Laboratory of separation, reaction and control operations

National University of Colombia

Group 6 Subgroup A
Experimental practice #5. September 13, 2017.

DISTILLATION OF ETHANOL IN AQUEOUS SOLUTION USING A

PACKED COLUMN WITH PROPAK PROTRUDED METAL 4 PACKING

J. S. Pinzn Lpeza, S.J. Avendao Peab, L.D. Perdomo Moralesc y K. L. Suarez Urizad
a, b, c, d
Chemical and environmental engineering department, Engineering Faculty, National University of Colombia

a b c d
jspinzonl@unal.edu.co sjavendanop@unal.edu.co ldperdomom@unal.edu.co klsuarezu@unal.edu.co
25492601 25492625 25492591 245307

Using a packed column of 0.8cm in diameter and 5m height, obtain the best
Main objective: possible recovery of ethanol from a mixture of 40% by volume of ethanol, with
a flow of 20 liters per hour, operating at ambient pressure and without using
heating along the column.

Determine the final composition in the distillate and the recovery of ethanol
operating at atmospheric pressure.
Construct the temperature and composition profile of the tower operating at
atmospheric pressure in the condenser and compare it with the values
predicted by a simulation made in Aspen Plus 9.
Specifics objectives: Vary the feed section and the heat along the column to obtain a purer product
in the top and a higher recovery of ethanol
If its possible, operate the column at reduced pressure and compare the
results with those obtained at atmospheric pressure.
Construct the Ponchon Savarit diagram for the operation and compare the
results of heat flows required with those given by Aspen 8.

Abstract: in this practice it was desired to recover ethanol from an aqueous solution at 40% volume-volume ethanol (rate flow 10 L/h), to generate azeotropic ethanol
at 95% weight-weight. This operation was carried out in a packed distillation column that has 8 cm of diameter, 5 meter of high and 5 sections with Propak Protruded
Metal 4 packaging. The mixture to separate was not preheated and the column operated at atmospheric pressure. The experimental data of this run (temperature and
composition profiles) were compared to those obtained in a simulation made in Aspen Plus 8, where a clear similarity was found, although the data were not completely
similar. The final composition of the ethanol in the distillate stream was 86% weight-weight, with an approximate recovery of 85%. Key words: distillation, packed
column, azeotrope, component recovery, bioethanol, simulation.

