Faculty of Chemical Engineering

FINAL REPORT SKF 3751 CHEMICAL REACTION ENGINEERING LABORATORY 2011/2012-SEM 02 EXPERIMENT 3

Saponification of Ethyl Acetate And Sodium Hydroxide in CSTR

DATE OF EXPERIMENT 16 March 2012 DATE OF REPORT SUBMISSION 23 March 2012 LECTURER Dr. Dayang Nurul Fairuz Bt Abang Zaidel TECHNICIAN Mr. Zainor Abidin SECTION 02 GROUP
NO 1 2 3 4 TEAM MEMBERS Mohd Syamsul Fitri Bin Saad Wan Nur'ain Nabila Binti Wan Nain Nur Mizatul Hidayah Binti Ismail Sarah Eleena Binti Mohd Usli MATRICS NUM. AK090144 AK090369 AK090224 AK090255 NRIC 890428-03-5843 911231-03-5284 900110-01-5814 900707-14-6462

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TABLE OF CONTENT

NUM CONTENTS 1.0 2.0 Abstract Introduction 1.1 Experimental background 1.2 Objective 1.3 Experimental scope Theory/Literature Study

PAGE

3.0

4.0

Methodology 3.1 Equipment and Materials 3.2 Experimental procedure/methodology

5.0

6.0

Result and Discussion 4.1Experimental data 4.2 Data analysis and discussion 4.3 Answer to the question in the experimental module Conclusion

7.0

References

8.0

Appendices

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1.0 ABSTARCT This experiment is carried out to understand the CSTR system, study the use of a CSTR and the effects of flow changes. Other significance of doing this experiment is to determine rate constant from data and also to study the temperature effects for reaction. The real objective of conducting the experiment is to study the reaction process of saponification reaction between sodium hydroxide and ethyl acetate in CSTR.

The first things before all the apparatus is set-up, the conductivity calibration curve is prepared using different molar concentration of sodium hydroxide and sodium acetate. This calibration curve can be used to determine the reaction kinetics and the rate law of the process. Then, both sodium hydroxide and ethyl acetate is prepared according to the given volume and molar concentration before it is transferred into the tank. When the process started, the conductivity and temperature of the reaction is recorded for every two minutes for over 30 minutes. The space time as well as the conductivity and the temperature of the reaction medium are recorded when the liquid level in the CSTR reach two litres. After flow the reaction into the buffer tank, the readings are recorded for another ten minutes. The process are repeated for different amount of feed flow rates.

Based on methodology section in the report, it tells about the steps involved while conducting the experiment while the results section shows the recorded value of conductivity and medium reaction temperature. In addition, it also shows the calculated concentrations of the input and output chemicals, rate of reaction and theoretical space time of the CSTR. Instead of that, the discussion section shows the graph plotted using the result obtained and discussed it more detail based on chemical reaction engineering theory. The error and recommendation to avoid mistakes while doing the experiment is also shared in the discussion. The conclusion section concludes all the objectives and calculations of this experiment.

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2.0 INTRODUCTION A common type of reactor used in industrial processing is the continuous-stirred tank reactor (CSTR) which is used primarily for liquid phase reaction. It is normally operated at steady state and assumed to be perfectly mixed. Usually there is no time dependence or position dependence of the temperature, the concentration or the reaction rate inside the tank. This means that every variable is the same inside the reactor. Because the compositions of mixtures leaving a CSTR are those within the reactor, the reaction driving forces, usually the reactant concentrations, are necessarily low. Therefore, except for reaction orders zero- and negative, a CSTR requires the largest volume of the reactor types to obtain desired conversions. However, the low driving force makes possible better control of rapid exothermic and endothermic reactions. When high conversions of reactants are needed, several CSTRs in series can be used. Equally good results can be obtained by dividing a single vessel into compartments while minimizing back-mixing and short-circuiting. The larger the number of CSTR stages, the closer the performance approaches that of a tubular plug-flow reactor.

