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EXP 1: BATCH REACTOR

Content

1.0 Objective 2

2.0 Summary 2

3.0 Introduction and Theory 3-4

4.0 Data & Result 5-8

5.0 Analysis and Discussion 9

6.0 Conclusion and Recommendation 10

7.0 Tutorial 11

8.0 Reference 12

9.0 Appendix 12-14

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EXP 1: BATCH REACTOR

1.0 Objective
1) To conduct mass balance and energy balance in batch process system.

2.0 Summary

The objective of this experiment is to conduct mass balance and energy balance in batch
process system by batch saponification reaction between sodium hydroxide (NaOH) and ethyl
acetate. The experiment began by preparing the solution of sodium hydroxide and ethyl acetate
and mixing it together with distilled water and poured into the batch reactor. The sample mixed
in the reactor and every 5 minutes, sample of the solution was taken to measure the conductivity
using conductivity meter. This procedure was repeated for 60 minutes and the temperature was
maintained at 30°C. Based on the result obtained, it can be concluded that the conductivity
decreased as the concentration of Sodium Hydroxide decreased. Thus, the conversion was
calculated and compare with the conductivity. As the conversion, X increased, the conductivity
decreased shown from the graph of conductivity against conductivity.

3.0 Introduction & Theory

The Batch reactor is the generic term for a type of vessel widely used in the process
industries. Vessels of this type are used for a variety of process operations such as solids
dissolution, product mixing, chemical reactions, batch distillation, crystallization, liquid/liquid
extraction and polymerization. A typical batch reactor consists of a tank with an agitator and
integral heating/cooling system. Liquids and solids are usually charged via connections in the
top cover of the reactor. Vapors and gases also discharge through connections in the top.
Liquids are usually discharged out of the bottom.

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EXP 1: BATCH REACTOR

Figure 1:Batch Reactor Unit

The reaction chosen is the hydrolysis of ethyl acetate by sodium hydroxide, this reaction
can be carried out under safe conditions of temperature and pressure. This type of reaction is
called a saponification because of its importance in the manufacture of soap. The reaction is
relatively slow and the changing ester concentration can be followed quite easily by analysing
samples from the reaction mixture every few minutes.

Saponification is the hydrolysis of a carboxylic acid ester in a basic medium.


Saponification is essentially a soap manufacturing process that takes place by reacting the fatty
acid with alkali, especially triglycerides producing glycerol and carboxylate salts (soap).

CH 3 COOC2 H 5  NaOH  CH 3 COONa  C 2 H 5 OH

EtAc  NaOH  NaAc  EtOH

Ethyl acetate  sodium hydroxide  sodium acetate  ethanol

As the reaction proceeds, hydroxyl ions are consumed and acetate ions are produced.
Both sodium hydroxide and sodium acetate contribute conductance to the reaction solution,
whereas ethyl acetate and ethyl alcohol do not. Hydroxyl ion has a very much larger specific
conductance than acetate ion. Hence, the alkaline hydrolysis of ethyl acetate may be monitored
by following the change in the conductance of the reaction mixture with time.

CH3COOC2H5 + OH- → CH3COO- + C2H5OH


Ethyl acetate + hydroxyl ion → acetate ion + ethanol

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EXP 1: BATCH REACTOR

4.0 Data and Result

Table 1: calibration curve

Concentration of Naoh (M) Conductivity (mS/cm)


0.0500 10.7
0.0375 9.7
0.0250 7.5
0.0125 5.6
0.0000 4.0

Calibration Curve
12

10
Conductivity (mS/cm)

y = 140x + 4
8

0
0 0.01 0.02 0.03 0.04 0.05 0.06
Concentration of NaOH (M)

Figure 2: Conductivity (ms/cm) against Concentration of Sodium Hydroxide, NaOH (M)

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EXP 1: BATCH REACTOR

Table 2: Conversion, X (%) at different Temperature (°C)