Resumen: en esta prctica se dese recuperar etanol a partir de una solucin acuosa al 40% de volumen-volumen de etanol (caudal de 10 L / h), para generar etanol
azeotrpico al 95% en peso. Esta operacin se llev a cabo en una columna de destilacin empaquetada que tiene 8 cm de dimetro, 5 metros de altura y 5 secciones
con el empaque Propak Protruded Metal 4. La mezcla para separar no se precalent y la columna oper a presin atmosfrica. Los datos experimentales de esta
corrida (perfiles de temperatura y composicin) se compararon con los obtenidos en una simulacin realizada en Aspen Plus 8, donde se encontr una clara similitud,
aunque los datos no fueron completamente similares. La composicin final del etanol en la corriente de destilado fue del 86% en peso, con una recuperacin
aproximada del 85%, por lo que, claramente, un mejor esquema de operacin podra ser propuesto. Palabras clave: destilacin, columna empaquetada,
azetropo, recuperacin de componentes, bioetanol, simulacin.
 1. Introduction
Anhydrous ethanol is widely used in the chemical industry as a very useful solvent and as a
raw material or an intermediary in the synthesis of esters, organic compounds with cyclic
chains, detergents, paints, cosmetics, aerosols, perfumes, medicine, food and many other
products (Gil ID, Uyazn AM, Aguilar, JL, Rodrguez, G. and Caicedo, LA, 2008). In addition
to this, mixtures of ethanol and water can be used as fuels and significantly reduce
environmental pollution, simultaneously, several studies have verified that this increases the
octane rating. The interest of ethanol ass an additive for fuels is due to the global interest in
the production of alternative fuels since fossils are limited and are being depleted.
One of the key challenges in the production of these blends called biofuels is the production
of high purity products and, in this sense, it is obvious that the production of high purity
ethanol is consolidated as a chemical process of considerable interest. The so-called
bioethanol (intended to be mixed with gasoline) is usually obtained by biochemical routes in
which the final product of the reactions is ethanol diluted with water.
The separation of ethanol and water is quite difficult due to the existence of an azeotropic
point in the mixture. Conventional distillation allows to obtain solutions of ethanol with the
concentration of the azeotrope and to obtain ethanol in higher concentrations it is necessary
the use of extractive or azeotropic distillation schemes, however, there have recently
appeared other emerging techniques such as distillation with salt mixtures, distillation by
pressure change and pervaporation (Ngema, P. T, 2010).
In Colombia, Law 693 of September 2001, establishes that the gasolines used in the country
must contain oxygenated components, like the fuel alcohols; the implementation of this law
helped to increase interest in the production of these products. The objective of the law was
to promote the diversification of the Colombian energy basket using alternatives compatible
with sustainable development in the environmental, economic and social fields (UPME,
2009).
In 2009, the production of ethanol in Colombia to fulfill the aforementioned purposes came
exclusively from the processing that was done to the sugar cane in Valle del Cauca; there
are located thirteen mills and five distilleries, which gives the conditions for the growth of the
production of biofuels.
Although the production of bioethanol in Colombia is not significant at a world level, the study
of production schemes could be beneficial afterwards given the great potential in the region.
In the current study, the distillation of the ethanol-water mixture is studied using a packed
distillation column available at the Chemical Engineering Laboratory of the National
University in Bogot; although it corresponds to a traditional scheme well studied the startup
of the column and the yield that is obtained from it will allow an analysis that guides a better
understanding of the separation for this mixture that has profiled itself as a very promising
product in the energy area.
Although it is not expected to provide conditions to produce large-scale anhydrous ethanol,
the discussion surrounding the results obtained and the evaluation of the operation of the
equipment could allow the consideration of carrying out extractive or azeotropic distillation
in the equipment to propose an alternative separation scheme.
 3

2. Theoretical framework

A. Packed distillation columns

Packed columns are used in a widely range of separation processes, such as distillation,
gas absorption and liquid-liquid extraction. The contact between the phases in this type of
equipment is continuous, not in stages, like in a tray column. In gas liquid contact the liquid
flows down over a packing surface and the movement of the gas is opposite, that is to say,
counter-currently. Some of the factors that affect the performance of a packed column are
the distribution of the liquid and the gas through the packing, the type of used packing and
the internal features of it, like the liquid distributors and redistributors.
The used of a packed column over a tray column must be correctly assessed due that the
two kinds of equipment have advantages and disadvantages. In this sense, it can be said
that:
- Tray columns can handle a broader range of liquid and gas flow rates.
- When there are very low liquid flow rates, packed columns are not appropriate.
- The HETP (height equivalent to a theoretical plate) and the HTU (height of transfer
units) are less accurately computed than the equivalent term of efficiency of a plate.
- When corrosive liquids are present, a packed column will be usually cheaper than
the tray equivalent.
- If flammable or toxic liquids are present, its desirable to use a packed column due to
lower hold up.
- If the operation involves a foaming system a packed column should be preferably
used.
- Pressure drop is usually lower in a packed column.

B. The transfer unit

The concentration varies continuously along the height of the packing and this should be
considered for the computation adjacent to this type of equipment. The Figure 1 shows a
schematic description of a packed column showing some of the interest variables; it can be
observed that as in tray columns a reboiler and a condenser are needed, the entrance of
the feed can be achieved by adding a section of the tower without packing, making sure that
there will be a good distribution of the liquid over the stripping section.
For packed towers the flows are based on the transversal area of it, that is to say, mol/(area
time). As seen in Figure 1 in the differential volume of the packing dZ the interfacial area will
be a dZ, being a the specific interfacial surface. The flux of the component A if the flows of
vapor and liquid are constant in a section of the tower so that equimolar counter-diffusion
can be achieved between the two phases is computed as:
 4

Figure 1. Schematic representation of a packed distillation column. The

stripping and enriching section are differentiated. The reader can easily infer
the used nomenclature, mentioning that, the e sub index will be used for
enriching section and the s sub index for stripping section.