Figure shows Continuous stirred tank reactors, (a) With agitator and internal heat transfer surface, (b) With pump around mixing and external heat transfer surface. This experiment was conducted to study the saponification reaction between sodium hydroxide and ethyl acetate in a continuous-stirred tank reactor (CSTR). The saponification process is a process that produces soap, usually from fats and lye. In technical terms, saponification involves base (usually caustic soda NaOH) hydrolysis of triglycerides, which are esters of fatty acids, to form the sodium salt of a carboxylate.
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Instead of carry out the saponification process as the scope of the experiment, it also conducted to identify the CSTR system and investigate its operational behavior of a reaction in it, to calculate the reactant conversion based on the conductivity calibration curve and to verify the reaction order obtained from the hypothesis of the experiment using graphical and analytical techniques. The results from both techniques are compared. Besides that, the significance of doing this experiment is to determine the rate constant of saponification reaction by using both techniques again. In fact, the experiment is carry out to scale-up the reactor for large scale production and to compare the kinetic reaction, rate law and conversion in a CSTR to the one in a batch reactor system for the same reaction. The reaction kinetics and rate law of saponification reaction in a CSTR can be determined using conductivity calibration curve. Conductivity is a measure of how well a solution conducts electricity. To carry a current a solution must contain charged particles, or ions. Most conductivity measurements are made in aqueous solutions, and the ions responsible for the conductivity come from electrolytes dissolved in the water. Salts like sodium chloride and magnesium sulfate), acids (like hydrochloric acid and acetic acid), and bases (like sodium hydroxide and ammonia) are all electrolytes. Although water itself is not an electrolyte, it does have a very small conductivity, implying that at least some ions are present. The ions are hydrogen and hydroxide, and they originate from the dissociation of molecular water. There are two ways to calibrate conductivity sensors. The sensor can be calibrated against a solution of known conductivity or it can be calibrated against a previously calibrated sensor and analyser. Normally, the sensor should be calibrated at a point near the midpoint of the operating range calibration changes the cell constant. In this experiment, the calibration curve is prepared using different molar concentration of sodium hydroxide and sodium acetate.

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3.0 LITERATURE REVIEW In the industrial, two type of the reactor that always used are continuous stirred-tank reactor (CSTR) and packed bed reactor (PBR). The CSTR reactor will operate at the steady state. The process of the reactants into the reactor bribes and spending is the product of the reactor along the reactor operates continues. As a whole, the reactor was stirred continues mixed perfect and there is no distinction in the overall density and temperature in the reactor. This assumption may be made namely the concentration and temperature is identified in all regions of the reactor is equal to the temperature and density at the reactor output. Another advantage of this continuous stirred reactor is a reactor of this type has the ability to escort the temperature and pressure.

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4.0 METHODOLOGY

A. Calibration graph plot 1. Conductivity calibration curve is prepared using three points: i. ii. iii. X = 0.0, use 10mL 0.1M NaOH X = 0.5, use a mixture of 5 mL NaOH and 5 mL sodium acetate X = 1.0, use 10 mL 0.1M sodium acetate

B. Operating procedure 1. 9L solution of 0.1M NaOH (8g per 2L H2O) and 9L solution of 0.1M EA (19.6mL per 2L H2O) are prepared and these solutions were poured into T1 and T2 respectively. 2. Pumps P1 and P2, and stirrer S1 are switched on. The feed flow rates into the CSTR are adjusted to be at 40 cm3/min using valves F1 and F2. The stopwatch was started immediately as the pumps and stirrer were switched on. The conductivity and temperature of the reaction medium in the CSTR were measured for every 2 minutes for over 30 minutes. 3. When liquid level inside the CSTR reached 2000cm3 (2L), the space time, conductivity and temperature of the reaction medium were recorded. 4. Then, the reaction is flowed into the buffer tank by opening valve V3. Measurements were continued taken for 10 minutes. 5. When 30 minutes of reaction is over, valves F1 and F2 were closed, and pumps P1 and P2 were stopped. All liquids were discharged through valve V4. 6. The experiment was repeated for different feed flow rates: 60, 100 and 120 cm3/min. 7. Once the experiments were done, all residual NaOH and EA were discharged. 8. The pilot plant was cleaned up.

