POLYTECHNIC INSTITUTE

NATIONAL

SCHOOL OF ENGINEERING
CHEMISTRY AND EXTRACTIVE INDUSTRIES

Practice number 2:

Batch rectification of a mixture

binary

Professor: Sergio Torres Pérez.

Student: Ocaranza Gutiérrez Mauricio Eduardo.
Group: 3IM73.
Team 4

Delivery date: March 7, 2019.

Objectives of the practice:

Conceptual
Develop the knowledge to understand the phenomenon of separation of
volatile liquids, through the distillation of a binary mixture in a column
batch rectification adiabatic, combining and comparing the results
experimental with the theoretical calculated from the Rayleigh equation and
to be able to predict the operation times, the masses, and the concentrations obtained.

Procedural
Create the binary equilibrium diagrams of the systems: ethanol-water, as
ideal gas solution and non-ideal gas solution.

Attitudinal
Observe appropriate behavior during the practice by exhibiting
a professional discipline. Conduct research on the references
available on the different applications of the distillation process
Theoretical Introduction
The distillation of binary mixtures is one of the most basic operations.
important in the chemical industry. The purpose of the design of the columns
distillation consists not only in achieving a product with the required quality at a
minimum cost, but a product with a degree of must also be provided
constant purity, even if there is some variation in the composition of the
batch mix (feeding), a quite common occurrence in industries.
Distillation units are essentially made up of one or more stages.
where these two vaporization operations are carried out simultaneously
partial condensation, with three methods of carrying it out: distillation
differential, sudden distillation and rectification; on this occasion, the analysis will focus on the
continuous distillation with rectification.

Batch rectification
Batch distillation is an operation that does not occur in a steady state, due to
to the composition of the raw material loaded that comes from the vaporization the
the content of this compound is decreasing. The above is reflected in the
increase in the temperature of the entire distillation system, due to the fact that in the
the less volatile components are concentrated in the container.
In intermittent distillations, also called batch or differential,
a specific amount of the mixture of interest is loaded onto the equipment so that,
during the operation, one or more compounds are separated from the mixture
A common example corresponds to the distillations that occur in the
laboratories, where the liquid is emptied into a container and heated until boiling.
The steam formed is continuously removed by condensation, which corresponds to the
more volatile compound.
The simplest equipment for batch distillation consists of a tank with
heating system, a condenser, and one or more tanks of
storage for the product. The material is loaded into the tank and its content is
It boils. The vapors are condensed and stored in a collection tank.
The evaporation rate is sometimes controlled to avoid overload.
of the capacitor, but practically no other type of control is required.
This is the reason why some authors refer to this process as
differential distillation.
If the moles of vapor are represented by V, the moles of the residue contained in the
container that boils like W, the fraction of the volatile component in the liquid as
x, y and the fraction of the same component in the gas phase as y, a balance of
material for this compound would give that for an average composition and of a
distilled with dV moles equals:
-ydV = d(Wx) (1)

Assuming a sufficiently small differential change such that the concentration

in the steam it does not vary.
Since the balance for currents corresponds to dV = - dW, when substituting and expanding
himselfhas:
ydW = Wdx + xdW (2)

Rearranging terms and integrating, we obtain:

ln (Wi/Wf) = -∫ dx/(y-x) (3)

Where the subscript i represents the initial composition of the distillation tank and f
the final composition of it.
Equation (3) can be easily integrated for the case when the pressure is
constant, the temperature change of the tank that stores the load is very
small and the equilibrium constant is independent of composition. If it
You know that y = kx, where k is the physical equilibrium constant, and if this were...
approximately constant, Equation (3) would become:
ln (Wi/Wf) = 1/(k-1)ln(x/x
i f) (4)
For a binary mixture, if the relative volatility is assumed to be constant, the
the integration of equation (3) leads to:
Ln (WI/Wf) = 1/(α-1) [ln(xi/xf) +αln((1-xf/(1-xi)) (5)
If the equilibrium relationship y=F(x) is presented in tabular or graphical form for the
since there is no simple analytical solution, equation (3), called the equation of
Rayleigh must be integrated graphically or numerically.
 CALCULATIONS OF BATCH RECTIFICATION PRACTICE OF A BINARY MIXTURE
Ethanol-Water
1.- EXPERIMENTAL AND BIBLIOGRAPHICAL DATA:
= 46 Etanol; = 18 kg
Initial data in the kettle:

∆ℎ ( ) 0 = ( ) 0( ⁄ 3
) %
25.5 35.5 0.986 6

Molar concentration of the mixture:

% 6
46 0.7652
= = = = 0.02436
0 % % 6 94 4.36
+ 46 + 18
= .

0 0 (35.5 L00.986 kg ⁄) 34.817

0= = = = 1.8736 kmol
(
460.02436 )
+18(00.9756 ⁄
kg kmol 22.9084
= .