d (Gy ) d ( Lx)
NA k y' ( yi y ) k x' ( x xi ) (1)
a dZ a dZ

Being NA the flux of the substance A, ky and kx the mass transfer coefficients, x the
concentration in the liquid, y the concentration in the vapor and G and L the flows of vapor
and liquid, respectively. The sub index i refers to the equilibria. Taking the enriching section
as reference the equation (1) becomes:
Ze ( Gy )2 ( Lx )
2
d (Gy ) d ( Lx)
Ze dZ
0

( Gy )a
'
k y a( yi y ) ( Lx )a k x a( x xi )
'
(2)

If usual simplifications such as that in any section the flows of liquid and gas are essentially
constant the heights of the transfers units HtG and HtL can be computed as:

G
H tG (3)
k y' a

L
H tL (4)
k'1a

Due to that these will be constant as well and the equation (2) can be converted into:
y2 2 x
dy dx
Z e H tG H tG N tG H tL H tL N tL (5)
ya
yi y xa
x xi

With NtG and NtL being the number of transfer units. The mathematical procedure until here
presented corresponds to that developed by Treybal (Treybal R. E, 1980).

C. The height equivalent to a theoretical plate

 5

If at a point of the distillation column the concentration of the liquid flow is x, and the
concentration of the counter-current vapor flow at the same point is y, then there is a height
above this point where the concentration of the vapor flow (y*) is in equilibrium with x. This
section is the Height Equivalent to a Theoretical Plate (HETP) (Budapest University, 2017).
The total height of the packing can be obtained as:
Z HETP N (6)

Being N the needed theoretical stages for the desired operation, this value can be easily
obtained using the McCabe Thiele method. The value of HETP can be obtained using the
modified Granville equation:
1/3
G Z
HETP 28 d p mE (7)
L 2.4

Being dp the diameter of the particle that conforms the packing and mE the average slope of
the equilibrium curve. For the computation of this last value consider the Figure 2, where an
equilibrium curve for an arbitrary binary system is presented; due that the liquid-vapor
equilibria is not defined by a straight line its necessary to make the linearization to certain
sections of the curve as shown, so, the average will be computed as:

mE
m i
(8)
nm

Being nm the total slopes computed.

Figure 2. Example for the calculation of the average slope for the equilibrium curve.

D. Properties of interest
It is necessary to know very well the liquid-vapor equilibrium for the system ethanol-water.
Experimental data for the system were retrieved at three pressures: 1 atm (Rieder, R. M.
and Thompson, A. R, 1949), 0.6513 atm (Otsuki, H. and Williams, F. C., 1953) and 0.3289
 6

atm (Kirschbaum, E. and Gerstner, F, 1939); the experimental data were fitted to the
UNIQUAC model with non-ideality correction by Hayden OConnell equation of state using
Aspen Properties 9, resulting in a very good fitting. The Figure 3 shows the xy diagram for
the system, while the Figure 4 shows the Txy diagram. The more desired value of the
equilibria is the composition of the azeotrope. Table 1 resumes several reports for the
azeotrope of the system at various pressures.

1
Molar fraction ethanol, vapor

0,9
0,8
0,7
0,6 0.3289 atm
0,5 1 atm
0,4 0.6513 atm
0,3
UNIQUAC HOC
0,2
45 line
0,1
0
0 0,2 0,4 0,6 0,8 1
Molar fraction ethanol, liquid

Figure 3. Relation between the concentration of ethanol in the liquid and vapor phases at three different
pressures. Note, that for all cases, after a molar fraction in the liquid of 0.8 the equilibria curve approaches the
45 line, indicating the existence of an azeotrope. Its observed that the chosen model fits quite well the
experimental data. In this case the presented fit (continuous black line) was computed at 1 atm.

100
Temperature (C)

90

80

70

60

50
0 0,2 0,4 0,6 0,8 1
Molar fraction ethanol, vapor and liquid

Figure 4. Temperature-composition diagram for the system ethanol water. The convention is the same as that
presented in Figure 3, and the adjustment to the UNIQUAC HOC model is presented for all the pressures. Note
that the approaching of the vapor and liquid curves indicates the presence of the azeotrope.

