DISTILLATION TOWER

Separation Operations and New Tecnologies

Chemical Engineering Program
Faculty of Engineering
Karolaim Vanessa Álvarez – María Angélica Barraza
August 22 2016

Abstract: It has been made a distillation process with an ethanol-water solution in the continuous distillation
column (UOP33CC), operating with a feed flux of 50 mL/min. The product flux, means the enrichment zone and
the depletion zone, were calculated with a mass balance being 35,02 mL/min and 14,94 mL/min. The number of
stages in the distillation column were determined with the graphical method of McCabe-Thiele, using a reflux
ratio of 0,61, it give a number of theorical stages 8 for the distillation column. Equally, a simulation in Aspen Plus
was performed and this give as a resulted 8 stages, with a recovery of 97% regarding the ethanol fed, compared
with the 93% obtained with McCabe-Thiele method. The precision on the results can increase considering the
thermodynamic properties depending on the variation of temperature and quantifying the heat loses in the
depletion zone.

Introduction:

The continuous distillation can be considered, from a simplified viewpoint as a process which carried a series of
stages of flash vaporization, so that produces that the vapor and liquid products of each stage flow in a cocurrent
way; the liquid of a stage, flows to a lower stage and the vapor of an specific stage flows into a higher stage. For
that reason, in each stage enters a vapor stream Y and a liquid stream L, which are mixed and both reach the
equilibrium generating that for an specific stage comes a vapor stream and a liquid stream in equilibrium
[ CITATION Gea98 \l 9226 ]. When a person is design a distillation column, the goal is not only to obtained a
product with an specific quality, also should provide that the product will have a constant value of purity although
some variations occurs in the composition of the mixture, something quite common in the industries that work
with natural raw materials [ CITATION Arn07 \l 9226 ].

The distillation columns have very different sizes because is being able to find columns from 0,3m to 10m in
diameter and since 3m to 75m in high, this values of size could affect the initial flows and in consequence in the
final stage would affect the purity of the substance and the values of final flux in the enrichment and depletion
zone. For our case, the UOP33CC have a process unit height of 2,25m, a process unit width of 0,85m and a
process unit depth of 0,8m; also the control console height have a value of 0,42m, the control console width
corresponds to 0,52m and the control console depth have a value of 0,4m [ CITATION arm \l 9226 ].

As it was indicated, this operation process must evaporate some liquid and for that reason, the distillation
column have to be supply with significant quantities of energy; the amount of energy that is required depends on
the ease of separation of components, which also is influenced by how the liquid and vapor are distributed in the
equilibrium. This distribution depends on volatility or vapor pressure of components, it means that the component
that have a higher value of volatility will tend to move to the vapor phase and the component that have a low
vapor pressure, remain in the liquid phase; the first ones were named, will exit by the top of the column, and the
second ones will exit from the bottom of the column [ CITATION Arn07 \l 9226 ].

McCabe and Thiele have development a mathematical graph method for determining the number of theorical
stages or plates necessary for the separation of a binary mixture; this method uses material balances over
certain parts of the tower and the equilibrium curve xy for the system. The principal thing in the McCabe Thiele
method is that there must be a equimolar leak through the tower between the feed inlet and the upper plate, and
between the feed inlet and the lower plate, in this way the liquid and vapor streams enter to a plate, establish the
equilibrium and leaving the same doing this with all the plates [ CITATION Gea98 \l 9226 ] . In this method, the
equilibrium curve and the operating lines determine the number of theorical plates required for separation and
this is determined by the number of steps that can be draw between the curve and the straights; is clearly that
the number of real plates is higher than theorical plates [ CITATION Jac10 \l 9226 ].
Finally, in the design of the distillation column there is involved the concept of reflux ratio, because the downdraft
reflux facilitates the separation of the components of the mixture because it provides greater contact between
the vapor ascending and liquid and favors low vaporization of the most volatile. That is, a ratio of small reflux
lead to the need for a greater number of plates for a given separation. Greater will the use of fewer dishes, but
their diameters will be greater and operating costs as well. The optimum reflux ratio is given by economic
considerations [ CITATION Arn07 \l 9226 ].

