Study Effect of Feed Flow Rate on Plug Flow Reactor Conversion

Abstract

The experiment is carry out with the reaction of Sodium Hydroxide, NaOH and Ethyl Acetate,
Et(Ac) to determine the effect of feed flow rate on the plug flow reactor conversion of the
solution. This experiment is conducted using the Tubular Flow Reactor. NaOH and Et (Ac)
solution are fed into the reactor with the constant operating temperature and different flow rates.
The conductivity value is observed every minute interval until the process is stabilized. The
concentration of solution exiting the reactor and extent of conversion were recorded from the
calibration curve. The graph of the conversion against conductivity and conversion against
residence time were constructed. The result for this experiment is shown that the higher the flow
rate, the higher the conversion and the lower the conductivity and residue time.

Introduction

The chemical reactors are something that is crucial and important in a chemical industries. It is
the most important things as it is the place for the reaction to happen. The type of reactor must be
suited with the reaction that we seek for. One of the most common example of the reactors is
Plug Flow Reactor (PFR). Plug flow reactor or Tubular flow reactor is a pipe-shaped tank
where a chemical reaction takes place and the reactant would flow in an axial direction in the
shape of plug (cylindrical shape) as shown below in Figure 1. It consists of a cylindrical pipe and
is normally operated at steady state, as is the CSTR.

Figure 1: Simple Schematic of Plug Flow Reactor

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Plug flow reactors are an idealized scenario where there is no mixing involved in the reactor. It is
the opposite of the continuous-stirred tank reactor, where the reaction mixture is perfectly
mixed. It is impossible to have no mixing at all during a reaction, but the amount of mixing in the
reactor can be minimized. There are several advantages to minimizing the amount of mixing so
that the reactor closely resembles a PFR. The plug flow reactor has an inlet flow composed of the
reactants. The reactant flows into the reactor and is then converted into the product by a certain
chemical reaction. The product flows out of the reactor through the outlet flow.

Plug flow reactor are usually used for a large scale production, fast reactions and continuous
reaction. Besides that, high temperature reaction usually done in the PFR. This is because the
PFR can withstand the high temperature of a reaction. PFR have a high volumetric unit
conversion and can run for a long periods of time without maintenance. That is why it is widely
used in the manufacturing of chemicals.

In the chemical industry, plug flow reactors are frequently used due to the non-mixing property
of the reactors. This is because it would be more advantageous than a mixed reactor such as a
CSTR. Plug flow reactors are frequently used in biological reactions when the substrate flows
into the reactor and is converted to product with the use of an enzyme. Since plug flow reactors
have an inlet and outlet stream, they are useful for continuous production. The streams are
opposite of a batch reactor, which is a reactor that has a constant volume and has no incoming or
outgoing streams. Flow of plug flow reactor is laminar, as with viscous fluids in small-diameter
tubes, and greatly deviate from ideal plug-flow behavior, or turbulent, as with gases. One Plug
flow reactor is an ideal tubular reactor with laminar flow behavior. Turbulent flow generally is
preferred to laminar flow, because mixing and heat transfer are improved.

Objectives
The objectives of this experiment are:

1. To carry out the saponification reaction between NaOH and Et(Ac) in tubular flow reactor.
2. To convert conductivity to conversion using a calibration curve.
3. To determine the steady state conversion.
4. To determine the effect of flow rate on the conversion in the tubular flow reactor.

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Theory

Plug Flow Reactor (PFR) is one of the ideal reactor in industry. Many plants and company used
PFR as the site for their reactants to react in producing valuable desired product. This reactor
mainly famous for process that involves gas or fast reactions process. This is because, in PFR the
reactants are fed continuously and products are also continuously removed. PFR becomes
favorable because it is easy to maintain, as it does not have any moving parts. Additionally, the
most favorable reason is it has the highest conversion per reactor volume of flow reactor. In
designing and modelling a PFR, an ideal condition are assumed in order to ease the calculation.
The PFR behavior are assumed to be perfect mixing at all times without dead time occurs in any
corner or area in the PFR. This composition is a function of residence time and rate of reaction.

