Engineering Growth Connection

Contents
1. Objective 1
2. Aim

3. Introduction

4. Theory 1

5. Description 3

6 Utilities Required 3

7 Experimental Procedure

8. Observation & Calculation 5

9. Nomenclature 6

10. Precautions & Maintenance Instructions 7

7
11. Troubleshooting
8
12. References

13. Block Diagram

sIAGRLF AATCH DISTILLATION

 Engineering Growth Connection

SIMPLE BATCH DISTILLATION

1. OBJECTIVE:

To study the process of simple batch distillation.

2. AIM:

To venfy Rayleigh equation for batch distillation.

3. INTRODUCTION:

Batch distillation is a process by which a mixture of volatile components is partially

separated by evaporation and condensation. The feed mixture is initially charged into the
still (boiler), heated and the vapour emerging from the still is condensed and collected as
distillate. As the distillation proceeds, the liquid in the still becomes more concentrated in
the less volatile component while the distillate tends to have a higher concentration of
the volatile component. The distillate
more can be collected whole
as a or several
fractions can be taken.

4. THEORY:
For simple
batch distillation process, initially the still is filled with F moles of feed with
xe
as the mole fraction of the more volatile
component. Let at any moment the number of
moles of liquid in the still be B having a mole fraction x of the more volatile
component
i.e. A) and let the moles of accumulated condensate be D. Concentration of the
equilibrium vapour is y. Over a small time, the change in the amount of liquid in the still
is dB and the amount of vapour withdrawn is dD. The following differential mass balance
equations may be written:

Total material balance:

dB dDb ..
(1)
Component A balance:

d(Bx) =
y'dD ..(2)

On solving the above equation:

Bdx xdB =
y dD

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 Englneering Growth Connectlon

Put dB= dD from eq" (1):

- Bax = y dD - xdD

- Bdx (y - x)dD

Again put dD = -dB

Bcx (y -x)dB .
(3)
By arranging the above equation:

dB dx
(4)
y-x
Where y is the vapour composition in equilibrium with liquid composition x

Integrating Eq" (4):

(5)
y-x
Eq. (5) is the Rayleigh equation, which describes the variation of the liquid and vapour
mole fractions, x, y in terms of the fraction remaining in the still.

"*** ******* (6)

We have:

aX

1+(a-1)x
For constant relative volatility, a we can write the equation (6)

dx
in X
1+(a-1)x

dx dx (7)
a-1)x(1-x) (1-x)
By partial differentiation ofthe above equation:

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 Engineering Growth Connection

n a-1 XB(1-x) (1-x) L(1-x) a-1 x(1-x)]

InF1-x)1 In X1-Xa)
B(1 Xg)a- Xp(1-x)

ain--in1-x,)1.F-)
B(1-X) x(1-X) B(1-x)

aF1-X)=In
B(1-X BxB (8)

The above eq" is more convenient form of Rayleigh equation.

5. DEsCRIPTION:

The set-up consists of a distillation still. A jacketed heater is provided to heat the feed. A
PID Controller is provided to control the temperature of heater. Condenser is provided to
condensate the vapour. Rotameter is given to measure the flow rate of cold water.
Temperatures sensors with digital temperature indicator is provided. Receiver tank is
given to collect the product

6. UTILITES REQUIRED:

6.1 Electrical Supply: Single Phase, 220 V AC, 50 Hz, 5-15 Amp combined socket
with earth connection. Earth voltage should be less than 5 volts.

6.2 Water Supply: 4 LPM at 1 bar.

6.3 Floor Drain Required.

6.4 Refractrometer for analysis.

6.5 Chemicals
Methanol 4 Ltrs

Distilled water 15 Ltrs

SIMPLE BATCH DISTILLATION

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 erng Growtn Conne

7. ExPERIMENTAL ProCEDURE:

7.1 STARTING ProcEDURE:

7.1.1 Prepare methanol water solution by mixing known amount of water and

methanol.

7.1.2 The total amount of soluton should not be less than 15 lters.

7.1.3 The composition of methanol in soluton should be in the range of 15 to 25

% by volume.

7.1.4 Note down the volume of water and methanol.

7.1.5 Collect sample offeed solution by valve Vs & measure the refractive index.

7.1.6 Close all the valves V1-Vs.

7.1.7 Ensure that switches given on the panel is at OFF posiion.

7.1.8 Fill water in cooling water tank.

7.1.9 Fill the vessel with methanok-water solution by open the valve V, and air

vent valve V2.

7.1.10 Connect electric supply to the set-up.

7.1.11 Set the temperature in PID controler by increment & decrement buttons.
The temperature should be in thee range of 85 to 95 C.

