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Lap, Reac 7

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Lap, Reac 7

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nasser nsoor
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Department of

Chemical Engineering

Reaction Engineering Lab


(CHE433)

OPERATION OF NONISOTHERMAL PLUG FLOW


Experiment title REACTOR

Experiment No. 7

Experiment date 24/05/2023

By

Student name ID Section

1 Nasser Abdulaziz Alammar 436017370 2

Instructors: Dr. Srinivas Tadepalli


Department of
Chemical Engineering

Evaluation sheet (Official use)


Marks
Checklist Details Marks Deducted Remarks

Cover Page
Plagiarism in results & discussion part must be < 50%

Table of Content 5

Introduction
15
(Experiment objectives, theory, etc.)
± 5 marks, depending
Contents

Experiment Procedure & setup 5 on the nature of


department/lab
Data, Results & calculations 25

Discussion and/or Conclusion 20

References, Standard, appendix, etc. 5

Subtotal 80 Min. 48

Text 12 Regular, with Spacing 1.5 4

Heading 14 Bold 2
Formatting

Standard Front Type 2

Paragraph: Justified 2

Figures/Tables/Equations: Numbered,
10
Caption & Cited in text

Subtotal 20 Min. 12

Total 100
Table of Contents

1. Introduction ................................................................................................... 2
1.1. Objectives ......................................................................................................... 2
1.2. Background / Theory ....................................................................................... 2

2. Experiment Procedure and Setup ............................................................... 3


2.1. Apparatus/device description ........................................................................... 3
2.2. Procedure ......................................................................................................... 5

3. Results ............................................................................................................ 6
3.1. Observations .................................................................................................... 6
3.2. Calculations...................................................................................................... 8

4. Discussion / Analysis ................................................................................... 10

5. Conclusion ................................................................................................... 11

References .......................................................................................................... 12

1
1. Introduction

The experiment mainly utilized two different mixtures of sodium hydroxide and ethyl
acetate and were pumped to the (PFR) Reactor without hoses at different rates in the device
and then record and note the temperature and conductivity at this different rate.

1.1. Objectives

• To determine the order and reaction rate constant for liquid phase in Non-isothermal
PFR.
• To study the effect of flow rate on the conversion of reactant.[3]

1.2. Background / Theory

Plug Flow Reactor (PFR) is one of continuous flow reactors that are normally operated at steady
state. It is normally used for gas phase reaction, but it can also be used for liquid phase reaction.
In PFR, there is no radial variation in terms of temperature and concentration. The reactants are
consumed continuously through the reactor in axial direction. The liquid phase reaction in this
experiment is:

NaOH + CH3COOC2H5 → CH3COONa + C2H5OH (A)

Material balance done for steady state is as follows:

(7.1)

From stoichiometry of the above reaction, we obtain relation between concentration of sodium
hydroxide (A) as function of conversion as follows:

CA = 𝐶𝐴𝑜 (1−𝑥) (7.2)

By taking

V
τ= (7.3)
v

2
One can modify eq. (1) into

= (7.4)

assuming the reaction rate is only depending on sodium hydroxide, one can easily get

−𝑟𝐴 = 𝑘. 𝐶𝐴𝑛 (7.5)

During the reaction, sodium hydroxide will dissociate into sodium ion and hydroxide ion while
ethyl acetate will also dissociate acetate ion and ethyl ion. Hydroxide ions will be bound to
ethyl ions producing ethanol while acetate will be bound with sodium resulting in sodium
acetate. The presence of hydroxide ions can be traced by measuring the conductivity of the
solution. Thus, conversion of the reaction can be directly related to the conductivity by the
following equation:

Λ∞−Λ
X=1− (7.6)
Λ∞−Λ0

[3]

2. Experiment Procedure and Setup

2.1. Apparatus/device description

Figure 7.1: CHEMICAL REACTORS TRAINER (CE310). [2]

3
1. Benchtop unit to study the kinetics of reaction kinetics of various types of chemical
reactors based on saponification

2. Chemicals pumped using 2 industrial diaphragm pumps

3. Reaction of 2.3% sodium hydroxide with ethyl acetate

4. High precision combined measuring unit for conductivity 0...200mS and reaction
temperature 0...100°C

5. Hot water circuit with centrifugal pump for moderating the reaction

6. Electrical heater, 2kW

7. Electronic two-point controller

8. Self-sealing quick action hose couplings

- Basic unit to study and compare various reactors using the example of a saponification

- High precision, combined conductivity, and reaction temperature measurement

- Usage of industrial diaphragm pump


Technical description:

The properties of different chemical reactors can be investigated by performing a saponification


reaction using this trainer. The contact time and reaction temperature can be varied. Their
influence on the conversion of reactants is observed in the respective reactor. The reactors are
available as accessories. The unit contains two supply tanks for the liquid chemicals. Two
variable speed diaphragm pumps pump the reactants through the reactor. Reactant conversion
and reaction temperature are measured with a combined conductivity and temperature
measuring unit. It is also possible to use PC data acquisition. The reaction is moderated using
a controlled hot water circuit. The resulting reaction product is collected in a stainless-steel tray
in the unit. [2]