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, the
ideal PFR mole balance with assumptions can be written as follows:

𝑨𝒄𝒄𝒖𝒎𝒖𝒍𝒂𝒕𝒊𝒐𝒏 = 𝒊𝒏𝒑𝒖𝒕 − 𝒐𝒖𝒕𝒑𝒖𝒕 + 𝒈𝒆𝒏𝒆𝒓𝒂𝒕𝒊𝒐𝒏

𝒅𝑵𝑨 𝑽

= 𝑭𝑨𝟎 − 𝑭𝑨 + ∫ 𝒓𝑨 𝒅𝒗
𝒅𝒕 �

Assumption made:

1. In steady state condition, 𝑑𝑁𝐴 = 0 but only in the radial direction.

𝑑𝑡

2. No axial mixing.
3. For a flow system, 𝐹𝐴 can be given in terms of entering molar flow rate 𝐹𝐴0 and
the conversion, XA.

𝑭𝑨 = 𝑭𝑨𝟎 − 𝑭𝑨𝑶𝑿𝑨

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Thus, rearranging the equation would obtained this equation,

𝑭𝑨𝑶𝑿𝑨 = 𝑭𝑨𝟎 − 𝑭𝑨

𝑽
𝟎 = 𝑭𝑨𝑶𝑿𝑨 + ∫ 𝒓𝑨 𝒅𝒗
𝟎

−𝒓𝑨𝒅𝑽 = 𝑭𝑨𝑶𝒅𝑿𝑨

Therefore, the general mole balance equation is reduced to the design equation of the PFR:
𝑿𝑨
𝒅𝑿𝑨
𝑽 = 𝑭𝑨𝑶 ∫
𝟎 −𝒓𝑨

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
𝑹𝒆𝒔𝒊𝒅𝒖𝒆 𝒗𝒐𝒍𝒖𝒎𝒆
𝒕𝒊𝒎𝒆 =
𝒇𝒍𝒐𝒘 𝒓𝒂𝒕𝒆

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 (CH 3OOC2H5) by sodium
hydroxide (NaOH) to produce sodium acetate (CH3COONA) and ethanol (C2H5OH) is
saponification reaction although the end product is not soap.

𝐂𝐇𝟑𝐎𝐎𝑪𝟐𝐇𝟓 + 𝐎𝑯− + 𝑵𝒂+ → 𝑪𝑯𝟑𝑪𝑶𝑶− + 𝑵𝒂+ +

𝐂𝐇𝟑𝑪𝑯𝟐𝑶𝑯

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.

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Materials and Methods
Apparatus used:

🖙 Balance
🖙 Beaker
🖙 Conductivity meter
🖙 Measuring cylinder
🖙 Pipette
🖙 Pump
🖙 Stop watch
🖙 Tubular flow reactor
🖙 Volumetric flask

Chemicals used:

🖙 Distilled water
🖙 0.01M Ethyl acetate, Et (Ac)
🖙 0.01M Sodium hydroxide, NaOH

Solution Preparation:

To prepare a 1L of 0.01M sodium hydroxide and 0.01M ethyl acetate solution, we should first
calculate the mass of NaOH and volume of Et (Ac) required.

For sodium hydroxide solution:

🖙 Molarity= 0.01mol/L
🖙 Molecular weight= 40g/mol
🖙 Volume of solution= 1L
🖙 Purity= 99%

𝒎𝒐𝒍𝒂𝒓𝒊𝒕𝒚 × 𝒗𝒐𝒍𝒖𝒎𝒆 × 𝒎𝒐𝒍𝒆𝒄𝒖𝒍𝒂𝒓 𝟎. 𝟎𝟏 × 𝟏 ×

𝒎𝒂𝒔𝒔, 𝒘𝒆𝒊𝒈𝒉𝒕 𝟒𝟎 = 𝟎. 𝟒𝟎𝟒𝒈
𝒎= =
𝒑𝒖𝒓𝒊𝒕𝒚 𝟎. 𝟗𝟗

Therefore we prepare the solution measuring 0.404g NaOH and dissolving it in 1L distilled water.

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For ethyl acetate solution:

🖙 Molarity= 0.01mol/L
🖙 Molecular weight= 88.11g/mol
🖙 Volume of solution= 1L
🖙 Purity= 99%
🖙 Density= 0.901g/mL

𝒎𝒐𝒍𝒂𝒓𝒊𝒕𝒚 × 𝒗𝒐𝒍𝒖𝒎𝒆 × 𝒎𝒐𝒍𝒆𝒄𝒖𝒍𝒂𝒓 𝟎. 𝟎𝟏 × 𝟏 ×

𝒗𝒐𝒍𝒖𝒎𝒆, 𝒘𝒆𝒊𝒈𝒉𝒕 𝟖𝟖. 𝟏𝟏 = 𝟏𝒎𝑳
𝒗= =
𝒅𝒆𝒏𝒔𝒊𝒕𝒚 × 𝒑𝒖𝒓𝒊𝒕𝒚 𝟎. 𝟗𝟎𝟏 × 𝟎.
𝟗𝟗

Therefore we prepare the solution by adding 1mL ethyl acetate to 999mL of distilled water to
prepare 1L solution.