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5.0 RESULT AND DISCUSSION Table 1 calibration data Calibration data conversion Conductivity 0.1M NaOH 0.0 15.66 0.05M NaOH + 0.05M Sodium Acetate 0.5 9.80 0.1M Sodium Acetate 1.0 6.05

Table 2 Experimental data: flow rate = 40cm3/min Time, Conductivity t (min) 0 6.11 2 6.25 4 7.21 6 7.88 8 9.32 10 11.2 12 10.06 14 11.92 16 9.60 18 9.80 20 9.91 22 8.02 24 8.11 26 8.22 28 8.89 30 8.47 Temp. (oC) 26.0 26.1 26.2 26.1 26.1 26.2 26.3 26.2 26.3 26.3 26.2 26.1 26.1 26.2 26.1 26.2 Conversion (mol) 0.950 0.936 0.837 0.769 0.621 0.427 0.546 0.353 0.594 0.573 0.562 0.758 0.749 0.738 0.668 0.712 CA (mol/L) 0.0043 0.0057 0.0157 0.0227 0.0377 0.0573 0.0454 0.0647 0.0406 0.0427 0.0438 0.0242 0.0251 0.0262 0.0332 0.0288 CB (mol/L) 0.0043 0.0057 0.0157 0.0227 0.0377 0.0573 0.0454 0.0647 0.0406 0.0427 0.0438 0.0242 0.0251 0.0262 0.0332 0.0288 CC (mol/L) 0.0950 0.0936 0.0837 0.0769 0.0621 0.0427 0.0546 0.0353 0.0594 0.0573 0.0562 0.0758 0.0749 0.0738 0.0668 0.0712 CD (mol/L) 0.0950 0.0936 0.0837 0.0769 0.0621 0.0427 0.0546 0.0353 0.0594 0.0573 0.0562 0.0758 0.0749 0.0738 0.0668 0.0712 1/rA x10-5 11.9625 11.7875 10.5375 9.6625 7.7875 5.3375 6.8250 4.4125 7.4250 7.1625 7.0250 9.4750 9.3625 9.2250 8.3500 8.9000

Table 3 Experimental data: flow rate = 60cm3/min Time, t (min) 0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 Conductivity Temp. (oC) 11.95 26.5 10.91 26.6 10.78 26.9 9.85 27.0 9.08 27.0 8.87 27.1 8.62 26.6 8.24 27.1 7.87 27.1 7.65 27.1 7.51 27.0 7.32 26.6 7.19 25.6 6.76 27.0 6.54 27.0 Conversion (mol) 0.349 0.458 0.472 0.568 0.648 0.669 0.696 0.735 0.774 0.797 0.811 0.831 0.845 0.889 0.912 CA (mol/L) 0.0651 0.0542 0.0528 0.0432 0.0532 0.0331 0.0304 0.0265 0.0226 0.0203 0.0189 0.0169 0.0155 0.0111 0.0088 CB (mol/L) 0.0651 0.0542 0.0528 0.0432 0.0532 0.0331 0.0304 0.0265 0.0226 0.0203 0.0189 0.0169 0.0155 0.0111 0.0088 CC (mol/L) 0.0349 0.0458 0.0472 0.0568 0.0648 0.0669 0.0696 0.0735 0.0774 0.0797 0.0811 0.0831 0.0845 0.0889 0.0912 CD (mol/L) 0.0349 0.0458 0.0472 0.0568 0.0648 0.0669 0.0696 0.0735 0.0774 0.0797 0.0811 0.0831 0.0845 0.0889 0.0912 1/rA x10-5 2.9083 3.8167 3.9333 4.7333 5.4000 5.5750 5.8000 6.1250 6.4500 6.6417 6.7583 6.9250 7.0417 7.4083 7.6000
8

