Determination of Effect of Feed Flow Rate on the Conversion in a

Continuous Stirred Tank Reactor (CSTR)

Abstract

This experiment is carried out in order to understand how the continuous stirred- tank reactor
(CSTR) system is working and to study the saponification reaction of sodium hydroxide and ethyl
acetate as well as to know the effect of different flow rates. CSTR is used primarily for liquid
phase reactions and normally operated at steady state with the assumption of ideal mixing. In this
experiment, the conductivity calibration curve is obtained to be reference for calculating
conversion from the measured conductivity by varying feed rate into the reactor between sodium
hydroxide and ethyl acetate. Other than that, the significance of doing this experiment is to
determine residence time from the data obtained in addition to study the effects of feed flow rate.
The experiment is conducted through specific steps, before all, setting the apparatus and preparing
the solution of sodium hydroxide and ethyl acetate as required comes first then plotting the
calibration curve and obtaining the general mathematical equation to calculate the conversion at
different flow rates and conductivities. From the obtained conversion and the recorded time,
different graphs can be plotted such as conductivity-conversion, conversion-time or conversion-
residence graphs at flow rate of 30rpm, 40rpm and 50rpm.

Introduction

Continuous Stirred Tank Reactor (CSTR) is a reaction vessel particularly used in a liquid phase
where reactants are continuously added and products are withdrawn while the contents are
assumed perfectly mixed and at steady state. The inlet and outlet streams inside of the reactor must
be more reachable than any other reactors. The inlet streams will bring all the reactants in at
particular rate and this stream will flow into a larger container where there is a shaft with a stirrer
attached in the reactor that rotates around continuously to mix the reactants. Consequently, there
is no time dependence or position dependence of the temperature, the concentration or the reaction
rate inside the CSTR. In other words, the concentration and temperature is the same at every point
inside the reactor therefore, the temperature and concentration in the exit stream are modeled as

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being the same as those inside the reactor. This is an extremely helpful and important point because
otherwise, in systems where mixing is not ideal, we would not know the concentration of the exit
stream using a well-mixed model and would have to resort to the other methods, such as residence
time distribution to obtained meaningful results.

CSTRs can be used both alone and in series, depending on the specific requirements of a chemical
process. A standalone CSTR is used when a continuous, well-mixed reaction environment is
sufficient for the desired process whereas series configurations are often employed when a more
intricate control of reaction parameters is needed, or when different stages of a reaction require
distinct conditions. In industrial settings, the selection of reactor configurations is based on
optimizing the overall efficiency, yield and selectivity of the desired product.

This experiment was carried out to study the saponification reaction between sodium hydroxide
and ethyl acetate in a CSTR. Saponification is a process whereby the triglycerides are reacted with
sodium or potassium hydroxide to produce glycerol and a fatty acid salt, called 'soap' although the
end product here is not soap. There are so many studies available in the literature on the process
improvement for this saponification reaction.

CSTRs are widely used in industrial processes such as in the production of chemicals,
pharmaceuticals and biochemical. CSTR does not require much work to keep it running and due
to its simplicity of the components involved in the reactor, the maintenance is easy and cheap.
However, this reactor takes more space to mix the component compare to other reactor. In reactor
design, we have the exact size and type of reactor as well as the method of operation that suitable
for a given job. This may require the conditions in the reactor vary with the position and time.

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Theory

The CSTR is a widely employed reactor type in chemical engineering, characterized by continuous
mixing of reactants within a well-mixed, constant-volume vessel. The reactor operates under
steady-state conditions, allowing a continuous inflow of reactants and outflow of products. As a
result, there is no time or position dependence of the temperature, concentration or reaction rate
inside the reactor. Therefore, all variables are the same at any point within the reaction vessel.

Residence Time

Residence time refers to the average time a reactant spends within the reactor. It is a critical
parameter influenced by the feed flow rate. Higher flow rates result in shorter residence times,
affecting the extent of reaction completion.

𝒓𝒆𝒂𝒄𝒕𝒐𝒓 𝒗𝒐𝒍𝒖𝒎𝒆
𝑹𝒆𝒔𝒊𝒅𝒆𝒏𝒄𝒆 𝒕𝒊𝒎𝒆 =
𝒇𝒍𝒐𝒘 𝒓𝒂𝒕𝒆

Conversion

Conversion represents the fraction of reactants that have been transformed into products. It is a
key performance metric for assessing the efficiency of a chemical reaction. The experiment aims
to quantify how variations in feed flow rate impact the overall conversion within the CSTR.