7.1.12 Open the airvent valve V4.

7.1.13 Switch ON the heater and wait 25-30 minute for the system to achieve
steady state.

7.1.14 Close the airvent valve V4

7.1.15 Adjust the cooling waterflow rate by valve V3.

7.1.16 Now take out the samples from the bottom& distillate chamber by open
the valve Vs and Vs.

7.1.17 Cool down the samples to room temperature & measure the refractive

indices
7.1.18 Repeat the experiment for different set point temperatures and
compositions.

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 Engineering Growth Connection

7.2 CLosING ProcEDURE:

7.2.1 When experiment is over stop the water supply.

7.2.2 Switch OFF the heater.

7.2.3 Switch OFF the main power supply.

7.2.4 Drain the vessel by open the valve Ve

8. OBsERVATION & CALCULATION:

8.1.a DATA:1
Relative volatility a 3.32
Molecular weight of methanol M 32 g/mole

8.1.bDATA:2
1.34
1.338
1.336
1.334
1.332
1.33
1.328
1.326
1.324

1322
0.2 0.4 0.6 0.8 1.2

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SIMPLE BATCH DISTILLATION
Page No. 5 of 9 (Rev. 1)
 Engineering Growth Connection

Xthe R.I. (at 25°C)

1.33
0.1 1.3315
0.2 1.3325
0.3
1.3345
0.4 1.336
0.5 1.337
0.66 1.3375
0.75 1.337
0.8 1.3345
0.9 1.3305
1
1.3235

8.2 OBsERVATIONS:
V Lit.

T C

RIp

RI
RIp

8.3 CALCULATIONS:
To calculate the property of methanol (p) at temperature T (C) from data book.

P (kg/m)
Xp From R.I vs. x graph, value of x corresponding to R.

From R.I vs. x graph, value of x corresponding to R.lel

Xg
[From R.I vs. x graph, value of x corresponding to R.lbl
Xp

pV
F (kmole)
Mx1000

SIMPLE BATCH DISTILLATION

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 Engingeríng Growth Connection

B-
Xg Xp
x F (kmole)

aln-x)
B(1-Xa
B(1-X)
9 NoMENCLATURE:

Nom Column Heading Units Type

B Moles of methanol in residue kmole Calculated

E Eror Calculated

F Moles of methanol in feed kmole Calculated

Molecular weight of methanol g/mole Given
Measured
R.le Refractive indexofresidue sample
R.lD Refractiveindex of distillate sample Measured
R.F Refractive index of feed sample Measured

Temperature °C Measured

V Volume of methanol in feed Measured

Xthe Mole fraction of methanol in liquid phase Given

Mole faction of methanol in feed Calculated

Mole fraction of methanol in residue Calculated

Mole fraction of methanol in distillate Calculated

Xp
Relative volatility Given

kg/m Calculated
P Density ofmethanol
Symbols are unitless.

10. PRECAUTION & MAINTENANCE INsTRU

10.1 Heater should not be switch ON before charging the solution in stil.

10.2 Always drain the tanks and re-boiler after the end of experiment.

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 Engineering Growth Connection
10.3 Always use clean water and ensure that there are no foreign particles in the flow
stream.

11. TRoUBLESHOOTING:
11.1 In case of any problem regarding operation of the apparatus; the apparatus
should be quickly switch OFF and electric supply should be cut OFF.

11.2 Electric shock: It means that either earth wire has loose connection or there is no
earth provided in the socket to which the equipment is plugged in. So make it
sure that the equipment is earthed properly.
11.3 Leakage: The point of leakage should be detected & the concermed part is
tightened properly. If the problem persists then that part should be remove&
teflon tape is wrapped on the threads properly and refitted carefully.

12. REFERENCES:
12.1 McCabe, Waren L Smith, Julian C. Harriot, Peter (2005). Unit Operations of
Chemical Engineering. 7h Ed. NY: McGraw-Hill. pp 724-727.

Dutta K. Binay (2007). Principles of Mass Transfer and Separation Processes.

12.2
ND: Prentice Hall of India Pvt. Ltd. pp 353-355, 391.

iDISTUiATION
 Engineern Growth Connection

13. BLOCK DIAGRAM:

T4 V4
cONDENSER
cOLD WATER

OUTLET T
COLD WATER
INLET DISTILLATE
CHAMSERR
cONTROL
PANNEL
V5

cOLD WATER TO
ROTAMETER
cONDENSER
PRESSURE V3

GAUGE
cOLD WATER INLETT
SUPPLY
FUNNEL SAFETY VALVE

V1
V2
LEVEL INDICATOR -

VESSEL

S.NO VAIVES
1. V1-FEED SUPPLY VALVE OF FUNNEL
2. v2-AIR VENT VALVE OF VESSEL_
3. V3 -WATER FLOW CON
BLOCK DIAGRAM
V AR VENT VALVE OF CONDENSER
ED NAME SIMPLE BATCH DISTILLATION
6
VALVE FOR DISTILLATE COLLECTION|
V6-DRAIN VALVEOEVESSEL cODE- KCMT -115
SIMPLE BATCH DISTILLATION
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