OBJECTIVES

The purposes of this Continuous Stirred Tank Reactor experiment are:

To determine the order of saponification reaction

To determine the reaction rate constant, k by plotting the graph

THEORY
For stirred tank reactor (STR), it may be operated either in batch or at a steady-state flow,
which it is better known as Continuous Stirred tank Reactor (CSTR). CSTR is a common
ideal reactor type in chemical engineering. It is also known as vat- or backmix reactor, often
refers to a model that is used to estimate the key unit operation variables. The key or main
feature of this reactor is that mixing is complete so that properties such as temperature and
concentration of the reaction mixture are uniform in all parts of the vessels. Material balance
of a general chemical reaction is described below:
The conversion principle in an element of reactor of a volume V requires that the mass of
species A obeys the following statement:
[ Rate of A into ] [ Rate of A out of ] + [ Rate of A produced ] = [
volume element

volume element

within volume element

Rate of A

accumulated within
volume element

Batch Stirred Tank Reactor (BSTR)

In batch reactions, there are no feed of exits streams and therefore the general equation can be
simplified into:
[Rate of A produced in volume element] [Rate of A accumulated in volume element]
The rate of reaction of component A is defined as:

-rA = 1
V

dNA
dt

= [moles of A appear by reaction] / [unit volume] [unit time]

by reaction

By this definition, if A is a reaction product, the rate is positive; whereas if it is a reactant

which is consumed, the rate is negative.
(- rA) V = NAO dXA
dt
t = NAO dXA
(-rA)V

Steady State Mixed Flow Reactor

The general material balance for this reactor is:
Input of A (moles/time) = FAO (1-XAO) = FAO
Output of A (moles/time) = FA = FAO ((1-XA)
Dissapearance of A by reaction (moles/time) = (-rA) V
FAO XA = (-rA ) V
V = = XA = XA
FAO

CAO

-rA

-rA

= 1 = V = VCAO = CAO XA
S

Vo

FAO

-rA

APPARATUS
Chemicals
HCL, NaOH, Ethyl Acetate and phenolphthalein.

Equipment Description:
(a) Reactor
The reactor consists of a glass vessel with top and bottom plate made of stainless steel.
The reactor comes with a coiling coil, a 1.0kW heater, a temperature sensor, stirrer
system, an overflow tube and a gas sparging unit.
(b) Feed Inlet System (Liquid Reactions)
For each liquid reactant, a 20 L feed tank, a pump, a needle valve and a flow meter
are provided. Each reactant is pumped from the feed tank to the appropriate inlet port
at the top plate
(c) Gas Inlet System (Gas-Liquid Reactions:Optional)
Gas from gas cylinder flows through a needle valve, a flow meter and a gas sparger
before reacting with the liquid inside the reactor.
(d) Product/Waste Tank
A 50L rectangular tank made of stainless steel is provided for collecting the product or
waste before being discharged.
(e) Control Panel
The control panel consists of all the necessary electrical components for controlling
the operations of the unit. Components mounted on the panel door are all labeled for
convenience. The control panel also houses the necessary modules for data acquisition
system
(f) Data Acquisition System (Optional)

The Data Acquisition System consists of a personal computer, ADC modules and
instrumentations for measuring the process parameters. A flow meter with 0 to 5 VDC
output signal is supplied for each feed stream. A temperature sensor and temperature
transmitter with 4 to 20 mA output signal is provided to measure the reaction
temperature. A pH sensor with controller are provided for monitoring the changes in
pH while the reaction is taking place. All analog signals from the sensors are converted
by the ADC modules into digital signal before being sent to the personal computer for
display and manipulation.

Figure 1: Continuous Stirred Tank Reactor Equipment

PROCEDURE
Experiment: Batch Reactor Experiment
Reactant Preparation Procedure
1. 0.05 M NaOH and 0.05 M Ethyl Acetate solutions is prepared in two separate 20
liter feed tanks.

2. The concentration of 0.1 M NaOH solution is to be confirmed by titrating a small amount

of it with 0.1 M HCl using phenolphthalein as indicator. The concentration of ethyl acetate
solution is evaluated by the following manner. First, 0.1 M NaOH solution is added to a
sample of the feed solution such that the 0.1 M NaOH solution is in excess to ensure all of the
ethyl acetate has reacted. This mixture is let to be reacting overnight. On the following day,
the amount of unreacted NaOH is determined by direct titration with standard 0.1 M HCl.
The ethyl acetate real concentration is then recorded.
3. 1 liter of quenching solution of 0.25 M HCl and 1 liter of 0.1 M NaOH is prepared for back
titration.
Batch Reaction Procedure
1. The overflow tube in the reactor is adjusted to give a desired working volume (2.5L). The
pump P1 is switched on and 1.25L of the 0.1M ethyl acetate is pumped from the feed tank
into the reactor. The pump P1 is stopped.
2. The pump P2 is switched on and 1.25L of the 0.05 M NaOH is pumped into the reactor.
The pump P2 is stopped when 2.5L volume is reached. The stirrer is switched on and the
speed is set to be 180 rpm. Immediately, the timing of the reaction is recorded.
3. 10mL of 0.25 M HCl is quickly measured in a flask
4. After 1 minute of reaction, the valve V7 is opened. 50mL sample is then collected and
added immediately to the 10mL of 0.25 M HCl prepared in step 3 and let to be mixed. The
HCl will quench the reaction between ethyl acetate and sodium hydroxide.
5. The mixture is then titrated with 0.1 M NaOH to evaluate the amount of unreacted HCl.
6. Steps 3 to 5 is repeated for reaction times 5,10,15,20 and 25 minutes