Consider a general reaction: 𝒂𝑨 + 𝒃𝑩 → 𝒄𝑪 + 𝒅𝑫

where the uppercase letters represent chemical species and the lowercase letters represent
stoichiometric coefficients (moles). Suppose that species A were to be the limiting reagent:

𝒃 𝒄 𝒅
𝑨+ 𝑩→ 𝑪+ 𝑫
𝒂 𝒂 𝒂

For CSTR reactor, the conversion of chemical species A is simply the number of molar flow rates
of A that have reacted per molar flow rates of A fed into the system.

𝒎𝒐𝒍𝒂𝒓 𝒇𝒍𝒐𝒘𝒓𝒂𝒕𝒆 𝒐𝒇 𝑨 𝒓𝒆𝒂𝒄𝒕𝒆𝒅 𝑭𝑨𝑶 − 𝑭𝑨

𝑿𝑨 = =
𝒎𝒐𝒍𝒂𝒓 𝒇𝒍𝒐𝒘𝒓𝒂𝒕𝒆 𝑨 𝒇𝒆𝒅 𝑭𝑨𝑶

The general mole balance equation for the above reaction is:

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 𝑽
𝒅𝑵𝑨
𝑭𝑨𝑶 − 𝑭𝑨 + ∫ 𝒓𝑨 𝒅𝒗 =
𝟎 𝒅𝒕

Assumption taken for an ideal CSTR is:

𝑑𝑁𝐴
1. Steady state, =0
𝑑𝑡
𝑉
2. Perfectly mixed, ∫0 𝑟𝐴 𝑑𝑣 = 𝑟𝐴 𝑉

Therefore, the general mole balance equation is reduced to the design equation of the CSTR:
𝑭𝑨𝑶 − 𝑭𝑨 + 𝒓𝑨 𝑽 = 𝟎

𝑭𝑨𝑶 − 𝑭𝑨
𝑽=
−𝒓𝑨

Saponification

Saponification is the hydrolysis of an ester under basic conditions to form an alcohol and the salt
of a carboxylic acid and it is commonly used to refer to the reaction of a metallic alkali with a fat
or oil to form soap. Thus, the hydrolysis of ethyl acetate (CH3OOC2H5) by sodium hydroxide
(NaOH) to produce sodium acetate (CH3COONA) and ethanol (C2H5OH) is saponification
reaction although the end product is not soap.

The ethyl acetate molecules split into acetate ions and ethanol molecules, consuming hydroxide
ions provided by the sodium hydroxide in the process. The progress of the reaction can thus be
tracked accurately by the change in hydroxide ions. This can be observed by the conductivity
change in the reactor vessel, since the presence of hydroxide ions increase the conductivity in a
solution.

Objectives

The objective of this experiment is to:

 plot calibration curve and develop mathematical equation;

 determine the conversion achieved by varying feed rate into the CSTR reactor;
 calculalte the residence time.

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Materials and Methods

Apparatus used:

 Balance
 Beaker
 Computer controlled CSTR reactor (QRCAC)
 Measuring cylinder
 Pipette
 Portable conductivity meter
 Pump
 Volumetric flask

Chemicals used:

 Distilled water
 Ethyl acetate, CH3COOC2H5
 Sodium hydroxide, NaOH

Solution Preparation:

To prepare a 1L of 0.05M sodium hydroxide and 0.05M ethyl acetate solution, we should first
calculate the mass of NaOH and volume of CH3COOC2H5 required.

For sodium hydroxide solution:

 Molarity= 0.05mol/L
 Molecular weight= 40g/mol
 Volume of solution= 1L
 Purity= 97%

𝑚𝑜𝑙𝑎𝑟𝑖𝑡𝑦 × 𝑣𝑜𝑙𝑢𝑚𝑒 × 𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 0.05 × 1 × 40

𝑚𝑎𝑠𝑠, 𝑚 = = = 2𝑔
𝑝𝑢𝑟𝑖𝑡𝑦 0.97

Therefore we prepare the solution measuring 2g NaOH and dissolving it in 1L distilled water.