Experimental:

The goal of this practice is to relate the power needed from the reboiler, the pressure drop and the temperature
changes in each tray of the continuous distillation column UOP3CC (Armfiled). For this, a calibration curve with
various concentrations of Ethanol in water was measured with the refractometer to compare with the results
taken from the column in the top, bottoms and the feed tray. We used a feed flow of 50mL/min and a feed
temperature of 20°C. A water cm manometer was used to calculate the drop pressure from the top to the
bottoms. Each change of power from the reboiler the pressure and all 9 temperatures were taken. The first 8
temperatures are from the column stages. The ninth is from the reboiler. The samples were taken from the first
power input of 0.5 kW. With these values, the McCabe-Thiele graph was made and with line iterations the reflux
L/D was found with the L/D= 2(L/D)min. To compare the results obtained with the equipment lecture, the
calculation of Qr was needed and it had to be close to 0.5 kW.
For the simulation experimentation in Aspen, we specify the separation between ethanol and water, taking the
NRTL method and setting the temperature for a value of 20°C, the pressure as a 0,74 atm and the feed flux as a
50mL/min. For this stablished values, the composition of this flow is 0,28834197 for ethanol, the reflux ratio is
0,61 and there is going to be an 8 stages. In the following diagram is presented the simulation of the distillation
continous column

Results:

For the calibration curve in the table Nº#1 are exposed the experimental values that we obtained from the
column distillation, after that, with this values we realized the calibration curve between IR and [vol/vol].

Ethanol
Water (mL) [vol/vol] IR
(mL)
0 1000 1 1,363
100 900 0,9 1,363
200 800 0,8 1,362
300 700 0,7 1,361
400 600 0,6 1,360
500 500 0,5 1,357
600 400 0,4 1,353
700 300 0,3 1,348
800 200 0,2 1,342
900 100 0,1 1,337
1000 0 0 1,317
Table #1. Experimental values
 IR
1.37
f(x) = 0.04 x + 1.33
1.36
1.35
1.34
1.33
IR

1.32
1.31
1.3
1.29
0 0.2 0.4 0.6 0.8 1 1.2
[vol/vol]

Ilustration 1: Calibration curve

With this calibration curve and the lineal equation we can obtained the values of refraction índices and
volumetric in the distillation column.

  IR vol
z 1,3578 0,670103093
Xd 1,3689 0,956185567
Xb 1,3414 0,001
Table #2. Values in distillation column

For the McCabe Thiele diagram, in first place and using the equations of mass balance, we stablished the values
of D and B that are the fluxes in the enrichment and depletion zone. Here we can see the equations for general
mass balance and components mass balance that we used for the calculations.

Feed (mL/min) 50
Z 0,670103093
Xd 0,956185567
Xb 0,001
D (mL/min) 35,02476984
B(mL/min) 14,97523016
Table #3. Initial values for McCabe – Thiele diagram

Then, for the operation line there are the values of the equilibrium that are presented in the table 4:

Xethanol Yethanol
 0 0
0,021 0,19
0,0804 0,4091
0,1003 0,4578
0,1423 0,4975
0,1898 0,5239
0,2503 0,5613
0,2842 0,5723
0,3472 0,6041
0,4189 0,6345
0,5115 0,6789
0,5000 0,6723
0,5988 0,7009
0,6963 0,7585
0,7612 0,8015
0,9102 0,9114
0,95 0,94
0,99 0,98
1 1
Table #4. Values in equilibrium

Ilustration #2. McCabe – Thiele diagram

The equilibrium between ethanol and water was drawn with volumetric values. Because it is a simulation, it was
needed iterations of the L/V line from the composition in the top obtained to match the 8 stages that the column
already has.

