EXPERIMENT 3

BATCH (DIFFERENTIAL DISTILLATION)

NAME-SAANA TANDON

ENROLMENT NUMBER-20118072

1. Objective
To verify the Rayleigh equation for a differential distillation in a binary system.
2. Utility and Equipment
1. Heating mantle, condenser and storage vessel
2. Test tubes for sampling
3. Electricity Supply: Single Phase, 220 V AC, 50 Hz, 6.5 kW with earth connection.
4. Water Supply. 2 LPM at 5m head.
5. Refractometer for analysis.
3. Chemicals required
1. Distilled water
2. Methanol

4. Theory

The word distillation refers to the physical separation of a mixture into two or more fractions
that have different boiling points. In this method components of a solution are separated
depending upon distribution of the substances between a gas and a liquid phase, applied to
cases where all components are present in both phases. Distillation differs from absorption and
stripping in that the second fluid phase is usually created by thermal means (vaporization and
condensation) rather than by the introduction of a second phase that may contain an additional
component or components not present in the feed mixture. There are three main methods used
in distillation practice. These are: (a) differential distillation or simple distillation (b) flash or
equilibrium distillation, and (c) rectification.

In the case of a differential distillation, the vapor at any time is in equilibrium with the liquid
from which it rises but changes continuously in the composition. Thus, the mathematical
approach used must be differential. A block diagram for distillation process is shown in Figure
1.
Assume that L mol of liquid in the still of composition x mol fraction A and that an amount dD
mol of distillate is vaporized of mol fraction y* in equilibrium with the liquid. The rate of
depletion of liquid is equal to the rate of distillate output. The instantaneous rate of depletion
of a component in the liquid therefore,

𝐼𝑛 − 𝑂𝑢𝑡 = 𝐴𝑐𝑐𝑢𝑚𝑢𝑙𝑎𝑡𝑖𝑜𝑛 (1)

0 − 𝑑𝐷 = 𝑑𝐿 (2)
0 − 𝑦 ∗ 𝑑𝐷 = 𝑑(𝐿𝑥) (3)
0 − 𝑦 ∗ 𝑑𝐷 = 𝑥𝑑𝐿 + 𝐿𝑑𝑥 (4)
𝑦 ∗ 𝑑𝐿 = 𝑥𝑑𝐿 + 𝐿𝑑𝑥 (5)
𝐹 𝑥𝐹
𝑑𝐿 𝑑𝑥 (6)
∫ =∫ ∗
𝑊 𝐿 𝑥𝑊 𝑦 − 𝑥

Equation (6) after rearrangement can be written in the form known as Rayleigh’s equation, as
follows:
𝑥𝐹
𝐹 𝑑𝑥 (7)
𝑙𝑛 =∫ ∗
𝑊 𝑥𝑊 𝑦 − 𝑥

where, F= moles of feed of composition xF, W= moles of residual liquid of composition xW.
The values of W and xW can be calculated from the material balance, as follows:

𝐹 =𝐷+𝑊 (8)
𝑥𝐹 𝐹 = 𝑥𝐷 𝐷 + 𝑥𝑊 𝑊 (9)

5. Experimental Setup Description

Set up consists of Heating Mantle, Distillation Flask, Condenser and a Distillate collector. A
mixture of known components A and B is fed in the distillation flask and constant heating rate
is supplied by heating mantle. Vapours escaping from the flask are passed through the
condenser and collected in the distillate collector. The schematic diagram for differential
distillation is shown in Figure 2.

6. Procedure
1. Prepare a calibration plot of mole fraction (x) vs. density of pure components A and B.
2. Weigh 8 nos. of tagged stoppered conical flasks.
3. Start the flow of water through the condenser
4. Fill the ¾th (approx 300 ml) volume of the distillation flask with a mixture of A and B
of known composition (xF). The mixture is weighed (w) before charging in the
distillation flask.
5. Start heating at a slow rate. When the mixture starts boiling, collect the distillate in a
weighed 50 ml flask. After approximately 30 ml of the distillate has been collected,
remove the flask and collect next 8 to 10 drops of the distillate in tagged test-tube and
then put another flask for the collection of the distillate. This procedure should be
repeated for collecting 8 distillate samples.
6. Measure the densities of the samples collected in the test-tubes (η1t, η2t…… η12t). Weigh
the samples collected in the conical flasks (ω1, ω2 ……. ω12). Measure the density of
the bulk from each of the flasks (eta1b, eta2b …… eta12b).
7. Observations
Data from Literature:
• Molecular weights of methanol and water are 32 g/mole and 18 g/mole respectively.
• Refractive indices of methanol and water are 1.3284 and 1.333 respectively.
• Density of methanol is 0.792 g/ml.
• Density of water is 1 g/ml.
Calibration data for mole fraction of methanol vs density at 25⁰C:

Sr. no. Mole fraction of Density

methanol (g/ml)
1. 0.1 0.9578
2. 0.2 0.9498
3. 0.3 0.9319
4. 0.4 0.9196
5. 0.5 0.9032
6. 0.6 0.8839
7. 0.7 0.8710
8. 0.8 0.8407
9. 0.9 0.8105
10. 1.0 0.7912

Equilibrium data for methanol-water system:

T (⁰C) x y
100 0 0
96.4 0.02 0.134
93.5 0.04 0.230
91.2 0.06 0.304
89.3 0.08 0.365
87.7 0.10 0.418
84.4 0.15 0.517
81.7 0.20 0.579
78.0 0.30 0.665
 75.3 0.40 0.729
73.1 0.50 0.779
71.2 0.60 0.825
69.3 0.70 0.870
67.5 0.80 0.915
66.0 0.90 0.958
65.0 0.95 0.979
64.5 1.00 1.000

Weight of empty bottle = 20.399 g

Composition of initial sample taken = 300 ml water + 200 ml methanol

S. No. Temperature Weight of Weight of Density (g/ml)

℃ Bottle + 25 ml Solution (g)
solution (g)
1. 81 41.457 21.058 0.84232
2. 84 41.670 21.271 0.85084
3. 86 41.791 21.392 0.85568
4. 87 41.876 21.477 0.85908
5. 89 42.001 21.602 0.86408
6. 91 42.369 21.970 0.87880
7. 94 42.605 22.206 0.88824
8. 97 42.987 22.588 0.90320
9. 99 43.401 23.002 0.92008

Using the calibration data, a graph between density and mole fraction of methanol is
plotted as shown below:
 Calibration Curve for Density vs Composition for Methanol-
Water System
1
0.9
0.8
0.7
Density (g/mL)

0.6
0.5
0.4
0.3
0.2
0.1
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Mole Fraction of Methanol

From the equilibrium data for methanol-water system given above, a T-xy diagram is
plotted as shown below:

Equilibrium Data for Methanol-Water System

100

95

90

85
T (in celsius)

80

75

70

65

60
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Mole Fraction (x,y*)

T-x T-y*

8. Calculations
 Weight
S. of 1/(y*-
F xF D xD W xW y* x ln(F/W)i
No. Solution x)
(g)
1 21.058 21.617 0.2289 0.7229 0.795 20.8941 0.2093 0.59 0.21 0.03401 2.632
2 21.271 21.617 0.2289 0.7355 0.78 20.8815 0.2095 0.52 0.16 0.03462 2.778
3 21.392 21.617 0.2289 0.7469 0.76 20.8701 0.2099 0.46 0.12 0.03516 2.941
4 21.477 21.617 0.2289 0.7536 0.75 20.8634 0.2101 0.43 0.11 0.03548 3.125
5 21.602 21.617 0.2289 0.7655 0.73 20.8515 0.2105 0.37 0.08 0.03605 3.448
6 21.97 21.617 0.2289 0.8149 0.64 20.8021 0.2128 0.31 0.07 0.03843 4.167
7 22.206 21.617 0.2289 0.8502 0.58 20.7668 0.2145 0.14 0.04 0.04012 10.000
8 22.588 21.617 0.2289 0.9035 0.5 20.7135 0.2171 0.06 0.02 0.04270 25.000
9 23.002 21.617 0.2289 0.9805 0.39 20.6365 0.2212 0.02 0.01 0.04642 100.000

Graph Between 1/(y*-x) and x

100.0

90.0

80.0

70.0

60.0
1/(y*-x)

50.0

40.0

30.0

20.0

10.0

0.0
0 0.05 0.1 0.15 0.2 0.25
x
9. Results
The % error obtained for Rayleigh’s equation is 22.279%.

10.Nomenclature

F-Feed flow rate

D-Distillate flow rate
L-moles of liquid
xF-mole fraction of product in feed
xD-mole fraction of product in distillate
xW-mole fraction of product in residue
W-Bottom flow rate
y*-Mole fraction of component A in equilibrium with liquid

11.Precautions and Maintenance Instructions

Heating should be regulated to be sufficiently slow that it can be assumed that the vapors
issuing from the liquid mixture are at all times in equilibrium with the liquid.