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Table 4 Experimental data: flow rate = 100cm3/min Time, t (min) 0 2 4 6 8 10 12 14 16 18 20 22 Conductivity Temp. (oC) 12.9 27.0 11.0 27.1 14.2 27.2 12.2 27.0 11.80 27.2 11.47 27.3 9.75 27.3 9.42 27.3 9.19 27.3 9.08 26.7 9.51 27.5 9.47 27.4 Conversion (mol) 0.251 0.448 0.115 0.323 0.365 0.399 0.578 0.613 0.637 0.648 0.603 0.607 CA (mol/L) 0.0749 0.0552 0.0885 0.0677 0.0635 0.0601 0.0422 0.0387 0.0363 0.0352 0.0392 0.0393 CB (mol/L) 0.0749 0.0552 0.0885 0.0677 0.0635 0.0601 0.0422 0.0387 0.0363 0.0352 0.0392 0.0393 CC (mol/L) 0.0251 0.0448 0.0115 0.0323 0.0365 0.0399 0.0578 0.0613 0.0637 0.0648 0.0603 0.0607 CD (mol/L) 0.0251 0.0448 0.0115 0.0323 0.0365 0.0399 0.0578 0.0613 0.0637 0.0648 0.0603 0.0607 1/rA x10-5 1.2550 2.2400 0.0575 1.6150 1.8250 1.9950 2.8900 3.0650 3.1850 3.2400 3.0150 3.0350

Table 5 Experimental data: flow rate = 120cm3/min Time, t (min) 0 2 4 6 8 10 12 14 16 18 20 Conductivity Temp. (oC) 12.06 27.1 9.29 27.3 10.71 27.4 11.43 27.3 11.24 27.4 10.57 27.3 10.57 27.1 10.44 27.1 10.35 27.1 10.48 26.8 10.33 27.6 Conversion (mol) 0.338 0.626 0.478 0.404 0.423 0.493 0.493 0.507 0.516 0.502 0.518 CA (mol/L) 0.0662 0.0374 0.0522 0.0596 0.0577 0.0507 0.0507 0.0493 0.0484 0.0498 0.0482 CB (mol/L) 0.0662 0.0374 0.0522 0.0596 0.0577 0.0507 0.0507 0.0493 0.0484 0.0498 0.0482 CC (mol/L) 0.0338 0.0626 0.0478 0.0404 0.0423 0.0493 0.0493 0.0507 0.0516 0.0502 0.0518 CD (mol/L) 0.0338 0.0626 0.0478 0.0404 0.0423 0.0493 0.0493 0.0507 0.0516 0.0502 0.0518 1/rA x10-5 1.4083 2.6083 1.9917 1.6833 1.7625 2.0542 2.0542 2.1125 2.1500 2.0917 2.1583

Table 6 Experimental data: space time Flowrate vo 3 (cm /min) 40 60 100 120 Theoretical Space time (min) 50.00 33.33 25.00 16.67 Actual Space time (min) 20 18 12 10 Conductivity Temp. (oC) Conversion X (mol) 0.562 0.797 0.578 0.493

9.91 7.65 9.75 10.57

26.2 27.1 27.3 27.3

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Calculation: Conversion From the calibration curve, straight line equation is Y = -0.1024X + 1.5757 Y - Conversion X Conductivity For the flow rate of 40 cm3/min, conductivity at time t = 2 min is 6.25. Thus the value of conversion is: Y = -0.1024X + 1.5757 = -0.1024(6.25) + 1.5757 = 0.936 Concentration CA=CAo(1-X) CB = CA CC = CAo. X CD = CC where CA = mol/L where CC = mol/L

At, t= 2 min, (flowrate = 40cm3/min), X= 0.936, CAo= 0.1 mol/L CA= CB = 0.1 mol/L x (1-0.936) = 0.0064 mol/L CC= CD = 0.1 mol/L x (0.936) = 0.0936 mol/L rate of reaction, -rA Design equation of the CSTR was used to find the -rA. The equation is as below: vC V - rA o AO X Example : 1/ rA = X / vo Cao V = 0.930 / 40 (0.1)(2000) = 11.962578 x 10-5

Theoretical space time, Theoretical space time can be calculated by using the equation below:
V vo

For flow rate 40 cm3/min, = 2000 cm3 40 cm3/min = 50 min

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