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ABSTRACT/SUMMARY

This experiment is conducted to carry out conversion determination on experiment samples
manually to verity the conductivity measurement values, determine the effect of residence time
onto the reaction extent of conversion and the reaction rate constant. In order to accomplish the
objective, the unit being used to perform this experiment is CSTR 40L. The design of the reactor
is very important to the success of the production. In this experiment sodium hydroxide and ethyl
acetate react in continuous stirred tank reactor. Both of reactants feed to the reactor at equimolar
flow rate for a certain time.
Form graph 1 it shows that conductivity is decrease proportionally with conversion. For the
graph 2 the result shows that, when residence time is increase, conversion also increase by
lowering the flow rate. The higher conversion is 92.4% at 200 min residence time and 0.2
mL/min total flow rate of solution. It can be conclude that the higher the flow rate, the smaller
the reaction rate constant and rate of reaction become highest.

INTRODUCTION
In the industrial chemical process, mostly a reactor is the key part of equipment in which raw
material undergoes a chemical change to form desired product. The design and operation of
chemical reactor is thus crucial to the whole success of the industrial operation. There are many
type of reactor depending on the nature of the feed materials and products.
Reactor is the heart of any process in industry. Reactor can be classified into two types;
continuous stirred tank reactor and a plug flow reactor. Both of this type of reactor can be operate
in a continuous and a batch mode depending on the nature of the reaction. Reactor can be equips
with a heating or cooling coil for heating process or cooling process. It is depending on the
nature of reaction which is exothermic or endothermic. A reactor also can be equip with bed of
catalyst for a better reaction processes.

Reactor is one of the most important parts in industrial sector. Reactor is equipment that changes
the raw material to the product that we want. A good reactor will give a high production and
economical. One of criteria to choose or to design a good reactor is to know the effectiveness of
the reactor itself. There a many types of reactor depending on the nature of the feed materials and
products. One of the most important in the various chemical reactions was the rate of the
reaction.

Material balance of a general chemical reaction described below.(rate of A out of volume element) + (rate of A produced within volume element) = (rate of A accumulated within vol. The key or main feature of this reactor is that mixing is complete so that properties such as temperature and concentration of the reaction mixture are uniform in all parts of the vessel. The conservation principle requires that the mass of species A in an element of reactor volume dV obeys the following statement described below. element) . (Rate of A into volume element) .A stirred tank reactor (STR) may be operated either as a batch reactor or as a steady state flow reactor (CSTR).

To verify the conductivity values by manual determination on experimental samples. 3.To determine the reaction rate constant . 2.OBJECTIVES 1.To determine the effect of residence time onto the reaction extent of conversion.

[P] and [Q] are referred to the molarity of the substances. Consider the chemical reaction as below: The lowercase letter which are a.p. [B]. r in the chemical reaction is occur in a closed system which is under a constant–volume conditions. The mass balance for any system in general is: IN .and q refer to the stoichiometric coefficient while the capital letter which are A.B.P and Q refer to the reactants and products.b. hence given a control volume V the sum of mass flows entering the system will be equal to the sum exiting minus (plus) the consumed (generated) or accumulated fractions.THEORY Rate of equation and rate law The rate of reactions or speed of reaction for a reactant and products in particular reaction scan be defined as how fast or slow the reaction takes place. According to the IUPAC’s Gold Book definition the rate of reaction. without build up of reaction intermediates. For examples is about the oxidation process between iron under the atmospheric is undergoes a slow reaction compare to the combustion of butane in a fire that can be categories as fast reaction. is defines as: Where [A]. Based on IUPAC the times must be in second and the rate of reaction is in a positive sign. .OUT + GENERATION -CONSUMPTION= ACCUMULATION Mass is a conservative entity.

It is an open system where material is free to enter or exit the system and runs at steady state with continuous flow of reactants and products. density. so the contents have relatively uniform properties such as temperature. Systems connecting several CSTRs are used when the reaction is too slow. CSTRs are very well mixed. where the condition in the reactor don’t change with time. General Mole Balance Equation . while product are continuously removed and assumes a uniform composition throughout the reactor.Continuous Stirred Tank Reactors (CSTR) A stirred-tank reactor (STR) may be operated either as a batch reactor or as a steady-state flow reactor which is better known as Continuous Stirred-Tank Reactor (CSTR). Also. The reactants are continuously introduced into the reactor. The key or main feature of this reactor is that mixing is complete so that properties such as temperature and concentration of the reaction mixture are uniform in all parts of the vessel. CSTR is the most basic of the continuous reactors used in chemical process. and concentration. Multiple CSTRs can also be used when two immicible liquids or viscous liquids are present and require a high agitation rate. conditions in the reactor's exit stream are the same as those inside the tank.

