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EXPERIMENT

DETERMINATION OF REACTION ORDER AND REACTION CONSTANT USING BATCH


AND CSTR SETUP

OBJECTIVES

At the end of this exercise, the students should be able to:


1. Calibrate the pumps
2. Determine the ionic conductivities using batch and continuous reaction
3. Differentiate Batch and Continuous reactor
4. Determine order of reaction and reaction constant
5. Plot conductivity vs time

LIST OF CHEMICALS/MATERIALS

 0.1M Ethyl Acetate  water


 0.1M NaOH

LIST OF APPARATUS AND SET-UP

 250-ml Graduated cylinder  Conductivity meter


 500-ml Graduated cylinder  Stop watch/Timer
 Continuous Stirred Tank Reactor

Agitation
system
Conductivity
meter
Heating
system

Reagents
inlet

Figure 1. Continuous Stirred Tank Reactor

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DETERMINATION OF REACTION ORDER AND REACTION CONSTANT USING
BATCH AND CSTR SETUP

SAFETY PRECAUTIONS

Avoid skin contact with the reagents specially ethyl acetate. Inhalation of the
vapors for long periods of time should be avoided. Skin contact should likewise be limited.
Spills should be dispersed on paper toweling immediately and the toweling removed at
once to the fume hood for evaporation of the liquid.

INTRODUCTION

In chemical engineering, there are various equipment that had been used to
improve the production of different products from raw materials (Moncada, Lopez, &
Marin, 2015). One common equipment are reactors which chemical engineers usually
design. There are many types of reactors like Batch Reactor, Continuous Stirred Tank
Reactor (CSTR), Plug Flow Reactor (PFR), Semi-batch Reactor and Catalytic Reactor. In
this research, we will focus on one reactor which is the CSTR. CSTRs are one of the most
used chemical reactors since it can be easily operated under steady conditions of
temperature, pressure and compositions (Moncada, Lopez, & Marin, 2015). The feed or
reactant is continuously added in the tank and there is also a continuous output flow in
the process (Benitez, Bermudez, &Rodriguez-Calo, 2017). Also, the exit stream has the
same conditions as those inside the tank. The nature of its flow is better for certain
reactions because it provides “smoothing” of time fluctuation of reactants or product to
aid process control (Jones, Taşkin, & Yianneskis, 2009).

Due to the characteristics of above, CSTRs are generally modeled by considering


that there are no variations in concentration, temperature, or reaction rate throughout
the vessel. The temperature and the concentration of the exit stream are identical
everywhere within the reactor. A simple diagram of CSTR is shown in Figure 2 (Fogler,
2004).

Reactants
Products

Figure 2. Continuous-stirred tank reactor.

Applying the general mole balance equation, defined in Eq. 1, to a CSTR at


steady state (i.e., there is no change in the conditions with time or no accumulation),
𝑉
𝑑𝑁𝑗
𝐹𝐽0 − 𝐹𝑗 + ∫ 𝑟𝑗 𝑑𝑉 =
𝑑𝑡 Eq. 1
𝑉𝑜
Where,
𝐹𝐽0 - rate of flow of j into the system (moles/time)

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DETERMINATION OF REACTION ORDER AND REACTION CONSTANT USING
BATCH AND CSTR SETUP

𝐹𝑗 - rate of flow of j out of the system (moles/time)


𝑑𝑁𝑗
- rate of accumulationof j within the system (moles/time)
𝑑𝑡

𝑉
∫𝑉 𝑟𝑗 𝑑𝑉 - rate of generation of j by chemical reaction within the
𝑜
system (moles/time)

At steady state,
𝑑𝑁𝑗
=0 Eq. 2
𝑑𝑡

There is no variation in the rate of reaction,


𝑉

∫ 𝑟𝑗 𝑑𝑉 = 𝑉𝑟𝑗 Eq. 3
𝑉𝑜

By substituting the Eq. 2 and Eq.3 in the general mole balance, the design
equation for a CSTR will be derived and defined as,

𝐹𝐽0 − 𝐹𝑗
𝑉= Eq. 4
−𝑟𝑗

In terms of conversion, xj,

𝐹𝑗 = 𝐹𝐽0 ( 1 − 𝑥𝐽 )
Eq. 5
𝐹𝐽0 𝑥𝐽
𝑉= Eq. 6
−𝑟𝑗
In liquid phase,
𝐹𝐽0 = 𝐶𝐽𝑜 𝑣𝑜 Eq. 7

Where, 𝐶𝐽𝑜 , is the initial concentration (mole/volume).


