Study of a non-catalytic homogeneous reaction in a batch reactor between NaOH and Ethyl Acetate and to determine,
1. Order of the reaction 2. Rate Constant (k) 3. The effect of temperature on k and determine Activation Energy
BATCH REACTOR Page 2 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR APPARATUS REQUIRED Apparatus Quantity i. Measuring cylinder (1000ml) 1 ii. Measuring cylinder (500ml) 1 iii. Pipette (5ml/10ml) 1 iv. Burette (25ml) 1 v. Conical flask (2500ml) 4 vi. Beaker (100ml) 3 vii. Volumetric flask 1 viii. Bucket 2 ix. Mug 1 x. Thermometer 1 xi. Conical funnel 1
REAGENTS REQUIRED Reagents i. NaOH pellets ii. HCl iii. Ethyl acetate iv. Sodium carbonate v. Phenolphthalein indicator
BATCH REACTOR Page 3 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR INTRODUCTION
In the batch reactor the reactants are initially charged into a container, are well mixed and are left to react for a certain period. The resultant mixture is then discharged. This is an unsteady-state operation where composition changes with time; however, at any instant the composition throughout the reactor is uniform.
BATCH REACTOR Page 4 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR THEORY
IDEAL BATCH REACTOR Make a material for any component A. For such an accounting we usually select the limiting component. In a batch reactor, since the composition is uniform throughout at any instant of time, we may make the accounting about the whole reactor. Noting that no fluid enters or leaves the reaction mixture during reaction, which was written for component A, becomes Input = Output + disappearance + accumulation (Eq.1) Evaluating the terms of Eq.1, we find
By replacing these two terms in Eq.1, we obtain
Rearranging and integrating then gives
This is the general equation showing the time required to achieve a conversion XA for either isothermal or non-isothermal operation. The volume of reacting fluid and the reaction rate remain under the integral sign, for in general they both change as reaction proceeds. This equation may be simplified for a number of situations. If the density of the fluid remains constant, we obtain
BATCH REACTOR Page 5 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
For all reactions in which the volume of reacting mixture changes proportionately with conversion, such as in single gas-phase reactions with significant density changes, then it becomes
They are applicable to both isothermal and non isothermal operations. For the latter the variation of rate with temperature, and the variation of temperature with conversion, must be known before solution is possible. Graphical representation of two of these equations Graphical representation of the performance equations for batch reactors, isothermal or nonisothermal Space-Time and Space-Velocity
Just as the reaction time t is the natural performance measure for a batch reactor, so are the space-time and space-velocity the proper performance measures of flow reactors. These terms are defined as follows
Space-time:
BATCH REACTOR Page 6 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
Space- Velocity:
Thus, a space-velocity of 5 hr -l means that five reactor volumes of feed at specified conditions are being fed into the reactor per hour. A space-time of 2min means that every 2 min one reactor volume of feed at specified conditions is being treated by the reactor. Now we may arbitrarily select the temperature, pressure, and state (gas, liquid, or solid) at which we choose to measure the volume of material being fed to the reactor. Certainly, then, the value for space-velocity or space-time depends on the conditions selected. If they are of the stream entering the reactor, the relation between s and r and the other pertinent variables is
It may be more convenient to measure the volumetric feed rate at some standard state, especially when the reactor is to operate at a number of temperatures. If, for example, the material is gaseous when fed to the reactor at high temperature but is liquid at the standard state, care must be taken to specify precisely what state has been chosen. The relation between the space-velocity and space-time for actual feed conditions (unprimed symbols) and at standard conditions (designated by primes) is given by
BATCH REACTOR Page 7 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
In most of what follows, we deal with the space-velocity and space-time based on feed at actual entering conditions; however, the change to any other basis is easily made.
BATCH REACTOR Page 8 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR DIAGRAM
Schematic Diagram of batch reactor
BATCH REACTOR Page 9 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR PROCEDURE
1. Measure the volume of the reactor using water .Let it be V. 2. Prepare 10L of N/40 HCl. Put 20 ml of this into each of the 6 different conical flasks. 3. Put 0.3V of ethyl acetate and NaOH solution one by one into the reactor and switch on the magnetic stirrer. Note down the temperature of the reaction at T o C. 4. After an interval of 5 minutes, withdraw 10 ml of sample through pipette from the reactor and transfer this into the 20 ml of HCL in a conical flask. 5. Titrate 10ml aliquot from the solution against N/100 NaOH using phenolphthalein indicator and note end point. 6. Repeat step 5. To get 5 different sets of sample at an interval of 5 minutes for a total of 30 minutes and analyse them as described in step 6. 7. Repeat the above procedure for two more sets at temperature T+10 o C and T+15 o C. 8. Titrate 10 ml of a mixture (5ml N/100 NaOH + 20ml N/40 HCl+ 5ml M/100 ethyl acetate) against N/100 NaOH using Phenolphthalein as the indicator. The reading of this titration is to be used in the calculation of the C Ao . 9. Ensure that the stock solutions of the individual reactant must have been stirred before using them.