The curve is constructed by measuring the concentration and absorbance of several prepared solutions. with the concentration of solution plotted on the x-axis and the observable variable—for example. X = (FAo–FA) / FAo V = (FAoX) / -rA A calibration curve is a method used in analytical chemistry to determine the concentration of an unknown sample solution. V = (FAo–FA)/ -rA In terms of conversion. called calibration standards. Rearranging the generation. Once the curve has been plotted. the concentration of the unknown solution can be determined by placing it on the curve based on its absorbance or other observable variable. therefore dNA/dt = 0 Well-mixed therefore is the same throughout the reactor. It is a graph generated by experimental means. the solution’s absorbance—plotted on the y-axis.Assumptions Steady state. .

but in estimating the yield of a given reaction and designing future reactors. .Residence Time The reactor’s residence time is defined as the reactor volume divided by the total feed flow rates. Residence time is a probability distribution function that describes the amount of time a fluid element could spend inside the reactor. This is useful. not only for troubleshooting existing reactors. Residence time widely use to characterize the mixing and flow within reactors and to compare the behavior of real reactors to their ideal models.

1M) II-Ethyl acetate.1M) III-Deionised water IV-Phenolphthalein 6. . Conical flask 5. 200 mL beaker 4. 50 mL burette 3. Continuous stirred tank reactor. Model: BP 143 2. Et (Ac) (0. 100 mL measuring cylinder. NaOH (0.APPARATUS 1. Solution : I-Sodium hydroxide. Conductivity probe 7.

V7. All the valves was ensured initially closed. V3. V8 and V11 was opened. The following solutions have been prepared for the expirement: a) 40 L of sodium hydroxide. 4. 3. 4. b) NaOH solution was carefully pour into vessel B1 and the Et(Ac) solution into vessel B2. HCL (0. V7 and V8. The power was turn on for the control panel. The cooling water valve V13 was open to allow the cooling water to continue flowing. c) The charge port caps closed for both vessels. (Only for Experiment 2) 7. Both pumps P1 and P2 was switch off. The unit is now ready for experiment. V3. 2. 6. Let the liquid in the reaction vessel R1 cool down to room temperature. Preparation of Calibration Curve for Conversion vs Conductivity: .1M) b) 40 L of ethyl acetate. Adjusted the overflow tube to give a working volume of 10 L in the reactor R1. 5. The feed vessels was charged as follows: a) The charge port caps was opened for vessels B1 and B2. 9. Refill if necessary. 6. V9 and V12 was open to drain any liquid from the unit. The power was turn off for the control panel. Checked that there is sufficient water in the thermostat T1 tank. 3.OPERATING PROCEDURES General Start-Up Procedures 1. Then. Closed valves V2. NaOH (0. Valves V4. General Shut-Down Procedures 1. 8. Et(Ac) (0. The thermostat T1 was switch off. Opened cooling water valve V13 and let the cooling water flow through the condenser W1. switch off stirrer M1. for quenching 2. 5.1M) c) 1 L of hydrochloric acid. Closed cooling water valve V13. The valves V2.25M).

2. 2.1 L of sodium acetate .1 L of sodium hydroxide.A few drops of pH indicator were added into the mixture. i.1M) iii. 4.1 M NaOH solution.1M) ii.25% cinversion : 75 mL NaOH + 25 mL Et (Ac) iii. 5.1 L of deionised water.75% conversion : 23 mL NaOH + 75 mL Et (Ac) v. Et (Ac) (0.50% conversion : 50 mL NaOH + 50 mL Et (Ac) iv. The amount of NaOH titrated was recorded. NaOH (0.The following solution were prepared: i.0% conversion : 100 mL NaOH ii. H2O. 3. The conductivity and NaOH concentration for each value were determined by mixing the following solution into 100 mL of deionised water.The mixture was titrated with NaOH solution from the burette until the mixture was neutralized.A 50 mL sample was obtained from the experiment and immediate the sample was added to the HCl in the flask to quench the saponification reaction.25 M HCl was measured in a flask.10 mL of 0.1. .A burette was filled up with 0.100% conversion : 100 mL Et (Ac) Experiment 1: Back Titration Procedures for Manual Conversion Determination: 1.