Time Temperature Conductivity Concentration of NaOH, CNaOH (M) Conversion, X


(min) (°C) (mS/cm) (From Calibration Curve) (%) (Self
calculation)
0 30 10.23 0.0445 0
5 38 10.05 0.0432 2.92
10 40 9.97 0.04260 4.27
15 42 9.52 0.0394 11.46
20 44 8.96 0.0354 20.45
25 46 8.62 0.0330 25.84
30 47 8.60 0.0329 26.07
35 49 8.59 0.0328 26.29
40 49 8.58 0.0327 26.52
45 50 8.58 0.0327 26.52
50 51 8.52 0.0323 27.42
55 52 8.50 0.0321 27.87
60 54 8.42 0.0315 28.99

Conversion, X (%) VS Time


40

35

30
Conversion, X (%)

25 28.99
27.42 27.87
25.84 26.07 26.29 26.52 26.52
20
20.45
15

10
11.46
5
4.27
0 2.92
0 5 10 15 20 25 30 35 40 45 50 55 60
Time (min)

Figure 3: The Conversion, X (%) against Time (min)

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EXP 1: BATCH REACTOR

5.0 Analysis & Discussion

This experiment was conducted to conduct mass balance and energy balance in batch
process system. Through this experiment, the reaction between sodium hydroxide and ethyl
acetate was analysed in order to improve understanding and gain hands-on experience in
reaction engineering in general and batch reactors in specific. Both ethyl acetate and ethyl
alcohol are none conductive. On the other hand, sodium hydroxide and sodium acetate are
conductive, sodium hydroxide is a stronger ionic compound than sodium acetate and as a result,
it has higher conductivity.

Based on the figure 1, the graph shows increasing of conductivity against concentration of
sodium hydroxide. From these relations, the increase in conductivity that occur as the reaction
proceeds also indicate an increase in sodium hydroxide concentration and an increment in
sodium acetate concentration. The higher conductivity was 10.7 ms/cm at concentration of
sodium hydroxide was 0.0500 M. While the lowest conductivity was 4.0 ms/cm at
concentration of sodium hydroxide was 0 M.

According to the calibration curve, the higher the conductivity, the lower the conversion.
Conductivity is caused by the ionic solution such as sodium hydroxide and ethyl acetate.
Sodium hydroxide has a higher conductivity compared to ethyl acetate. Therefore, when
sodium hydroxide is used to produce sodium acetate; the concentration of the strong sodium
hydroxide ions decreases, thus causing the conductivity to decrease as well. Based on the best
line obtained, the relationship between concentration and conductivity can be expressed in the
equation of Y=140x +4.

Based on Figure 2, the graph shows as the reaction time increases the rate of conversion
increases until a state of equilibrium has achieved and the reaction has ended. The graph also
shows that the rate of conversion increases over time. This supports the theory that sodium
hydroxide has a higher conductivity than ethyl acetate and when sodium hydroxide is reacted
to form sodium acetate and ethyl alcohol in the saponification reaction, the conductivity
decreases.

The conductivity decreases faster and the rate of conversion in Figure 2 is higher as the
concentration decreases. A reaction in a higher temperature occurs faster because as the
temperature increases, the particles vibrate and move faster, causing them to collide more with
each other. This causes a higher rate of effective collisions and minimum activation energy is
needed to let the reaction started. The highest conversion is 29.05% at 60 minutes. Furthermore,

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EXP 1: BATCH REACTOR

the relationship between conversion and time can be expressed in the equation of Y=0.4942x
+4.7431.

Sodium hydroxide + Ethyl acetate → Sodium acetate + Ethyl alcohol

NaOH + CH3COOC2H5 → CH3 COO Na + C2H5 OH

It was noted that the concentration-time curve slope change with time, where the curve
becomes less steep at the final stage, due to the decrease in reagents concentrations. The
reaction rate increases with increasing temperature, hence higher conversions are achieved for
higher temperatures at equal time intervals. The error % that resulted at the end of the
calculations was found to be relatively high. This is a result of human error factor and
inaccurate temperature control.