Temperature (C) x y x y Pressure (atm) Source

78,15 0,8940 0,8940 0,9556 0,9556 1,0000 Reinders et al, 1947
49,99 0,9288 0,9288 0,9708 0,9708 0,2917 Balcazar-Ortiz et al, 1979
 7

49,99 0,9439 0,9439 0,9772 0,9772 0,2915 Wilson et al, 1979

Table 4. Some of the reported azeotropic concentrations for the system. A lower pressure the change in the
concentration is not so significant. Convention: x: liquid molar fraction of ethanol, y: vapor molar fraction of
ethanol, x and y: mass fractions.

3. Materials and equipment

In this practice, a reactive distillation column will be used. The column is in the pilot plant of
Laboratorio de Ingenieria Quimica (LIQ) and has as denomination T1503 in Key Plan. The
description of the column and some of its components is:

A. Column1:
The column has a diameter of 8 cm in stainless steel, conformed by five sections
of 1m high each one packaged with Propak Protuded Metal 42 packing. Each
section allows the flow of steam through a jacket and has an insulating sheet.
Two tanks of stainless steel for feed with capacity of 30 L and 45 L.
A pump that connect the tank of 30 L with the column.
A centrifugal pump that connect the tank of 45 L with the column.
Heater for each tank:
Shell and tube heat exchanger for the tank of 30 L; Shell of 8 cm diameter
and 45 cm large; 12 tubes of in and single step.
Sell and tube heat exchanger for the tank of 45 L; Shell of 11.5 cm
diameter and 40 cm large; 14 tubes of in and single step.
Reboiler of 20 L with stirring agitation (in this case the agitation will not be used).
Condenser of stainless steel, shell of 15 cm diameter and 1 m large, 36 tubes, of
in with two steps.
Tanks of 1.15 L each one for distilled and bottom.
Thermostatic oil bath.

B. Additional materials:
Rotameter for measuring water to condenser.
Coriolis flow meter for reflux.
Honeywell flow meter for tank of 45 L.
Rotameter for measuring flow for tank of 30 L.
Eleven thermocouples located throughout the column.
A pressure gauge located at the vapor inlet to the heater.
A differential pressure gauge that measures the pressure drop of the column.

1 A schematic diagram for the equipment to be used is shown in Figure 6, where a additional description is
presented.
2 A description of this kind of packing is presented in this link:

https://www.cannoninstrument.com/Image/GetDocument/425?language=en
 8

Figure 6. Simplified schematic diagram for the distillation column to be used. All the sections in the column can
be heated independent and the feed can be loaded in two different positions, in the transfer unit 2 or in the
transfer unit 3. It is seen that the feed can be previously heated so that a flow of vapor enters the column as well.
Temperature can be measure in all units so a temperature profile can be constructed, and, assuming
thermodynamic equilibrium, a composition profile can be derived. Although just one tank is positioned for the
recovery of the distillate product indeed there are three tanks that can supply this task. A more detailed diagram
(P&D) can be obtained in the study realized by Bello Hernandez, Forero Quimbaya, Lancheros Castaeda and
Tibocha Bonilla, which is cited in references.
 9

Control Panel, an electronic panel (Siemens ) where you can directly see
temperature in several points of the column, the pressure of the heating vapor,
the pressure in the reboiler and the flows of the feed and the reflux.
Breathalyzer, device for estimating alcohol content, only used for ethanol.
Densimeter Metler Toledo, and additional equipment for the measure of the
composition, using equation (9).

C. Substances
Water
Ethanol3
Steam

4. Experimental procedure4
I. Cleaning the equipment: firstly, the equipment must be cleaned along with materials
due that the equipment has had changes and modifications in this years, and can
have wastes of previously experiments. It should be noted that the column is
designed for reactive distillation processes.
II. Identification of ignition switches: it is necessary to identify the ignition switches of
the control panel, because the equipment doesnt have an experimental guide. A test
is performed to identify the functions of each switch. Whit this test the operation of
the equipment can be understood.
III. Verification of the flow of services: through the opening of valves in the process lines
of the plant, the flow steam is verified in the reboiler, heaters and flow water in
condenser. Also, the pipeline of oil will be identified.
IV. Review of measuring instruments: before any operation is carried out in the column,
the operation of the measuring instruments must be checked. This activity is mainly
made for flow meters, rotameters and manometers, and temperature or
thermocouples.

a. Thus, for flowmeters it will necessary to supply water flow with the pumps
through the piping circuit to a drainage point, where a graduated cylinder will
be placed to perform the calibration. However, it must be verified that the
diaphragm pump doesnt provide a flow that can overcome the resistance
exerted by the pipe circuit.

