Untitled

Objective: To observe the operation of batch distillation.
Aim: (a)To determine the number of theoretical plates needed for total reflux operation in the distillation
column.
(b) To draw the calibration curves for density and refractive index in relation to volume fraction.
(c) To determine the still's composition when distillation is conducted in partial reflux .
Introduction:
Batch distillation is the method of separating mixtures based on differences in their volatilities in a boiling liquid
mixture. The components in a sample mixture are vaporised by the application of heat and then cooled by the
action of cold water in a condenser. The process is often carried out in a distillation column that has packing or
trays to increase the surface area for vapor-liquid contact and improve separation efficiency.
Theory:
Batch distillation involves heating a batch of liquid in the still, returning some of the condensed distillate as reflux
after the vapours have reached the condensing apparatus. The material in the still degrades as top product take
off occurs, becoming less rich in the more volatile component(s). As a result, as distillation progresses, the reflux
ratio must be raised to preserve the top-product quality, or compromise must be made in the sharpness of
separation.
In continuous fractional distillation, the Fenske equation is used to determine the minimal number of theoretical
plates needed for a fractionation column operating at complete reflux to separate a binary feed stream.
Where, α = Relative volatility ; N = Theoretical plates
xp = Product concentration, mole fraction.
xs = Final still concentration, mole fraction.
If the column is operated at a fixed known reflux ratio, then the product concentration varies during the cycle. The
variation of product concentration with amount of liquid remaining in the still is given by
Where, S1= initial batch charge, moles
S2=residue in kettle at the end, moles
For the creation of high purity and added value goods, batch distillation is frequently employed for the separation
of speciality and fine chemicals as well as for the recovery of small amounts of solvent.
Materials and apparatus:
Ethanol-Water binary system, Thermometer, Test tube, Weighing machine, Thermocouple, Refractometer
Dropper, Beakers.
Experimental Setup: Refractometer:

Cycle Timer:
Line Diagram
Procedure:
1. The volume of each sample should be 10 ml. Make samples of 20%, 40%, 60%, and 80% (volume-by-
volume) ethanol-water mixture and record the weight and refractive index using a weighing scale and a
refractometer, respectively. Make the calibration curve for Refractive Index vs. Vol% of Ethanol using
this data.
2. Calculate the quantity of the ethanol and water mixture, add it to the still, and begin heating.
3. Take distillate and bottom samples (Xp and Xs) every 20 and 25 minutes, respectively, while running the
column in total reflux mode.
4. Measure the substantial data, such as the top and bottom temperatures, the specific gravities of the
samples taken from the top and bottom streams, and the cooling water and reflux rates.
5. Note the weight of the still sample.
6. Run the column once more with a partial reflux ratio. Every time at a 10 to 15 minute interval, note the
values of the same quantities as in step 4's recording.
7. Plot the graph with the relevant information obtained.
Observations & RESULTS:
S.G. vs x
1
0.95
0.9
S.G.
0.85
0.8
0.75
0.000 0.100 0.200 0.300 0.400 0.500 0.600 0.700 0.800 0.900 1.000
x (mole fraction, ethanol)
R.I. vs x
1.37 y = -0.0705x2 + 0.092x + 1.3362
1.365
1.36
1.355
R.I.
1.35
1.345
1.34
1.335
1.33
0.000 0.100 0.200 0.300 0.400 0.500 0.600 0.700 0.800 0.900 1.000
x (mole fraction, ethanol)
S.G. vs vol. frac.

1.05
0.95
S.G.
0.9
y = -0.2245x + 1.024
0.85
0.8
0.75
0 0.2 0.4 0.6 0.8 1 1.2
Ethanol (vol. frac.)
1/(xp-xs) vs xs
1.600
1.400
1.200 y = 2.15x + 1.077
1.000
1/(xp-xs)
0.800
0.600
0.400
0.200
0.000
0.100 0.120 0.140 0.160 0.180 0.200 0.220
xs
SAMPLE CALCULATIONS
(a) For Total Reflux

(b) For Partial Reflux
Precaution:
1. Wait until the sample is cooled down. We can put the beaker in water to cool down its
temperature.
2. While operating the refractometer, ensure that it is clean.
3. Use filter paper and wait for appropriate time until the procedure is completed. As the machines are old
and have been used for long time there might be a chance of getting an impurity in it. Thus, it is advised
to use this filtration process.
Conclusion:
From Graph we can observe:
1. For Total Reflux

• Still density increases with time.
• Distillate density decreases with time.
2. For Partial Reflux

• Still density increases with time.
• Distillate density decreases with time.
3. The still density is greater than feed and

distillate density is less than feed.
Results:
1. Minimum number of Theoretical stages required is 4 which is less than actual number of
stages i.e. 21.
2. The no. of moles left in the still for the column under a partial reflux (reflux ratio=2) is
62.47 to an initial value of 70.28.
LAB WORK:-

Untitled

Uploaded by

Copyright:

Available Formats

Untitled

Uploaded by

Document Information

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Untitled

Uploaded by

Copyright:

Available Formats

Objective: To observe the operation of batch distillation.

Where, α = Relative volatility ; N = Theoretical plates

xp = Product concentration, mole fraction.

xs = Final still concentration, mole fraction.

Where, S1= initial batch charge, moles

S2=residue in kettle at the end, moles

Materials and apparatus:

Experimental Setup: Refractometer:

S.G. vs vol. frac.

1.200 y = 2.15x + 1.077

(a) For Total Reflux

2. While operating the refractometer, ensure that it is clean.

From Graph we can observe:

1. For Total Reflux

2. For Partial Reflux

3. The still density is greater than feed and

You might also like