Flow Reactor (PFR) there is no mixing in the direction of flow and complete
mixing perpendicular to direction of flow. Concentration of reactants varies along the length of
reactor but not in radial direction. In case of a coil turbulence is introduced due to frequent
change in direction of flow and presence of secondary flow, so a higher value of reaction rate
constant is expected in coil tube type plug flow reactor. This set-up is used to study a non-
catalytic homogeneous reaction under isothermal condition. The set up consists of two feed tanks
through which two reactants are fed to the reactor. Rotameters are provided to measure the
individual flow of Chemicals. The flow rate can be adjusted by operating the needle valves
provided on respective Rotameter. The compressed air is used for circulation of feed. It is a
helical coil tube type reactor kept in a constant temperature water bath to conduct the experiment
at various temperatures. Reactants enter at lower end coming out of the top of coil from where
samples are collected for analysis. Pressure Regulator, Pressure Gauge and Safety Valve are
fitted in the compressed air line.

 Scope of study:

 Saponification Reaction study in Isothermal Plug Flow Reactor.

 To determine Reaction Rate Constant and effect of temperature on it.

 Apparatus

 Reactor: Material Stainless Steel, Capacity.

 Water Bath: Material Stainless Steel, Double wall, insulated with Ceramic Wool.
 Heater.
 Stirrer (Water Bath).
 Feed Tank.
 Feed Circulation: By Peristaltic Pump.
 Piping: Stainless Steel and Silicon Pipe.
 Temp. Sensor.
 Conductivity meter.
 Conductivity meter

 Materials

 Sodium hydroxide
 Ethyl acetate
 Distilled water

Procedure
 preparing Ethylene Acetate and Sodium Hydroxide at 0.03 M in volume of 2 liters.
 measuring the conductivity of solutions using a conductivity measurement device.
 Draining the diluted solutions into the running actuators, respectively, and making sure
the keys for the actuators are open.
 Waiting until the first operator is filled with the solution (until the solution reaches the
sensitive) then turning on the stopwatch and calculating the conductivity every minute.
 recording the readings until the operators reach a stable state.
 Find the size of the operator in the traditional way by emptying the solution in a small
tube.

Calculations and Results

a μ=0.03 b μ=0.03
And
v a=1.268 v b =0.499 v t =1.767 T = 296.2 K° V = 0.41 L

So that

( 1.268
a 0=
1.767 )
( 0.03 )=0.0215 mol /l

( 0.499
b 0=
1.767 )
( 0.03 )=0.0085 mol /l

a 0< b 0 so that:

a ∞=a 0−b 0=0.0215−0.0085=0.013 mol/l

c ∞ =b0=0.0085 mol/l

ʎ 0=ʎ a 0=0.195 ( 1+0.0184 ( 296.2−294 ) ) ( 0.0215 )=0.0044 sei

ʎ a ∞ =0.195 ( 1+0.0184 ( 296.2−294 ) ) ( 0.013 )=0.00264 mol /l

ʎ c ∞=0.195 ( 1+ 0.0184 ( 296.2−294 ) ) ( 0.0085 )=0.00172 mol/l

ʎ ∞ =0.00264+ 0.00172=0.0034 mol/l

a t=( 0.013−0.0215 ) ( 0.0044−ʎ t

0.0044−0.0034)+ 0.0215

0.0215−at
X a=( )
0.0215

1.767 0.0215−at
k= ( 2
)
410 at

−r A k a 2t

F A 0=a0 v a
 F A 0=( 0.0215 )( 1.268 )=0.02726 mol /s

Time ʎt at Xa K −r A −r A F A 0 /−r A

(min) (msiem) (mol /l) (l/mol . s ) ¿ ¿)
       
       
       
       
       
       
       
       
       
       
       
       
       
       
       
       
       
       
       
       

𝑋𝑎 vs 𝐹𝐴0/−𝑟𝐴

0
-1000
-2000
-3000
-4000
-5000
-6000
-7000
-8000
-9000
9 7 5 2 3 7 5 6 1 9 4 9 2 5 6 6 7 6 4 1
81 83 59 34 76 57 66 91 32 80 41 01 70 46 18 98 90 32 74 58
1.8 1.3 1.0 0.8 0.6 0.5 0.4 0.3 0.3 0.2 0.2 0.2 0.1 0.1 0.1 0.0 .07 .06 .04 .03
- - - - - - - - - - - - - - - - -0 -0 -0 -0

X a VS F A 0 /−r A

Area under the curve is calculated to be = 0.240 L

So that:
V 0.410
space time τ = = =1.71 S
v 0.240

DISCUSSION
In this work hydrolysis of ethyl acetate was investigated experimentally in a Plug Flow reactor to
determine the significant process parameters using statistical experimental design. In the
screening experiment, two variables: NaOH initial concentration and ethyl acetate initial
concentration were found to be significant operating parameters for the hydrolysis of ethyl
acetate. To obtain maximum conversion, optimum values of the initial concentrations of sodium
hydroxide and ethyl acetate were determined to be 0.03 mol/L.
Notice an increase in conversion over time, and this is due to the end of the reactants and the
formation of products. It is clear that there is an error in this experiment due to the presence of
illogical results in many of the values, one of these results is that the concentration of sodium
hydroxide at a certain time was always greater than its initial concentration. This is illogical,
because it will lead to negative results for the concentration values, and thus negative results for
the reaction rate constant. The total area under the curve also showed a negative value. There
may be an error in the calculation the Thermal conductivities. Perhaps the reason is due to the
presence of human errors when conducting the experiment, the lack of correct calibration of the
device, or the failure to take readings correctly.

CONCLUSION
By conducting this experiment, we learned to observe the concept and how the PFR works, as
well as determine the value of the reaction constant K during the saponification of ethyl acetate.
We explained how to calculate k through mathematical equations as well as through a graph, and
we also explained the effect of speed on the conversion rate. The reaction was studied in order to
improve observation and gain experience in reaction engineering, especially PFRR. Our results
were inaccurate in this process, and we explained the reasons in the discussion.

RECOMMENDATIONS
The titration process must be done slowly in order to achieve the best results. as well as adding
the two titrated solution quickly to each other to avoid any errors that may occur. Lastly,
recording the conductivity quickly as possible.