Mass balance for the batch reactor

Limiting and excess reactant.

NaOH + CH3COOC2H5 CH3COONa + C2H5OH

NaOH CH3COOC2H5
g kg
ρNaOH = 2.13 cm3 ρCH3COOC2H5 = 902 m3
1m3 1003 cm3 g kg 1 m3 1000 g
massNaOH = 3L × 1000 L × × 2.13 cm3 massCH3COOC2H5= 3L × 902 m3 × 1000 L ×
13 m3 1 kg
= 6390 g = 2706 g
6390 g 2706g
nNaOH = g nCH3COOC2H5 = g
39.997 88.11
mol
mol

= 159.76 mol NaOH = 30.71 mol CH3COOC2H5

159.76 mol NaOH


For NaOH = = 159.76 mol NaOH
1

30.71 mol CH3COOC2H5


For CH3COOC2H5 = = 30.71 mol CH3COOC2H5
1

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EXP 1: BATCH REACTOR

In this reaction, 30.71 mol CH3COOC2H5 is smaller than 159.76 mol NaOH, therefore, Ethyl
Acetate (CH3COOC2H5) is the limiting reactant and Sodium Hydroxide (NaOH) is the excess
reactant.

Total mole = 159.76 mol + 30.71 mol

= 190.47 mol total

Molar Fraction CH3COOC2H5 Molar Fraction NaOH


30.71 mol CH3COOC2H5 YNaOH = 1- 0.16
YCH3COOC2H5 = 190.47 mol total
= 0.84
= 0.16

Coefficient of reactants:

We know nCH3COOC2H5, feed = 30.71 mol CH3COOC2H5 and nNaOH, feed = 159.76 mol NaOH

1 mol NaOH consumed


nNaOH, stoichiometry = nCH3COOC2H5, feed ×
1 mol CH3COOC2H5 consumed

1
= 30.71 mol CH3COOC2H5 × = 30.71 mol NaOH
1

𝑛𝑓𝑒𝑒𝑑 −𝑛𝑠𝑡𝑜𝑖𝑐ℎ𝑖𝑜𝑚𝑒𝑡𝑟𝑦
% Excess of NaOH = × 100%
𝑛𝑠𝑡𝑜𝑖𝑐ℎ𝑖𝑜𝑚𝑒𝑡𝑟𝑦

(159.76−30.71)mol CH3COOC2H5
× 100% = 420.22 %
30.71 mol CH3COOC2H5

Mass Balance Calculation:

NaOH + CH3COOC2H5 CH3COONa + C2H5OH

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EXP 1: BATCH REACTOR

n1 (NaOH) = 4.20 mol


ntotal = 190.47 mol total n2 (CH3COONa)
n3 (C2H5OH)

CH3COOC2H5 = 0.16 n4 (CH3COOC2H5)

NaOH = 0.84
Figure 3: Flowchart of the process

Extend of reaction:

NaOH: n1= (0.84 × 190.3) + ξ1 + ξ2

CH3COOC2H5: n2= (0.16 × 190.3) + ξ1 + ξ2

C2H5OH: n3= 0 - ξ1 - ξ2

CH3COOC2H5: n4= 0 - ξ1 - ξ2

Carbon:

4 (0.16 × 190.3) = 2n2 + 2n3 + 4n4 → eq1

Hydrogen:

(0.84 × 190.3) + 8 (0.16 × 190.3) = n1 + 3n2 + 6n3 + 8n4 →eq2

Oxygen:

(0.84 × 190.3) + 2 (0.16 × 190.3) = n1 + 2n2 + n3 + 2n4 →eq3

Sodium:

(0.84 × 190.3) = n1 + n2 →eq4

Substitute n1= 4.23 mol into eq4

(0.84 × 190.3) = (4.23) + n2

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EXP 1: BATCH REACTOR

n2 = 155.622 mol

Substitute n1= 4.23 mol and n2 = 155.62 mol into eq3

(0.84 × 190.3) + 2 (0.16 × 190.3) = (4.23) + 2(155.62) + n3 + 2n4

n3 = -94.722-2n4 →eq5

Substitute n1= 4.23 mol, n2 = 155.62 mol and n3 = -94.722-2n4 into eq2

(0.84 × 190.3) + 8 (0.16 × 190.3) = (4.23) + 3(155.62) + 6(-94.722-2n4) + 8n4

-4n4 = 500.678

n4 = -125.17 mol

Substitute n4 = -125.17 mol into eq5

n3 = -94.722-2(-125.17)

n3 = 155.618 mol

n1 (NaOH) = 4.23 mol

n2 (CH3COONa) = 155.622 mol

n3 (C2H5OH) = 155.618 mol

n4 (CH3COOC2H5) = -125.17 mol

Energy balance for the batch reactor


𝐸𝑖𝑛 − 𝐸𝑜𝑢𝑡 = ∆𝐸𝑠𝑦𝑠𝑡𝑒𝑚

𝑄 − 𝑊𝑠 = ∆𝐻 + ∆𝐸𝑘 + ∆𝐸𝑝

𝑄 = ∆𝐻

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EXP 1: BATCH REACTOR

Thus,

𝑄 − 𝑊𝑠 = ∆𝐻 + ∆𝐸𝑘 + ∆𝐸𝑝

6.0 Conclusion & Recommendation

6.1 Conclusion

6.2 Recommendation

7.0 Tutorial

1. Describe an example of industrial applications other than saponification that utilized batch

reactors in its process. Discuss the advantages and disadvantages of using batch

reactors in chemical reaction.

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EXP 1: BATCH REACTOR

Manufacture of margarine applies the utilized batch reactor in its process. The
production of the fatty base for edible margarines by the hydrogenation of vegetable oil is
carried out at high temperature and has serious disadvantages, among them the toxicity of the
nickel catalyst and fire-hazardous filtration stage. Here, a batch reactor and selective, low
loaded palladium catalyst was described which allow vegetable oil hydrogenation to take place
at lower temperature producing high quality, pure hydrogenation fat, free of catalyst. Under
these milder temperature, the thermal decomposition of oils and fat does not form secondary
products, and heavy metals from catalyst do not enter the final product. In addition, even lower
hydrogenation temperatures can be used with palladium catalyst, resulting in fat with low
Transisomer content. The catalyst has been tested successfully in full-scale production. Using
an inertial separator in a batch reactor, catalyst loss has been eliminated.

Advantages Disadvantages

 High conversion per unit volume  High operating cost


for one pass  Product quality more variable
 Flexibility of operation-same than with continuous operation
reactor can produce one product
one time and a different product
the next
 Easy to clean

2. Write a one-paragraph summary of any journal article that studies chemical reaction in a

batch reactor. The article must have been published within the last 5 years. Explain on

the batch reactor used in the study and its significance to the study done.

The interest in the epoxidation of vegetable oils is constantly growing in the chemical industry.
The most common process is based on the oxidation of the unsaturated bonds by peroxyacids

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EXP 1: BATCH REACTOR

generated in situ, in the water phase, using concentrated hydrogen peroxide and the
corresponding organic acid in presence of a mineral acid as catalyst. The overall epoxidation
reaction is highly exothermic, hence operating conditions should be always addressed by safety
considerations related to the possibility of runaway reactions.

In this paper, best operating conditions and safety considerations have been defined for a
complex reaction network for the epoxidation of soybean oil, which includes the decom-
position reactions of the performic acid generated during the epoxidation. Furthermore,
sensitivity-based reactor stability criteria have been applied and compared, for the design of an
adequate Early Warning Detection System for the process

(Casson Moreno, Russo, Tesser, Di Serio, & Salzano, 2017)