Note: The volume of purges and samples was≅ 1.5 liters

2.- TOTAL REFLOWS OPERATION DATA:

Samples:

⁄ %
0.82 91.1
0.977 12

( 0 IA = ⁄ (l min)= 0.575
= . ⁄

Note: The reflux is in liters per minute as read from the rotameter at Total Reflux.
Calculation of the molar concentration of the samples at Total Reflux.
% 91.1
46 1.98
= = = = 0.8
% % 91.1 8.9 1.98 +0.494
+ 46 + 18

= .

% 12
= = 46 = 0.0506
% % 12 88
+ 46 + 18
= .

(0.575 L/min00.82 kg )⁄ 0.4715

= 0 = = = = 0.01167 kmol/min
̅̅̅̅̅ ( )+ 18(0.2) kg ⁄
460.8 40.4
= . /

Note: At this stage, 2.0 liters are used for purges and samples.

3.- OPERATION DATA FOR CONSTANT REFLUX RECTIFICATION:

Cut 1

⁄ %
1 0.83 84.0
1 0.977 12.5

Flow in rotameters:
DISTILLATE ROTAMETER 1= 0.01 l/min
REFLUX ROTAMETER 01 0.18 l/min
=

Cut size 1:
Volume = 2.150 liters
Time = 10 minutes
Note: The volume of samples, cuts, and purges was 4.0 liters.
Calculation of mole fractions:

% 84
46 1.826
1= = = = 0.6726
% % 84 16 2.7149
+ 46 + 18
= .

% 12.5
46 0.52174
1 = = = = 0.053
% % 12.5 87.5 4.744
+ +
46 18
= .

Calculation of flow in rotameter of the distillate:

(0.01 L/min0.83 / )
1= = 0.00225 kmol/min
[460.6726
( +) 18(0.3kg/kmol]
= . /

Calculation of flow in rotameter of reflux:

(0.18 L/min0.8292 kg/L
01= = 0.004 kmol/min
[460.6726
( +) 18(0.3kg/kmol]
= . /

Calculation of the reflux ratio at constant reflux:

01 0.004 kmol/min
1= = = 1.8
1 0.00225 kmol/min
= .

Steam flow:

1 = 01+ 1= 0.004 kmol ⁄ + 0.00225 kmol ⁄ = 0.0065 kmol/min

= . /
4.- CALCULATION OF THE MINIMUM NUMBER OF THEORETICAL PLATES (MNPT) AT TOTAL REFLUX,
APPLYING THE GRAPHIC METHOD OF Mc CABE-THIELE.
Required data:
NPR=16

= 0.8 ; = 0.139

Graph and trace the stages on the equilibrium curve as well as the operating line of the
minimum reflux (Rm): GRAPH 1, THEORETICAL PLATE TRAJECTORY OF Mc CABE-THIELE.
Using the data obtained from graph 1, the efficiency is calculated:
NMP - 1 5-1
= ( 100=) = 25%
16
= %

Calculation of minimum reflux (Rm):

Equation of the operating line in the enrichment zone:

= + ; = +
+1 +1
The slope is calculated:
− ′ 0.8 - 0.71 0.09
= = = = = 0.4225
+1 − ′ 0.8 −0.5870.213
= .

0.4225
= = = 0.7315
1 - m 1 -0.4225
= .

Also with the y-intercept (b).

00.8
= = = 0.462
+ 1 0.7315 + 1
= .
Where:
0.8
= -1= - 1 =0.7316
0.462
= .
The minimum reflux value obtained from the slope and the intercept
respectively is very approximate( = . ≅ = . ).

Calculation of the optimal reflux range:

 =( ( )0.7315
1.2= ( 1.2 )( )
= 0.8778
= .

=( ( 0.7315
1.5= ) ( 1.5 =)(1.09725
)
= .

Within this range, the costs are the lowest.

Calculation of the number of theoretical plates obtained with data from cut 1 of a
constant reflux rectification:
Cut 1 Data

⁄ %
1 0.837 81.0
1 0.977 12.5

0= 0.36 l/min =0.0081 kmol/min

= . /

1= 0.215 L/min = 0.00484 kmol/min

= . /

= .

Calculation of the y-intercept:

0.81
= = = 0.303
1+ 1 1.6736 + 1

= .