3 The problem mixture to use will have a 40% volume concentration of ethanol. The computation of how much
water and ethanol must be blended is shown later.
4 The experimental procedure was made based on the document Evaluacin del estado de la columna de destilacin

reactiva ubicada en la planta piloto del laboratorio de ingeniera qumica, provided by the engineer Andres Javier
Bello Hernandez. Some lights alterations for the procedure shown in the referenced document were made, but,
essentially, Its the same. Also, the experimental procedure is given in present time, so it can be used as
guideline for future experimentations.
 10

b. Finally, it is necessary to check the operation of the thermocouples, so water

flows in the column and temperature is recorded in each thermocouple, and
a test will be carried out by evaporating water.

V. Starting the operation: To initiate a practice of distillation in this column the following
steps must be followed:

1. Check that in the circuit breaker box, the switches corresponding to the
column are on.
2. Turn on the control panel with the stabilizer located inside the control
panel.
3. Verify all switches 0/1 inside the board are in 1.
4. Turn on the thermocouple and pressure sensor screens.
5. Turn on the flow meters.
6. Check that there are no residues in tanks and in sections of the tower.
7. Load aqueous solution into tanks.
8. Priming the pump and loading reboiler.
9. Open the valve that gives way to the condenser cooling water and fix the
flow with the rotameter.
10. Bleed the steam pipes from the exchangers, reboiler and column
sections.
11. Open the steam valve to the boiler up to the desired pressure and heat
the contents of the reboiler up to the desired value.
12. Open the steam and return valve of the reboiler, and keep the valves of
bottom, top product and reflux closed.
13. Wait for the vapors to rise to the condenser and see in the decanter.
14. If a batch operation is to be carried out, the distillate must be stored in the
tanks; while if the operation is continuous, the passage to the reflow pump
is opened to operate the column at full reflux.
15. For:

a. BATCH OPERATION:
Record the compositions obtained as a function of time.
b. CONTINUOUS OPERATION:
Handle the reflux valve allowing the level in the tank to be constant.
Allow the reflux to go down the spine for a few minutes.

16. Open the feed valve in the desired tower section and turn on the feed
pump and close the feed to the boiler
17. Open the outlet valve of the distillate by modifying the opening of the
reflux valve to reflux ratio.
18. Wait for the column to stabilize and then begin the measurements of
variables.
 11

5. Data report
The values for the temperature profiles are shown in Figure 8, where the evolution of the
process is shown. Table 2 resumes the streams summary where the flow and composition
of interest streams are shown while Figure 9 and Figure 10 compare the obtained profile
and composition profile (in vapor phase) in comparison to that given by Aspen Plus 85 for
the continuous distillation.

Figure 8. Temperature profiles as function of time. The operation profiles correspond to the beginning time of
the continuous distillation, 120 mins, when there was no a significant variance of the values.

Figure 9. Temperature profile obtained in the experiment with that given by the simulation in Aspen Plus 8.

5 UNIQUAC and RAD-FRAC models used. For the two degrees of freedom in the column the reflux
rate and the measure flow rate in the experimentation were given. The void fraction used for the
packing was 0.28 and the packing factor was 5.612 1/mm, values obtained making measurements in
some of the particles of the packing,
 12

Figure 10. Temperature profile obtained in the experimentation (using the equilibrium data for the system) and
that given by Aspen Plus 8.

Volume flow (L/min) Volume fraction ethanol Mass fraction ethanol Molar fraction ethanol

Distillate 3.85+ 0.92 0.90 0.78

Bottoms 7.65+ 0.17 0.14 0.06

stream

Feed 10.01 0.40 0.34 0.17

Reflux 2.63* 0.92 0.9 0.78

Table 5. Streams summary. * Mass flow (kg/hr), registered from the control panel of the column.