After all the previously calculations, now we are going to show the values for the power needed in the reboiler;
the samples to evaluate this result were taken from the initial setup power of 0,5kW.
 Property  Value
Feed (mL/min) 50
Z 0,670103093
Xd 0,956185567
Xb 0,001
D (mL/min) 35,02476984
B(mL/min) 14,97523016
L/D 1,915
Qr (cal/min) 22699,07599
Qr (KW) 1,582882233
Table #5. Values on the distillation column

Analysis:

Separation process of liquid mixtures, especially those that involve the purification of a high industrial compound
as ethanol, are so important from de point of view of maximizing yields and the use of the resources that are
available for it. For the understanding of distillation column, the calculation of the number of stages was
influenced by the feed rate, which determines the yields on the mass balance, in this way, while the supply of
high temperature vapor was circulated increasing the available energy requiring for the circulation of the cooling
fluid. In other way, in the energy balance we can see that feed steam delivery much more energy than the
energy that is required for the distillation process, this must be inflicted because the distillation supply is quite
large [CITATION Wan \l 9226 ].

The first topic of analysis must be the comparison between the power obtained from the reboiler during the
mathematical procedure and the programmed with the distillation equipment. It can be seen a similarity between
them. The distillates and bottoms extract was determinate with the help of the refractometer and sometimes it is
not well cleaned before using it. Also, as seen in the excel book, the calibration curve is not very accurate, thus
when calculated the composition of ethanol in the bottoms, because the value was so low, using the equation
given developing the curve, the value of Xb would have been negative, therefore a value of 0.001 was supposed
to continue with the rest of the procedure [ CITATION Tre80 \l 9226 ].

For the temperature changes between stages, it was used the T-XY Ethanol-Water from the simulation in Aspen
to obtain the compositions of ethanol in each stage including stage 9 that is the reboiler. As it is known the power
in the reboiler, heats up the whole column which means the temperatures will elevate proportionally with the duty
of the heater [ CITATION Pér10 \l 9226 ].

Also heating up the reboiler makes the liquid fraction disappear easier as it is seen in the tables in excel.
Therefore, the value in the composition in the last stage of Ethanol in the column is almost cero, knowing that the
mixture given in the laboratory had already a very small fraction of ethanol (0,25).

Conclusions:

 There were determined the product flows of the enrichment and depletion zone as 35,02mL/min and
14,97mL/min, respectively.
 The graph method of McCabe-Thiele indicated a number of steps for the distillation column of 8 and the
simulation performed by Aspen Plus indicated a number of steps for the distillation column of 8, meaning
that all the calculations and values that are taken for the distillation are good.
 The precision in results can increase or decrease considering a variation on the thermodynamic
properties depending on temperature variation and the heat losses are quantified in the depletion zone.
 The energy provided by the tower to condensate the distillate is more that sufficient in this case.
 The small amount of ethanol from feed flow affected the mathematical procedure, due to the low
concentration of this compound in the bottom and assumption had to be made possibly changing some
results.
References:

[]Aarmfield. (s.f.). Discover with armfield: Distillation Columns. Obtenido de armfield: Engineering Teaching &
Research Equipment: http://discoverarmfield.com/en/products/view/uop3/distillation-columns

Arnaiz, C. (2007). Operaciones Básicas, destilación. Sevilla, España: Universidad de Sevilla.

Geankopolis, C. (1998). Procesos de transporte y operaciones unitarias. CECSA.

Jacques, A. (2010). Métodos gráficos en destilación. Transferencia de Masa.

Pérez, O., Díaz, J., Zumalacárregui, I., & Gozá, L. (2010). Revista de Facultad de Ingeniería de la Universidad
de Antioquia. Evaluación de las propiedades termodinámicas de mezclas Etanol - Agua. Medellín,
Colombia.

Treybal, R. (1980). Operaciones de Transferencia de Masa. San Francisco, Estados Unidos: McGraw Hill.

Wankat, P. (2007). Ingeniería de Procesos de Separación. México D.F, México: Pearson Pretince Hall.

No realizaron el análisis de una torre tipo semi continua como la que trabajaron. Hablan todo el tiempo de un
equipo en funcionamiento continuo. No vi gráficas de perfiles de temperatura en el tiempo durante la práctica.
Tampoco vi de perfiles de presión.

Reconozco un buen trabajo, pero falta ajustar bastante en el análisis de los casos de estudio.