0.20. It directly proceed with the back titration procedures to manually determine the concentration of NaOH in the reactor and extent of conversion. and 0. The stirrer M1 was switched on and the speed was set about 200 rpm. The flow rate was recorded into a data.25.The experiments was repeated (steps 5-9) for different residence times by adjusting the feed flow rate of NaOH and Et(Ac) to about 0. 3. 2. This is to ensure that the reactor has reached steady state.15. 7. the flow rate for both valves must be same. 0.Pump 1 and pump 2 were switched on and valves V5 and V10 were opened to obtain the highest possible flow rate into the reactor. The steady state conductivity value was recorded and the concentration of NaOH andextent of conversion in the reactor was found out from the calibration curve. 9. 5. The conductivity value at Q1 was started monitoring until it does not change over time. Sampling valve V12 was opened and 100mL of sample was collected.1 L/min. 6.The general start-up procedures was performed. . the flow rate for both must be same.Valves V5 and V10 were readjusted to give a flow rate of about 0.The reactor was filled up with both of the solution until it is just about to overflow. 8. 4.Experiment 2: Effect of Residence Time of The Reaction in a CSTR: 1.30 L/min.

01 2.99 Conductivity (ms/cm) Linear (Conductivity (ms/cm)) 5 0 0% 50% 100% 150% Conversion % Graph 1: Calibration curve for conductivity vs conversion Back titration for manual conversion determination: .0000 (ms/cm) 14.Results Table for preparation of calibration curve Conductivit Conversion Solution Mixtures 0.1 0% 25% 50% 75% 100% 0.0500 0.81x + 14.57 7.3 R² = 0.48 10.0250 0.0375 0.14.1 Conductivity vs Conversion 20 15 Conductivity (ms/cm) 10 f(x) = .1 M NaOH 100mL 75mL 50mL 25mL Concentration y M Et (Ac) H2O 100mL 100mL 100mL 100mL 100mL 25mL 50mL 75mL 100mL of NaOH (M) 0.31 0.0125 0.

01120 0.10 0. y concentration .67 Reaction rate constant.0 18.00 66.10 2.000378 0.33 100.30 200.4 .6 76.4 84.21 3.min) 0.10 0. -r (M-1min-1) 15. Flow rate of Flow rate of Resisdence Conductivit Exit Conversion NaOH Et(Ac) time.Sample 1 2 3 4 5 Vol. k Rate of reaction.10 M No.4 19.10 M Concentration of Et(Ac) in feed vessel = 0.20 0.30 3.000318 0.000475 A 92.15 0.25 0.000231 0.25 0. X (%) (mL/min) (mL/min) τ (min) (mS/cm) of NaOH. 2.CNaOH 1.20 0.2 19.8 77.507 3.00038 0.00 133.297 (mol/L.1 21.41 3. 1. 3.0 74.00760 0.997 5.30 0.6 Table of experiment 1 and 2: Reactor volume = 40 L Concentration of NaOH in feed vessel = 0.00 80. 4.01200 0.012 3. 5.01280 0.78 (M) 0.15 0. of NaOH (mL) 23.

000558 Residence time vs Conversion 100 90 80 70 60 Residence time.4055 0.3.τ (min) Conversion.2 L/min Known quantities: Volume of sample.1+0. Vs= 50 mL 160 180 200 220 . X (%) 50 40 30 20 10 0 60 80 100 120 140 Graph 2: residence time vs conversion SAMPLE CALCULATIONS 1) F0= 0.1 = 0.