For compare of result the packing and plate column, is calculated the HETP, first is
determinate the average slope of the equilibrium curve -mE- (equation 8), where is evaluated
the slope in the operating range, mE=0.518.

0.25 N HETP
1/3
2
HETP 28 8 10 0.518
0.55 2.4

Lather, is evaluated the Savarity-Ponchon method, where calorific capacities (vapor and
liquid) and enthalpy of vaporization (at 25C) are required.

Properties Ethanol Water

a (kJ/kmolk2) 0.1606 0.0043
CP,vap
b (kJ/kmolk2) 17.868 32.600
a (kJ/kmolk2) 0.4765 0.0826
CP,liq
b (kJ/kmolk2) 24.021 24.021
298k (kJ/mol) 4256.8 4398.2
Table 6. Properties for the calculated of equilibrium liquid vapor in function of enthalpy and molar fraction
(determinate in Aspen Properties by UNIQUAC method).
 13

2
H liq (T , xi ) xi
T
CPliq,i dT (9)
298 K
i 1

2
H vap (T , yi ) yi i (298K )
T

298 K , i dT
CPvap (10)
i 1

CP,i ai T bi (11)

For the Savarity-Ponchon method (Treybal, 1998);

H D H liq , n H D H vap , n 1
(12)
xD xn xD yn 1

H W H vap , m 1 H vap , m 1 H liq , m

(13)
xw ym 1 ym 1 xm

H D H1,vap
Rop (14)
H1, vap H 0,liq

H D H F H F H W
(15)
xD xF xF xW

Applicated the Savarity method has the following operation profiles:

125

100
Enthalpy (kJ/mol)

75

50

25

0
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1
-25
Molar fraction of Ethanol
Figure 11. Equilibrium liquid (blue)-vapor (red) in function of enthalpy and molar fraction, minimum line operation
(green), line operation (violet), equilibrium x=y (dark blue), mass and energy balance for plate (orange) and molar
fraction in distillate and bottoms (gray).
 14

Molar vapor fraction of Ethanol 1

0,9
0,8
0,7
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
Molar liquid fraction of Ethanol
Figure 11. Equilibrium liquid-vapor (blue) function of molar fraction of vapor and liquid, x=y (black) and lines
operation (red).

For Savarity-Ponchon method, the column had 9 plates, with the equation for the
computation of the height it will be obtained that
3/2
0.25 N
1/3

HETP 28 8 102 0.518 0.74m

0.55 2.4

Z 9 0.74m 6.68m
Measured the flow energy of condenser and reboiler, had a balance energy and balance
component total of column:
F D W (16)

xF xD xW (17)

F H F D ( H D QC / D) W ( HW QR / W ) (18)

F H F D H D W H W (19)

Stream Flow (mol/h) Enthalpy (kJ/mol) Energy (kJ/h)

F 4.019 0.000 0.000

D 0.620 7.065 4.378

W 3.406 4.660 15.872

QC/D 0.620 101.869 63.125

QR/W 3.406 24.476 83.374

Table 7. Profiles of flow, enthalpy and energy of stream of column.

 15

6. Discussion of the results

Figure 9 shows the temperature profile of the different zones of the tower, the experimental
results of the distillation are lower than the simulation except point 5 that is above the value
expected by the simulation, this point corresponds to the input of the tower from the reboiler
and the value is higher because the boiler supplies more heat than the necessary to
evaporate the mixture that should be distilled. The simulation process is carried out using
aspen plus 8 with the UNIQUAC and RAD-FRAC models. The simulation shows that the
tendency of temperature over the equipment is greater than the one obtained
experimentally. This could be due to, although the implemented models consider the
molecular contributions, considerations of the groups of each molecule is not contemplated.
Some interactions of the molecules are not having into account and therefore, there is only
approximations that help to understand and to predict an approximation of the reality.
Another aspect to consider is that the characterization of the packaging was made with a
measure of the dimensions of the same, thus obtaining values of fraction of vacuum and
packing factor of 0.28 and 5.612 L/mm. As mentioned, the simulations have the inherent
error of being determined by non-exact methods.