With the composition of the distillate from cut 1 ( 1and

) the ordinate (b), the line is drawn from
operation and the operational plates are scaled, see graph 2.
With the number of theoretical plates: NPT=8, the overall efficiency of the column is calculated.
 NMP - 1 8−1
= ( 100=) * 100= 430.75%
16
= . %

Calculation of the theoretical average composition of the distillate,( ó ) with data

experimental
( 0 )( 0) −( 1 )( )1
ó =
0− 1

Data:

0 = 41 liters 01.8736 kmol 0

= 0.02436

A total of 7.5 liters were used in samples, purges, and cut 1, therefore:

1
= 41 l - 7.5 = 430.5 L ; = 0.125
1
y ρ = 0.9771 kg ⁄
Therefore:
( 1)( 1) ( 41 ) (0. 977 ⁄ ) 28.32
1= = = 1.863
1 ( 460.125
)( + )18((0.875)
) ⁄ 21.08

= .
:
(1.8736 kmol0125) − (1.863 )(0.02436)
= = 0.793
1.8736 kmol - 1.863
ó = .
= .
Calculation of operating time:

0− 1 0.177 kmol 0.177

- = = =
0.0081 kmol ⁄ 0.00484
V(1 - ) 0.01294 kmol⁄min(1 - )
0.01294 kmol ⁄
= .

+1 1.6736 + 1
2. − = ( 0− 1 )= ( 0.29 kmol =
) 36.57 minutes
0.01294 kmol ⁄
= .

= 62 minutes, considering: multiraid, surgery, lecture and the total reflection.

Layout and use of the integration curve obtained in batch reflux rectification
constant.

The following procedure exists:

1.- Assume values of( ,) starting with the total reflux value( = 0.8)for this
case, towards lower value.

2.- For each assumed value of( ) assume the y-intercept( = +1

) , with the value
obtained from constant reflux of cut 1. (R=1.6736).
3.- once the corresponding values are obtained from , trace the lines on the graph
of equilibrium. They will result in lines parallel to the operation line of cut 1.

With the number of theoretical stages of operation of cut 1 (NET=3), trace the steps in
each operating line and obtain the corresponding values of , using the three
exact steps.
4.- Once the corresponding value is obtained from for each assumed value of ,
calculate the function of (x):
 1
( ) =
−

The following table will be generated with the previous steps:

TABLE 1
STEPS 1 2 3 4
= b= 1
+1 ( ) =
−
0 0.8 0.2992 0.71 11.111
1 0.7 0.2622 0.14 1.786
Data from 0.6726 0.2516 0.092 1.722
practice
2 0.6 0.2244 0.04 1.785
3 0.5 0.1870 0.03 2.127
4 0.4 0.1496 0.02 2.631
5 0.3 0.1122 0.015 3.508

1
5.- Graph against (=) on graph paper (see graph 4)
−

USE OF THE INTEGRATION GRAPH:

If I want to know a = 0.65based on my initial data of:

0 0 (37 l)00.941 kg ⁄) 34.817

0= = = = .
(
460.1753+ )18(0.8297 kgkmol ⁄ 22.9084
Y
% 35.2
46 0.7652
= = = = .
0 % % 35.2 64.8 4.36
+ +
46 18
And assuming a value of for example = 0.05:
With this data in the integration curve, I obtain the values of corresponding
( ) to
these points obtained:

0
= 00.1752 kmol→ =( 2.3
)
 = 0.05 kmol→ 1.8
( )

With these data and with the integration equation using the trapezoidal method, it
calculate( ).

TRAPEZOID METHOD.
1
ln( =) ∫ =∆ [ ]
0 − −
0

The integration is the area under the curve of y 0

, but it also goes through points 2 and
3 (see graph 4), therefore substituting we have s:
( 2.3+ 1.8+) 1.8( + 1.786+ (1.786
) + 1.722)
ln( =) (0.05 -01752[ ]
0 6

(
ln( =) −0.1252 )[
1.8656= ]
−0.2336
0

−0.2336 0 1.52 kmol

∴ = ; = = 1.2 kmol
0
0.2336 1.26314
= .

á
( 0)( )0 − ( )( ) (
1.520.1752 )
−1.20.05 ( kmol
)
= = = 0.645
0− ( 1.52 − 1.2 )
= .

á ( = ).
0− 1 ( 1.52 − 1.2 )
= = 66.116 minutes
V(1 - ) 0.00484 kmol min⁄

= .

If it is necessary to know the exact value of = 0.65a value of is estimated a

a little smaller and the same calculations are done again, that is, by trial and error.
Observations

The operation was carried out irregularly due to technical problems.

foreign to our team and our teacher, since the water services
they did not function regularly.
The rotameters did not reach the minimum flow rate to be able to perform
the measurements correctly.
Physical relationships were used for the percentages, weights, and moles.
determine them indirectly.
The concentration of ethanol increased in each cut.
The instrumentation in this equipment is placed in such a way that it allows us
allows us to understand the magnitudes of the variables necessary to understand and
analyze the process.

Conclusions

There are a series of very specific conditions involved in the

operation of batch binary distillation, such as temperature, the
flow relationships, pressure, etc.
The data obtained in the practice were measured with great difficulty
due to technical difficulties, which resulted in an obstacle for
the calculations corresponding to this practice.
The utility of batch binary rectification was verified and how it operates.
to achieve the desired separation.
Graphical methods are extremely useful and necessary in this type.
of problems.
One must be careful with the graphical method in order to carry out a good
layout, and therefore a good reading.