Experiments:

In conjunction with the various types of reactors available as accessories in the CE 310 series,
comprehensive experiments on the reaction kinetics and on the conversion of reactants during

4
a saponification reaction can be performed. Specifically, the following experiments can be
performed: - Variation of contact time of the two chemicals

1. Variation of reaction temperature

2. Adiabatic reaction in a batch reactor

3. Isothermal reaction in a batch reactor

Figure 7.2 Tubular Reactor (CE 310.02 of GUNT). [1]

2.2. Procedure

Solution Preparation

Dilution of ethyl acetate:

• Take 40 ml of ethyl acetate (𝜌 = 0.9 g/cm3; Mw = 88.11 g/mol) to prepare 4000 mL


of ethyl acetate 0.1 M.
• Dilute it until the total volume reach 4000 mL in a 4L-beaker.

• Stir it rigorously until ethyl acetate and water are completely mixed.

Dilution of Sodium hydroxide:

• Take 16 g of sodium hydroxide (Mw = 40 g/mol) to prepare 4000 mL of sodium


hydroxide 0.1 M.
• Dilute it until the total volume reach 4000 mL in a 4L-beaker.
5
• Stir it rigorously until sodium hydroxide and water are completely mixed.

PFR operational procedure.

• Calibrate the actual flow rate of both pumps needed in this experiment at speed scale
of 20; 40 and 80.
• Connect the correct chemical hoses from the pumps to the tank.
• Insert conductivity measuring sensor at the outlet of PFR.
• Set required temperature for the heating regulator to 40oC and switch on the heater.
• Switch on the chemical pumps and adjust both to the same flow rate approximately
20:20.
• At specific interval (as provided in the log sheet) measure the conductivity and
temperature until it reaches steady state.
• Repeat step e-f for the flow rate to 40:40 and 80:80 .[3]

3. Results
3.1. Observations

Table 7.1: Data collected for NON ISOTHERMAL PFR reactor at temperature 20°C Rom
temperature and at different pump speed

- 20:20 40;40 80:80


Time
Time
Min:
[sec]
sec cond. Temp. cond. Temp. cond. Temp.
0.00 0.00 4.80 20.40 7.10 20.40 8.20 20.70
30.00 0.30 4.80 20.40 7.20 20.40 8.70 20.70
90.00 1.30 4.80 20.40 7.50 20.40 9.00 20.80
120.00 2.00 4.80 20.40 7.70 20.50 9.10 20.80
150.00 2.30 4.80 20.40 7.80 20.50 9.30 20.90
180.00 3.00 4.80 20.40 7.90 20.50 9.30 20.90
210.00 3.30 4.80 20.30 8.10 20.50 9.30 20.90

6
240.00 4.00 4.70 20.30 8.10 20.50 - -
300.00 5.00 4.90 20.30 8.10 20.60 - -
360.00 6.00 5.60 20.30 - - -
420.00 7.00 6.50 20.20 - - - -
480.00 8.00 7.40 20.20 - - - -
540.00 9.00 7.50 20.20 - - - -
600.00 10.00 7.40 20.20 - - - -
660.00 11.00 7.20 20.20 - - - -
720.00 12.00 7.10 20.20 - - - -
750.00 12.30 7.10 20.20 - - - -
780.00 13.00 7.00 20.30 - - - -
810.00 13.30 7.00 20.30 - - - -
840.00 14.00 7.00 20.30 - - - -

Table 7.2: Data collected for NON ISOTHERMAL PFR reactor at rom temperature

20:20 40;40 80:80


Conversion Conversion Conversion
X Cao X Cao X Cao
0.000 0.100 0.000 0.100 0.000 0.100
0.000 0.100 0.100 0.090 0.455 0.055
0.000 0.100 0.400 0.060 0.727 0.027
0.000 0.100 0.600 0.040 0.818 0.018
0.000 0.100 0.700 0.030 1.000 0.000
0.000 0.100 0.800 0.020 1.000 0.000
0.000 0.100 1.000 0.000 1.000 0.000
-0.045 0.105 1.000 0.000 - -
0.045 0.095 1.000 0.000 - -
0.364 0.064 - - - -
0.773 0.023 - - - -
1.182 0.018 - - - -
1.227 0.023 - - - -
1.182 0.018 - - - -

7
1.091 0.009 - - - -
1.045 0.005 - - - -
1.045 0.005 - - - -
1.000 - - - - -
1.000 - - - - -
1.000 - - - - -