BATCH REACTOR Page 10 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
BATCH REACTOR Page 11 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR CALCULATIONS & GRAPHS
1. CALCULATION FOR C A0 (INITIAL CONCENTRATION) Volume of aliquot sample = 30ml Volume of NaOH consumed = 11.5 ml Volume of HCl consumed in titration = V 1 ml N 1 V I = N 2 V 2
V 1 = ((40/N)*11.5)*(N/100) = 4.6ml Volume of HCl reacted with feed solution V 4 = 20-4.6 = 15.4ml So, concentration of solution initially N 1 V 4 = N 3 V 3
BATCH REACTOR Page 12 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR III. Time = 15 min Volume of aliquot sample = 30ml Volume of NaOH consumed = 13.4 ml Volume of HCl consumed in titration = V 1 ml N 1 V I = N 2 V 2
V 1 = ((40/N)*13.4)*(N/100) = 5.36ml Volume of HCl reacted with feed solution V 4 = 20-5.36 = 14.64ml So, concentration of solution N 1 V 4 = N 3 V 3
Thus for temperature =39.2 o C C A0 =0.0385 mol/lit C A1 =0.0380 mol/lit C A2 =0.0372 mol/lit C A3 =0.0366 mol/lit C A4 =0.0360 mol/lit C A5 =0.0353 mol/lit C A6 =0.0348 mol/lit
3. CALCULATION FOR COCENTRATION AT TEMPERATURE =46.2 o C
I. Time = 5 min Volume of aliquot sample = 30ml Volume of NaOH consumed = 13 ml Volume of HCl consumed in titration = V 1 ml N 1 V I = N 2 V 2
V 1 = ((40/N)*13)*(N/100) = 5.20 ml Volume of HCl reacted with feed solution V 4 = 20-5.20 = 14.80 ml So, concentration of solution N 1 V 4 = N 3 V 3
Thus for temperature =39.2 o C C A0 =0.0385 mol/lit C A1 =0.0370 mol/lit C A2 =0.0360 mol/lit C A3 =0.0351 mol/lit C A4 =0.0346 mol/lit C A5 =0.03405 mol/lit C A6 =0.0337 mol/lit
BATCH REACTOR Page 16 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR 4. GRAPH BETWEEN ln(C Ao /C A ) &TIME
For Temperature =39.2 o C
For Temperature =39.2 o C
0 0.02 0.04 0.06 0.08 0.1 0.12 0 5 10 15 20 25 30 35 l n ( C A o / C A )
Time 0 0.02 0.04 0.06 0.08 0.1 0.12 0.14 0 5 10 15 20 25 30 35 l n ( C A o / C A )
Time
BATCH REACTOR Page 17 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR RESULT
From graphs it is clear that reactions follows first order (because of straight line graph between ln(C Ao /C A ) &time). So, Value of k at Temperature, T=39.6 o C K 1 = Slope of the straight line of graph-1 = 0.0035 min -1
And at Temperature, T= 46.2 o C K 2 = Slope of the straight line of graph-2 = 0.0043 min -1
We know ln (K 1 /K 2 ) = E/R*(1/T 2 -1/T 1 ) where E=Activation Energy and R=constant So, E= 25.8745 KJ/ mol
CONLUSIONS
The performance equation of batch reactors is similar as the PFR reactors. For endothermic reaction as the temperature is increases the rate of the reaction is also increases.
BATCH REACTOR Page 18 DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR PRECAUTIONS
All apparatus should be clean and dry. Note down the readings only after steady state has been attained. Burette reading should be noted carefully. Titrate carefully as end point can come on any one drop.
REFERENCES
i. Octave Levenspiel, Chemical Reaction Engineering., 3 rd edition. ii. Jones, R.W., Chemical Engineering Programme.