Substituting Eq.7 to Eq. 6,
𝐶𝐽𝑜 𝑣𝑜 𝑥𝐽
𝑉= Eq. 8
−𝑟𝑗

The design equation will be able to give the volume of the reactor needed to
reduce the entering flow rate of species, 𝐹𝐽0 , and the exit flow rate, 𝐹𝐽 (Fogler, 2004).
Space time, Ʈ, is the time necessary to process one reactor volume of fluid based
on entrance conditions. For constant density systems, space time is equal to the
residence time. It is defined as:
𝑉
Ʈ= Eq. 9
𝑣𝑜

Where, 𝑣𝑜 is the flowrate (volume/time). By rearranging Eq.8,


Eq. 10
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DETERMINATION OF REACTION ORDER AND REACTION CONSTANT USING
BATCH AND CSTR SETUP

𝑉 𝐶𝐽𝑜 𝑥𝐽
=
𝑣𝑜 −𝑟𝑗

Therefore,
𝐶𝐽𝑜 𝑥𝐽
Ʈ= Eq. 11
−𝑟𝑗

PROCEDURE

I. DETERMINATION OF IONIC CONDUCTIVITY IN A BATCH REACTION

Chemicals and Laboratory Apparatus:


 250 ml of 0.1M NaOH
 250 ml of 0.1M Ethyl Acetate
 CSTR unit
 Conductivity meter
 Timer

Procedure:
1. Switch ON the unit and the software
2. Place 250 ml of 0.1M NaOH inside the tank/reactor
3. Add 250 ml of 0.1M Ethyl Acetate and immediately turn on the stirrer and set it to
100% agitation rate.
4. Place the conductivity meter after the last drop of ethyl acetate and record the
initial conductivity.
5. Record the conductivity every 20 seconds for 30 minutes.

II. CALIBRATION OF THE PERISTALTIC PUMPS

Chemicals and Laboratory Apparatus:


 Water
 CSTR unit
 250 ml graduated cylinder
 Stop watch

Procedure:
1. Fill up the two reagent bottles with 1L of water each
2. Fill the tank with 500 mL water
3. Activate AB-2 pump and set it to 100%
4. Simultaneously record the time to fill up every 20 mL volume (20 mL, 40 mL, 60 mL,
80 mL and 100 mL)
5. Close AB-2 pump
6. Activate AB-3 pump and set it to 100%

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DETERMINATION OF REACTION ORDER AND REACTION CONSTANT USING
BATCH AND CSTR SETUP

7. Simultaneously record the time to fill up every 20 mL volume (20 mL, 40 mL, 60 mL,
80 mL and 100 mL)
8. Set AB-3 pump to other rate (about 70%-80%) until the flow rate of AB-3 is equal or
almost same as AB-2
9. This set-up will be the foundation for the next part.

III. DETERMINATION OF IONIC CONDUCTIVITY IN A CONTINUOUS REACTION

Chemicals and Laboratory Apparatus:


 6L of 0.1M NaOH
 6L of 0.1M Ethyl Acetate
 CSTR unit
 Empty discharge bottle
 Conductivity meter

Procedure:
1. Place the 6L Reagents at the back of the set-up and place the tubes in their
respective places.
2. Add 50 ml of water in the tank and use this to prime the pumps. Make sure that
both valves are open.
3. If the bubbles are completely purged out, activate the pumps with the set-up from
the previous experiment. The pumps must be at equal flow rates.
4. Place the conductivity meter and record the conductivity from the first reading
and every after 5 seconds. Note that you can use camera to take a video of the
conductivity meter and record it later.
5. Place an empty discharge 15L bottle at the end of the overflow tube.
6. Record the conductivity for 1 and a half hour.
7. Plot the recorded conductivity vs time

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