In Figure 10, the molar concentration values were obtained by using the equilibrium system
and compared to the curve given by the simulator, the trend was like that of Figure 9 in that
the experimental data were located at lower values to those expected or projected by the
simulator, except at one point, the top of the tower where the experimental value exceeded
the simulated value.

Operation of the equipment: Much of the distillation procedure is performed in the control
panel, but some specific actions had to be performed manually, such as the reflux ratio in
the column, although there is a valve for this action, the opening can be controlled just
manually. this prevents a timely feedback at the time of operation of the equipment, if it is
condensing much or little at the top of the column, it is impossible to change this reflux ratio
and is only observed in the window that is after the condenser and varying the opening of
said valve.

The condenser at the top of the column does not have any type of control, the flow of
refrigerant (water) must be large, since it must guarantee the full condensation of the
destination, as much for safety, as for operation matters, (condensate handling is easier
than steam handling), in addition to the column, the solution is recirculated in liquid phase,
the fact of guaranteeing a condensate at the top involves costs in operation services,
unnecessary cooling of the fluid involves large amounts of unnecessarily used water, also
involves energy costs (if this flow of water should be cooled in a cooling tower would imply
more costs in the operation, in this case only water was available), when the fluid is
recirculated to the tower, this fluid should preferably be at the operating conditions of the
column to ensure stable operating conditions, which then involves a heat exchanger, which
requires steam and therefore involves costs due to this service. Although there is no control
in condensation, there is a flow meter that gives an estimate of the flow rate of water passing
through refrigerant. Finally, the steam trap could be plugged, that implies an increase of the
pressure in the system, increasing boiling points and making it difficult to operate the
distillation tower, but there were no flood or abnormalities.

An additional comment can be made about the Granville equation used for the computation
of HETP and the later computation of the theoretical height of the tower. The result, although
 16

relatively close to the real value should not be considered as representative of the operation
because the equation is supposed to be used when there are rigid packings. The used tower
had a sparse packing, however, the equation used few information of the rigid packing and
in that sense, is not very strict, thing that could lead to the near value obtained. The closer
result can also be explained because the Ponchon-Savarit method seems good for the
system ethanol-water until the azeotrope is reached, where other calculations method
should be proposed in order to consider advanced methods of separation such as extractive
distillation or azeotropic distillation.

7. Conclusions
For the separation of a liquid stream (10L / h) of ethanol-water with 40% volumetric alcohol
concentration, by the continuous distillation operation using a packed column with propak
protruded metal 4 packing of 0.8m diameter and 5m height. Operating with a steam valve
opening in a range of 60-80% were obtained: a top product (ethanol) and a bottom product
(water) with a concentration of 92% and 17% (v / v) respectively. Recovering 12.5 liters of
92% ethanol for 2 hours of continuous operation.

The aspen plus simulator represents an important tool for a general understanding of the
mass transfer phenomena, however, the experimental reality shows behaviors relatively
different to those projected by the simulation because the thermodynamic packages with
which these estimates were made they dont analyze interactions of molecules.

The calculated height (6.7 m) of the tower trough the Ponchon-Savarit method and later
application of the Granville equation seems close to the real height (5 m) although other
methods for the HETP should be considered for this operation because there is sparse
packing.

8. Response to expectations and

recommendations
One of the objectives set by the work team was to operate in vacuum to observe the
incidence of this variable in the separation operation, however, this procedure could not be
carried out due to the short time it was to the practice. Since during the first session of the
distillation there were still failures with the operation of the equipment and therefore in the
second session the time was designated to make the pertinent corrections for the
separation. the same happened with the aim of modifying the feed section, therefore we
recommend performing these procedures for a deeper compression of the continuous
distillation phenomena.

The error in the above-described operation was tried not to completely open the valve of the
reflux section which allowed the passage of the distillate to the storage tanks, it was operated
at full reflux and for this reason a volume of distillate higher than 1 L during this session, for
all this we recommend to readers to ensure the opening range of the valves, as it may that
despite having been turned a good number of times the valve is still not allow the flow. Also,
a following of the quantity of steam condensed in the reboiler should be made in order to get
a measurement of the energy required for the process.
 17

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