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For ethyl acetate solution:

 Molarity= 0.05mol/L
 Molecular weight= 88.11g/mol
 Volume of solution= 1L
 Purity= 99%
 Density= 0.901g/mL
𝑚𝑜𝑙𝑎𝑟𝑖𝑡𝑦 × 𝑣𝑜𝑙𝑢𝑚𝑒 × 𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 0.05 × 1 × 88.11
𝑣𝑜𝑙𝑢𝑚𝑒, 𝑣 = = = 5𝑚𝐿
𝑑𝑒𝑛𝑠𝑖𝑡𝑦 × 𝑝𝑢𝑟𝑖𝑡𝑦 0.901 × 0.99

Therefore we prepare the solution by adding 5mL ethyl acetate to 995mL of distilled water to
prepare 1L solution.

Experiment Procedure:
1. A reagent solution of 1L of 0.05M ethyl acetate and 1L of 0.05M sodium hydroxide was
prepared.
2. The QRC unit with a QRCAC reactor was started.
3. A working temperature of 250C was set through the whole experiment.
4. The products outlet stainless steel tube was placed as low as possible so that the product
can be easily discharged without stop.
5. For both reagents, a 30rpm flow rate was set.
6. At the moment when the reaction mixture touches the conductivity cell, the conductivity
was recorded.
7. The stirrer was started when the reactant level reaches the stirrer’s blades.
8. The conductivity at the product outlet was measured every minute interval until reagents
completely flow in to the reactor vessel.
9. When all the reagents flow out, the system was stopped.
10. The experiment was repeated at a feed rate of 40rpm and 50 rpm.

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Result

From Experiment 1 on the manual, we can plot the calibration curve and develop a mathematical
equation that relates conductivity and conversion.

Figure 1: Calibration Curve

From the mathematical equation we develop from the calibration plot, we can calculate the
conversion from the measured conductivity and plot Conductivity vs. Conversion.

For 30 rpm:

Conductivity, 3.58 3.94 4.20 4.35 4.44

mS/cm
Conversion, 1.4 41.85 63.34 73.14 78.19
%

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 Figure 2: Conductivity vs. Conversion for 30rpm

For 40rpm:

Conductivity, 3.72 4.17 4.58 4.67 4.82

mS/cm
Conversion, 18.72 61.16 84.87 88.47 93.33
%

Figure 3: Conductivity vs. Conversion for 40rpm

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For 50rpm:

Conductivity, 3.93 4.32 4.75 4.78 5.18

mS/cm
Conversion, 40.91 71.32 91.23 92.17 99.90
%

Figure 4: Conductivity vs. Conversion for 50rpm

To plot Conversion vs. Time, conductivity was measured every 1 minute interval until the solution
in the reactor finished for 30rpm, 40rpm and 50rpm flow rates.

Time, sec 0 60 120 180 240

30rpm Conversion, % 1.40 41.85 63.34 73.14 78.19

40rpm 18.72 61.16 84.87 88.47 93.33

50rpm 40.91 71.32 91.23 92.17 99.90

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 Figure 5: Conversion vs. Time for different flow rates

To plot a Conversion vs. Residence time curve, we first have to calculate the residence time from
the recorded volume and time.

For 30rpm:

V, mL Time, sec ∆V ∆t Flow rate, L/sec

1000 0 100 46.5 0.0022
900 46.5 100 55 0.0018
800 101.5 100 50 0.0020
700 151.5 100 50.5 0.0020
600 202 75 35 0.0021
525 237 - - -
Average flow rate= 0.002 L/sec

𝑟𝑒𝑎𝑐𝑡𝑜𝑟 𝑣𝑜𝑙𝑢𝑚𝑒 1𝐿
𝑅𝑒𝑠𝑖𝑑𝑒𝑛𝑐𝑒 𝑡𝑖𝑚𝑒, 𝜏 = = = 500𝑠𝑒𝑐
𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 0.002𝐿/𝑠𝑒𝑐

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For 40rpm:

V, mL Time, sec ∆V ∆t Flow rate, L/sec

1000 0 100 35 0.0029
900 35 100 44.5 0.0022
800 79.5 100 41.5 0.0024
700 121 100 34 0.0029
600 155 45 30 0.0015
555 185 - - -