Experiment Procedure:

1. A reagent solution of 1L of 0.01M ethyl acetate and 1L of 0.01M sodium hydroxide was
prepared.
2. The TFR tank was filled with the prepared solutions in two separate tanks.
3. The interface was switched on and the QRC software was run.
4. The START button was pressed and the name of the file that will contain the data in the
new window was introduced.
5. A working temperature of 250C was set through the whole experiment.
6. An initial flow of 40rpm in the low range of the pumps was selected; so that both flows
of Et (Ac) and NaOH are the same.
7. The result obtained when the conductivity cell indicates a constant value was recorded.
8. The pump was stopped and a different flow value of 50rpm and 60rpm was set.
9. The conductivity when the system is stabilized was recorded again.

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Result

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

100

75

y = -161.97x + 596.5
Conversion,

R² = 0.9718
50

25

0
0 1 2 3 4
Conductivity, mS/cm

Figure 2: Calibration curve of Conversion vs Conductivity

🖙 To convert the pump rotation to a volumetric flow rate, recall:

𝑐ℎ𝑎𝑛𝑔𝑒 𝑖𝑛 ∆𝑉
𝐹𝑙𝑜𝑤 𝑟𝑎𝑡𝑒, =
𝑣𝑜𝑙𝑢𝑚𝑒 ∆𝑡
𝑄 =
𝑡𝑖𝑚𝑒
𝑐ℎ𝑎𝑛𝑔𝑒

∆V, mL ∆t, min QA, mL/min QB, mL/min Q, mL/min

40 rpm 100 1.25 80 80 160
50 rpm 0.91 110 110 220
60 rpm 0.67 150 150 300
Table 1: Calculation of volumetric flow rate

For 40 rpm:

∆𝑉 100
𝑄𝐴 = 𝑄𝐵 = = = 80 𝑚𝐿/𝑚𝑖𝑛
∆𝑡 1.25
𝑄 = 𝑄𝐴 + 𝑄𝐵 = 160 𝑚𝐿/𝑚𝑖𝑛

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For 50 rpm:

𝑄𝐴 = 𝑄𝐵 = 110 𝑚𝐿/𝑚𝑖𝑛

For 60 rpm:

𝑄𝐴 = 𝑄𝐵 = 150 𝑚𝐿/𝑚𝑖𝑛

🖙 To convert the measured conductivity to conversion using the calibration cure above:

Equation Conductivity, mS/cm Conversion, %

40 rpm y=-161.97x+596.5 3.19 79.82

50 rpm 3.39 47.42
60 rpm 3.52 26.37
Table 2: Converting measured conductivity to conversion

100

80
Conversion,

60

40

20

0
3.15 3.2 3.25 3.3 3.35 3.4 3.45 3.5 3.55
Conductivity, mS/cm

Figure 3: Conversion vs Conductivity graph

🖙 To calculate residue time (space time) and concentration of NaOH at the outlet:

C'AO, M QA, mL/min Q, mL/min 𝑟, min CAO, M XA,% CA , M

0.01 80 160 12.5 0.005 79.82 0.0010

110 220 9.09 47.42 0.0026

150 300 6.67 26.37 0.0037

Table 3: Calculating residue time

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Where,

C'AO = concentration of NaOH in the inlet before mixing

CAO = concentration of NaOH in the inlet after mixing

𝑪𝑨𝑶 = 𝑸𝑨
× 𝑪′𝑨𝑶
�+
𝑨

𝑸𝑩

QA = flow rate of NaOH

QB = flow rate of Et (Ac)