3.2. Calculations

Table 7.3: Data collected for NON ISOTHERMAL PFR reactor at rom temperature
20:20 40:40:00 80:80
Time Time Min: 1-
ln(cao-ca) 1-xa ln(cao-ca)3 1-xa2 ln(cao-ca)4
[sec] sec xa3
0.00 0.00 - 1.000 - 1.000 - 1.000
30.00 0.30 - 1.000 4.605170186 0.900 3.091042453 0.545
90.00 1.30 - 1.000 3.218875825 0.600 2.621038824 0.273
120.00 2.00 - 1.000 2.813410717 0.400 2.503255788 0.182
150.00 2.30 - 1.000 2.659260037 0.300 2.302585093 0.000
180.00 3.00 - 1.000 2.525728644 0.200 2.302585093 0.000
210.00 3.30 - 1.000 2.302585093 0.000 2.302585093 0.000
240.00 4.00 - 1.000 2.302585093 0.000
300.00 5.00 -1.56861592 1.000 2.302585093 0.000
360.00 6.00 -1.56861592 1.000
420.00 7.00 -1.56861592 1.000
480.00 8.00 -1.56861592 1.000
540.00 9.00 -1.56861592 1.000
600.00 10.00 -1.56861592 1.000
660.00 11.00 -1.56861592 1.000
720.00 12.00 -1.56861592 1.000
750.00 12.30 -1.56861592 1.000
780.00 13.00
810.00 13.30

8
840.00 14.00

Follow the calculation steps for all data as shown (taking 9 min for 20:20 as example of
calculations):

• Calculate the initial of concentration:

𝑚 16 𝑔
CA0 =𝑀 = 𝑔 × (10−3𝐾𝑚𝑜𝑙/𝑚𝑜𝑙) (1 𝑚𝑙/𝑐𝑚3 )(1003 𝑐𝑚3/𝑚3 )
𝑤 .𝑉 (40 )(4000 𝑚𝑙)
𝑚𝑜𝑙

Kmol
CA0 = 0.1 m3

• Calculate the conversion using equation (7.6) where Λ∞ = 7 𝑚𝑆/𝑐𝑚, and Λ0 = 4.8
𝑚𝑆/𝑐𝑚:

7−4.8
X=1- 7−4.8 = 0

• Calculate the concentration at t = 9 min by using equation (6.2):

CA = 0.1(1 − 0) = 1

• Get the vales of Activation energy and frequency factor by:

−E
k = k o e(RT)
At T = 25℃ , k o = 2194760 ,E= 41400 J/mol and R= 8314 J/mol.K
−41400
( )
k = 2194760e 8314×(25+273) = 2160120 J/mol

• For the time space Ƭ


π
V= 4 D2 H
π
= 4 (0.1)2 (0.1) = 0.00079 m3

ml m3
ν = 80 min = 0.00000133sec

9
V 0.00079 m3
Ƭ=ν = m3
= 592.5 sec = 9.9 min
0.00000133
sec

4. Discussion / Analysis

At the beginning, the device must be calibrated and compared with the factory setting, and the
results were seen with similar values as shown in Table 7.2

Table 7.4: Calibration

20:20 40:40 80:80

Theo. Calibrate 79 Calibrate 162 Calibrate 330


Flow ml/min Flow ml/min Flow ml/min
rate rate rate

Calibrate Calibrate 162 Calibrate


80 335
Ref. Flow Flow ml/min Flow
ml/min ml/min
rate rate rate

Looking at the figure 7.1 shown below, it can be seen that some of the readings are not
logical, during the experiment some errors occurred as some of the conversion values are
negative.

10
6

4
y = 3.457x
3
ln(cao-ca)

0
-2 0 2 4 6 8 10 12 14 16 18 20

-1
1-xa

Figure 7.3: ln (Cao-Ca) vs (xa-1)

11
1.200

1.000

0.800

0.600
Conversion X

Linear (20:20)
Linear (40:40)
Linear (80:80)
0.400

0.200

0.000
-0.000001 0 0.000001 0.000002
Ƭ 0.000003 0.000004 0.000005

-0.200

Figure 7.4: Ƭ vs conversion x


Also, there is a relationship that time space vs conversion is a linear relationship, but through
values it is not a linear relationship since it is corrected to be linearized since the actual value
in time space is different from experiment which is show in figure 6.3 and as shown in the
equation relationship (7.5) n is equal two

5. Conclusion

Finally, this experiment was supported by showing the relationship between conversion and
temperature in this reaction shows the change in concentration over time the impact directly
rises with temperature. After achieving constant transmission, the first and second temperatures
are determined by the conductivity number.

12
References

[1]. Elements of Chemical reaction engineering 5th Edition.

[2]. Equipment catalogs.

[3]. Chemical Reactions Lab Manual.

[4]. Fogler, H.S, Elements of Chemical Reaction Engineering, 4th edition, 2007, Prentice Hall
NY.

[5]. Reaction Engineering Lab CHE-433 Manual.

[6]. Octave Levenspiel, “Chemical reaction engineering,”3rd ed., John Wiley & Sons, NY,
2001.

[7]. Coulson & Richardson, “Chemical Engineering Vol-3” 4 th ed., Asian Books Pvt.Lt, ND,
1991.

[8]. Perry’s Chemical Engineering Handbook 7th Edition.

13

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