Average flow rate= 0.0024 L/sec

1𝐿
𝑅𝑒𝑠𝑖𝑑𝑒𝑛𝑐𝑒 𝑡𝑖𝑚𝑒, 𝜏 = = 416.67𝑠𝑒𝑐
0.0024𝐿/𝑠𝑒𝑐

For 50rpm:

V, mL Time, sec ∆V ∆t Flow rate, L/sec

1000 0 100 36.5 0.0027
900 36.5 100 36.5 0.0027
800 73 100 35 0.0029
700 107.5 90 24 0.0038
610 131.5 - - -

Average flow rate= 0.003 L/sec

1𝐿
𝑅𝑒𝑠𝑖𝑑𝑒𝑛𝑐𝑒 𝑡𝑖𝑚𝑒, 𝜏 = = 333.33𝑠𝑒𝑐
0.003𝐿/𝑠𝑒𝑐

At maximum conversion, the solution starts to pour out from the reactor. So now we can plot the
graph from the residence time calculated above at maximum conversion.

Residence time, sec Conversion, %

50rpm 333.33 99.90

40rpm 416.67 93.33
30rpm 500 78.19

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 Figure 6: Conversion vs. Residence time

Discussion

The conductivity of the reaction mixture changes with conversion and therefore the extent of the
reaction can be monitored by recording the conductivity with respect to time. A calibration curve
is needed to relate conductivity data to concentration values. From Figure 1, we can see that order
4 polynomial function best fits the curve. Using the developed mathematical equation, we
calculated the conversions for 30rpm, 40rpm and 50rpm from the measured conductivity. Figure
2, 3 and 4 shows conductivity vs. conversion curves for 30rpm, 40rpm and 50rpm respectively.
From the result obtained, we can see that as the pump speed increases, both the conversion and
conductivity are increasing for same time interval.

Conductivity of the solution was measured every minute interval after the liquid started dropping,
so from that we plotted easily conversion vs. time curve. The conversion was found from the
mathematical equation and the time interval was same for the three different flow rates. Figure 5
shows that as pump speed increases, the conversion also increases with respect to time.

Finally, to plot the conversion vs. residence time curve, we first needed to calculate the residence
time using the equation t=V/vo. In our experiment, residence time is the average time for the
processing of the feed in one liter reactor volume measured at specific condition that is 250C. It is

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related to the reactor volume and the volumetric flow rate, the reactor volume is known while flow
rate is calculated from the recorded data of volume and time. From Figure 6, we can observe that
as residence time increases, conversion decreases. Generally, when the pump rotation increases,
residence time decreases while conversion increases.

Conclusion

The aim of this experiment was to investigate the influence of operating conditions on the
conversion. The parameters considered for analysis were temperature, feed flow rate, residence
time and volume of reactor. Calibration curve helps to get a general mathematical equation that
can relate conductivity with conversion using different software, in our case we use Excel to
generate the mathematical equation and plot all the curves.

From this experiment, the conversion for the 30rpm, 40rpm and 50rpm are 0.7819, 0.9333 and
0.999 respectively. In the meantime, the residence time for each volumetric flow rate are 500s,
416.67s and 333.33s respectively. It can be concluded that the smaller the flow rate, the higher the
residence time of the reactant in the reactor, the higher the conversion. A CSTR system operates
in such a way that the reactant conversion, X would have some fluctuation during the start-up and
would reach a relatively constant value over time, indicating that the CSTR attained steady state.

The results obtained in this experiment may be helpful in maximizing the conversion of ethyl
acetate saponification reaction at industrial scale in a CSTR.

Reference

https://public.websites.umich.edu/~elements/6e/asyLearn/bits/cstr/index.htm

https://www.coursehero.com/file/25573793/Lab-CSTR-40Ldocx/

http://wwwresearch.sens.buffalo.edu/karetext/unit_21/learning/21_Info.pdf

https://www.vssut.ac.in/images/chemical-lab/laboratory-pdf/Chemical-Reaction-Engineering-lab-
manuals.pdf

https://www.coursehero.com/file/68199470/Saponification-of-Ethyl-Acetate-and-Sodium-Hydroxide-in-
CSTR-Lab-reportpdf/

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