Q = total flow rate

𝑸 = 𝑸𝑨 + 𝑸𝑩

𝑟 = residue (space) time

𝒓𝒆𝒂𝒄𝒕𝒐𝒓 𝟐𝟎𝟎𝟎
𝑟 = 𝒗𝒐𝒍𝒖𝒎𝒆 𝒎𝑳 = 𝟏𝟐. 𝟓 𝒎𝒊𝒏
=
𝒇𝒍𝒐𝒘 𝒓𝒂𝒕𝒆 𝟏𝟔𝟎
𝒎𝑳/𝒎𝒊𝒏

XA = conversion of NaOH at the outlet

CA = concentration of NaOH at the outlet

𝑪𝑨 = 𝑪𝑨𝑶 − 𝑪𝑨𝟎𝑿𝑨
Conversion,

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20

0
6 7 8 9 10 11 12 13
Residue time, min

Figure 4: Conversion vs Residue time graph

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Discussion

Figure 2 shows that the conductivity is inversely proportional with the conversion. Conductivity
decreases as the conversion increases. The graph shows the theoretical value and relationship
between conversion and conductivity. Based on the graph, we can relate conductivity and
conversion into linear equation where,

𝒚 = 𝒎𝒙 + 𝒃

Where, y = the Conversion, %

x = the Conductivity, mS/cm

Thus, the linear equation of the graph is

𝒚 = −𝟏𝟔𝟏. 𝟗𝟕𝒙 + 𝟓𝟗𝟔. 𝟓

Whereas, in Figure 3, the graph shows the experimental value not the theoretical, and the
recorded conductivity is inversely proportional to the calculated conversion again. The
conductivity decreases as the conversion increases. In order to determine the conversion of
NaOH, the value of the conductivity is taken as the guidelines. The conductivity is decreasing
due to the less ionic content in the water. The conductivity basically is the ability of a solution to
conduct electricity. As the experiment going further, the conductivity decrease as the number of
ionic content in the solution is decrease over time. The higher the conversion, the lower the
concentration of the solution remaining inside the reactor, therefore the conductivity decrease.

From the calculation in Table 1, to convert pump rotation to volumetric flow rate, it is clear that
as pump rotation increases so do the volumetric flow rate, but they are inversely proportional to
the change in time.

Figure 4 shows that the conversion is directly proportional with the residence time. The
conversion increases as the residence time increases. Residence times refer to the time taken
needed to process one volume of the reactor fluid at the entrance condition whereas the
conversion refers to how many moles of products are formed for every mole of NaOH
consumed. Three values of conversion which are 26.37% at 6.67 min, 47.42% at 9.09 min and
79.82% at 12.5 min are recorded.

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Conclusion
From the experiment, we were able to found out a saponification between Sodium Hydroxide,
NaOH and Ethyl Acetate, Et (Ac) in tubular flow reactor, TFR. By using a Plug Flow Reactor,
PFR, both Sodium Hydroxide, NaOH and Ethyl Acetate, Et (Ac) were flowed into the reactor,
mixed and let to react for a certain period of time.

The flow rate of the sodium hydroxide, NaOH and ethyl acetate, Et (Ac) is 80mL/min,
110mL/min and 150mL/min each. The residence time for each flow rate is 12.5min, 9.09min and
6.67min respectively. The conversion of the reactant to product is 79.82%, 47.42% and 26.37%
respectively.

Based on the result that we have collected, we can conclude that the higher the conductivity, the
lower the conversion of solution. The lower the total flow rate of solutions, the higher the
residence time for each test.

Last, we were able to determine the effect of flow rate on the percentage of conversion. The
higher the flow rate, the lower the conversion. Therefore we can conclude that the experiment
was successfully conducted since we were able to fulfill the objective of this experiment.

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Reference
🖙 Fogler H.S. , “Elements of Chemical Reaction Engineering, 3rd Ed.”, Prentice Hall (USA) ,
1999.
🖙 Lab Report Effect of Residence Time On The Reaction in TFR (2015). Retrieved from:
https://www.academia.edu/18747178/CHE244_Lab_Report_Effect_of_Residence_Time_On_
The_Reaction_in_TFR_2015_
🖙 Lab Report Tubular Flow Reactor. Retrieved from:
https://www.academia.edu/31859058/Lab_Report_Tubular_Flow_Reactor
🖙 Lab Report on Plug Flow Reactor (2018). Retrieved from:
https://www.academia.edu/37932046/CHE506_Lab_Report_On_Plug_Flow_Reactor_L5_20
🖙 Plug Flow Reactor Lab Report. Retrieved from:
https://pdfcoffee.com/plug-flow-reactor-lab-report--pdf-free.html

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