REACTION IN CSTR

[SAPONIFICATION (2ND ORDER) REACTION]

Aim: To predict the CSTR performance for second order saponification reaction during
steady state condition.

Apparatus:
 Containers for reagents and product
 Magnetic stirrer
 Conductivity cell
 Stop watch
 Graduated cylinder

Chemicals:
 0.05 N NaOH solution
 0.05 N ethyl acetate solution

Experimental procedure:
1. Calibrate the Conductivity cell as given in the appendix.
2. Prepare 2 litres of each 0.05 N NaOH solution and 0.05 N ethyl acetate solution
3. Pour the solution into two overhead storage tanks
4. Measure the flow rates of NaOH and Ethyl acetate and maintain them such that NaOH
will be limiting reactant (𝜗𝜗NaOH < 𝜗𝜗EA).
5. Start measuring conductivity with time
6. Note the time when flow becomes steady
7. Continue to take readings of conductivity till you get nearly constant readings of
conductivity for approximately 2 min.
8. After getting constant conductivity stop the flow of both solutions and the magnetic
stirrer
Theory:

Diagram:

Reaction:

NaOH CH3COOC2H5 CH3COONa C2H5OH

(A) (B) (C) (D)

For CSTR mass balance is given as:

𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼 = 𝑂𝑂𝑂𝑂𝑂𝑂𝑂𝑂𝑂𝑂𝑂𝑂 + 𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷 𝑏𝑏𝑏𝑏 𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟 + 𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴𝐴 (1)

𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼 𝑜𝑜𝑜𝑜 𝐴𝐴, 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚⁄𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡 = 𝐹𝐹𝐴𝐴0 (1 − 𝑋𝑋𝐴𝐴0 ) = 𝐹𝐹𝐴𝐴0 (2)

𝑂𝑂𝑂𝑂𝑂𝑂𝑂𝑂𝑂𝑂𝑂𝑂 𝑜𝑜𝑜𝑜 𝐴𝐴, 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚⁄𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡 = 𝐹𝐹𝐴𝐴 = 𝐹𝐹𝐴𝐴0 (1 − 𝑋𝑋𝐴𝐴 ) (3)

𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷 𝑜𝑜𝑜𝑜 𝐴𝐴 𝑏𝑏𝑏𝑏 𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟 𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚⁄𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡 = (−𝑟𝑟𝐴𝐴 )𝑉𝑉 (4)

Introducing these three terms in above mass balance equation we get,

𝐹𝐹𝐴𝐴0 𝑋𝑋𝐴𝐴 = (−𝑟𝑟𝐴𝐴 )𝑉𝑉 (5)

Therefore we get,
𝑉𝑉(−𝑟𝑟 𝐴𝐴 )
𝑋𝑋𝐴𝐴 = (6)
𝐹𝐹𝐴𝐴 0

Now we have to put value of (-rA) in above equation. But this reaction is reversible reaction.
Therefore,
𝐶𝐶𝐶𝐶 ∗𝐶𝐶𝐷𝐷
−𝑟𝑟𝐴𝐴 = 𝐾𝐾[𝐶𝐶𝐴𝐴 ∗ 𝐶𝐶𝐵𝐵 − ] (7)
𝐾𝐾𝑒𝑒

Where,
𝐶𝐶𝐴𝐴 = 𝐶𝐶𝐴𝐴0 (1 − 𝑋𝑋𝐴𝐴 ) (8)
𝐶𝐶𝐴𝐴 = 𝐶𝐶𝐴𝐴0 (𝜃𝜃 − 𝑋𝑋𝐴𝐴 ) (9)
𝐶𝐶𝐶𝐶 = 𝐶𝐶𝐴𝐴0 ∗ 𝑋𝑋𝐴𝐴 (10)
𝐶𝐶𝐷𝐷 = 𝐶𝐶𝐴𝐴0 ∗ 𝑋𝑋𝐴𝐴 (11)
Therefore we get,
𝑉𝑉 𝑋𝑋 𝐴𝐴
= 𝑋𝑋 2
(12)
𝐹𝐹𝐴𝐴 0
𝐾𝐾∗𝐶𝐶𝐴𝐴2 0 ∗[(1−𝑋𝑋 𝐴𝐴 )∗(𝜃𝜃−𝑋𝑋 𝐴𝐴 )− 𝐴𝐴 ]
𝐾𝐾 𝑒𝑒

As values of FA0, k, CA0, CB0, V and 𝜗𝜗 are known to us from equation (8) we can find out the
predicted value of XA.

Observations:

 𝜗𝜗1 = ........ litre/sec

 𝜗𝜗2 = .......... litre/sec
 𝜗𝜗 = 𝜗𝜗1 + 𝜗𝜗2 = ........ litre/sec
 k =........ litre/(mole.sec)
 CA0 =........ moles/litre
 CB0 = .......... moles/litre
 C0= ........ moles/litre
 V = ......... litre
 FA0 = ...... moles/sec

Observation Table:

Sr. No. Time (t) Conductivity Concentration (CAs)

1.
2.
3.
4.

Results:

1. Predicted value of conversion XA = ..........

2. Experimental value of conversion XA = ..........

Expectations:

1. Lab report in hand written format

2. Plot Calibration curve (MS Excel) and obtain the Calibration equation
3. Observation table, calculations of steady state reaction conversion: Xpredicted and
Xexperimental.
4. Your own conclusions and discussing the results obtained in hand written format
5. Submit all the soft copies along with the plots to the concerned TA

Appendix:

 Procedure for calibration of conductivity cell:

1. Take 50 ml of 0.05 N NaOH solution in a beaker.
2. Insert the conductivity cell in standard solution (0.05 N NaOH solution)
3. Then add some water (say 50 ml) to the solution. Thus, the concentration
decreases by half 0.025 N.
4. Measure the conductivity of this dilute solution.
5. Repeat the procedure to obtain 5 points including one of 0.05 N NaOH and one of
0.0 N NaOH (water) in the range of 0.05 N to 0.00 N.
  Generate the Calibration curve and the calibration equation

Conductivity vs Normality y = 0.034x - 0.004

0.06 R² = 0.995

0.05
0.04
Normality

0.03
Conductivity
0.02
Linear (Conductivity)
0.01
0
0 0.5 1 1.5 2
Conductivity

Use the calibration equation to calculate the value of concentration for the
conductivity values obtained during performance of the experiment.

Questions to think:

• Why it is necessary to calibrate every device before taking actual readings?

• Why do we measure NaOH conversion only and not ethyl acetate?
• How the reversibility of saponification reaction can affect the final conversion?
• What are the other ways to measure conversion?
• What do you mean by limiting reactant?
• Why the volumetric flow rate of NaOH is kept lower that of ethyl acetate?
• What do you mean by equilibrium state of reaction?