8.0 References

1) Astaria G., “Mass Transfer with Chemical Reaction”, Elsevier, 1967


2) Chemicals Reactor. (2014) Enzyme Technology.
http://www.essentialchemicalindustry.org/processes/chemical-reactors.html
3) Fogler H.H., “Elements of Chemical Reaction Engineering, 3rd Ed.”, Prentic Hall
(USA), 1999.
4) Rutherford Aris, Elementary Chemical Reactor Analysis, Butterworth-Heinemann,
2013, p150
5) Smith J.M., “Chemical Engineering Kinetics”, McGraw Hill, 1981

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9.0 Appendix
9.1 Equation obtained from the graph,
𝒚 = 𝟏𝟒𝟎𝒙 + 𝟒
𝒚 = 𝒄𝒐𝒏𝒅𝒖𝒄𝒕𝒊𝒗𝒊𝒕𝒚
𝒙 = 𝒄𝒐𝒏𝒄𝒆𝒏𝒕𝒓𝒂𝒕𝒊𝒐𝒏 𝑵𝒂𝑶𝑯
1. Time: 0 min = 0.0426
𝑦−4
𝑥=
140 4. Time: 15 min

10.23−4
= 𝑦−4
140 𝑥=
140
= 0.0445 9.52−4
= 140
2. Time: 5 min
= 0.0394
𝑦−4
𝑥=
140
5. Time: 20 min
10.05−4
= 𝑦−4
140 𝑥=
140
= 0.0432 8.96−4
= 140
3. Time: 10 min
= 0.0354
𝑦−4
𝑥=
140 6. Time: 25 min

9.97−4 𝑦−4
= 𝑥=
140
140

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EXP 1: BATCH REACTOR

8.62−4 10. Time: 45 min


= 140
𝑦−4
𝑥=
140
= 0.033
8.58−4
7. Time: 30 min = 140

𝑦−4 = 0.0327
𝑥=
140
11. Time: 50 min
8.60−4 𝑦−4
= 𝑥=
140
140
= 0.0329 8.52−4
= 140
8. Time: 35 min
= 0.0323
𝑦−4
𝑥= 12. Time: 55 min
140
=
8.59−4 𝑦−4
140 𝑥=
140
= 0.0328 8.50−4
= 140

= 0.0321
9. Time: 40 min
𝑦−4 13. Time: 60 min
𝑥= 𝑦−4
140 𝑥=
140
8.58−4
= 8.42−4
140
= 140

= 0.0327
= 0.0316

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EXP 1: BATCH REACTOR

9.2 Conversion, X
𝑪𝑵𝒂𝑶𝑯 (𝒕=𝟎) − 𝑪𝑵𝒂𝑶𝑯 (𝒕)
𝑿= × 𝟏𝟎𝟎%
𝑪𝑵𝒂𝑶𝑯 (𝒕=𝟎)

1. Time: 0 min = 26.07


0.0445 − 0.0445
𝑋= × 100%
0.0445 8. Time: 35 min
=0 0.0445 − 0.0328
𝑋= × 100%
0.0445
2. Time: 5 min = 26.29
0.0445 − 0.0432
𝑋= × 100%
0.0445 9. Time: 40 min
= 2.92 0.0445 − 0.0327
𝑋= × 100%
0.0445
3. Time: 10 min = 26.52
0.0445 − 0.0426
𝑋= × 100%
0.0445 Time: 45 min
= 4.27 0.0445 − 0.0327
𝑋= × 100%
0.0445
4. Time: 15 min = 26.52
0.0445 − 0.0394
𝑋= × 100% 10. Time: 50 min
0.0445
= 11.46 0.0445 − 0.0323
𝑋= × 100%
0.0445
5. Time: 20 min = 27.42
0.0445 − 0.0354
𝑋= × 100% 11. Time: 55 min
0.0445
= 20.45 0.0445 − 0.0321
𝑋= × 100%
0.0445
6. Time: 25 min = 27.87
0.0445 − 0.0330
𝑋= × 100% 12. Time: 60 min
0.0445
= 25.84 0.0445 − 0.0316
𝑋= × 100%
0.04450
7. Time: 30 min = 28.99
0.0445 − 0.0329
𝑋= × 100%
0.0445

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