CHCls= 0. V1= 9.76 iv.24 mL iii.Concentration of NaOH in the feed vessel. CNaOH.1 = 9.1 mol/L Volume of HCL for quenching. CNaOHo. Concentration of NaOH that entering the reactor.8 mL Concentration of NaOH used for titration. C NaOHo= ½ C NaOHf = ½ (0.05 mol/L ii. CNaOHs= 0. n1 n1= (CHCls x V3) / 1000 = 0.24 = 0.25) x 23. Moles of HCl reacted with NaOH in sample.1/0.1 mol/L I. V3 V3= VHCls – V2 = 10 – 9. VHCl.s= 10 mL Concentration of HCl in standard solution.V2 V2= (C NaOHs/ CHCls) x V1 = (0.25 x 0. Volume of unreacted quenching HCl.76/1000 .1) = 0.f = 0. Volume of HCl reacted with NaOHin sample.25 mol/L Volume of titrated NaOH.

CNaOH C NaOH= n2/Vs x 1000 = 0. Residence time. Concentration of unreacted NaOH in the reactor. Conversion of NaOH in the reactor. k k = ( CAo – CA) / τCA2 = ( 0.0038/0.05) x 100% = 92.05 – 0.0038 mol/L Vii. Moles of unreacted NaOH in sample.4 % Viii.C NaOH/ C NaOHo) x 100% = (1– 0. Reaction rate constant.0062) = 15.00019 mol v. X X = (1.00019 mol vi. n2 n2= n1 = 0.= 0.0038) / (200 x 0.20 = 200 min ix. τ τ =VCSTR / Fo = 40 / 0.997 M-1min-1 .00019/50 x 1000 = 0.

-r A -r A= kCA2 = 15. to determine the effect of the residence time onto the reaction extent of conversion and lastly to . there are three objectives need to achieve which are to carry out the saponification process between NaOH and Et (Ac) in a CSTR reactor. Rate of reaction.997 x 0.x.00382 DISCUSSION According to the experiment that had been conducted.

Besides. From the data collected. As the result for rates of constant is not correspond to the theory. This can conclude that the experiment was successfully conducted since it give the right and verified result. But there are certain fluctuated peak which due to the error that may be affects the result and graph. the positions of the eyes must be parallel to the meniscus.by doing all these precaution. thus there are some errors occurred during this experiment such as while taking the reading of the burette the position of the eyes is not at the same level of the meniscus. to improve the reading and get the better results. CONCLUSION Based on the objectives of this experiment. So.01 mS/cm but then it suddenly decrease at 60% conversion until 80% conversion which is give a curve on the graph as shown. For the second graph which is residence time versus conversion. . From the graph 1. It can be conclude that residence is higher if the conversion is higher. This is to ensure that all the beakers. the graph can be concluded that the residence time is increase proportionally to the conversion. which is to determine the residence time on to the reaction extent of conversion. From the calculated data.determine the constant rate of reaction. or burette is clean so that any chemical that we put into these apparatus does not react with any others chemicals.10 L/min. controlled the valve carefully and slowly when adjusting the flow rate to obtain 0. it shows that the conductivity is constantly decreasing which are the line is inversely proportional until at 50% conversion which is the conductivity is 7. two graph had been plotted which are conductivity versus conversion and residence time versus conversion. Make sure reactor does not have any leaks and valve closed and opened as needed. we can get more accurate reading and thus improve the results. RECOMMENDATIONS 1. the relationship conversion and residence time was directly proportional. the rate constant of reaction is increasing when the conversion is higher. But the reaction rates constant were determined for all varies flow rate. we have to rinse all the apparatus before we use it. It is to make sure flow rate will stabilize and the experiment will run smoothly.

com/doc/143019471/cstr-40-L (24/03/2016) (3) http://www. Make sure CSTR 40 liters machine is running appropriately. REFERENCES · APPENDICES (1) http://www.scribd. 5.scribd. it to prevent harm to the machine and individual that used the machine.slideshare. 4. Divide into two teams which is the first team in charge of the CSTR 40 liters machine while the second team would carry out the back titration procedures. 3. Take conductivity reading when the conductivity not changes in time because it can change rapidly in short of time. Repeat titrations two or three times because a lot of error comes from titration or use another method other than titration.net/errafatiha/experiment-cstr-40l (24/03/2016) .2.com/doc/143019471/cstr-40-L#scribd (18/03/2016) (2) http://www.

wikipedia.(4) https://en.org/wiki/Continuous_stirred-tank_reactor (24/03/2016) (5) https://en.org/wiki/Residence_time_distribution (28/03/2016) .wikipedia.