Continuous Distillation Pre-Report

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October 16th, 2019

CONTINUOUS DISTILLATION
Universidad Nacional de Colombia
Faculty of Engineering
Department of Chemical and Environmental Engineering
Separation operations, Reaction and Control Laboratory
GROUP 7 -Team A
Daniel Alejandro Arévalo Peña a​ ​ ​Juan Antonio García Cortés b​ ​Laura Kristal Camacho Fandiño c​

Carol Ibáñez Rodríguez ​ d​ ​María Alejandra Vargas Castrillón e​ Brayam

Camilo Vela Galindo f​

a) daaarevalope@unal.edu.co b) j​ uagarciaco@
​ unal.edu.co c) lkcamachof​@unal.edu.co
d) cgibanezr@unal.edu.co e) ​mavargasc​@unal.edu.co f) b​ cvelag@unal.edu.co
___________________________________________________________________________________________________________________
 
Among  the  biggest  challenges  of  the  industry  is  the  evaluation  of  the  different  separation  operations, 
the  distillation  is  among  the  first  operations  considered  in  the  industry,  this  is  due  to  the  ease  of 
handling  and  its  functionality  without having to add any additional compound As a solvent, although 
simple  distillation  towers  are  the  easiest  to  operate  and  its  cost  is  quite  low,  in  most  cases  it  does  not 
generate  products  with  a  high  degree  of  purity so it is sought to increase the contact between the vapor 
and  liquid  so  that  heat  and  mass  transfer  occurs  more  effectively.  Given  the  importance  of  knowing 
this  process  in  depth,  the  practice  of  continuous  distillation  is  proposed.  In  this  pre-report  the 
objectives,  the  vital  information  to  have  a  context  regarding  the  distillation and the principles behind 
it,  the  experimental  management  sought  and the procedure of practice to use the equipment of the pilot 
plant of the University Laboratory of Chemical Engineering (LIQ)  

1. Introduction: ​Distillation is the method of separation of pure chemical substances, oldest and important
that is known. It is the separation of a liquid mixture by its partial vaporization, the vaporized fraction
condenses and is recovered as a liquid. The oldest distillation form is the one that is made to obtain
alcoholic beverages. Thus, when heating a mixture containing water and alcohol, the lightest components,
in this case alcohol, they concentrate in the distillate. Distillation columns, elements used to carry this
process is the result of the technological evolution in which it is done exactly the same thing only in a more
effective way: through a series of stages there are stepped evaporations and condensations, coupled
together.

The separation of ethanol and water its 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. That is the reason why it is necessary
to study this case and evaluate the cases in which we can make a correct operation taking into account the
dependence that have the results with the variables of the operation and the parameters handled.

2. Objectives

Main objective: ​Obtaining a 96% w / w ethanol solution by continuous distillation while determining
the optimal conditions to make the operation better.

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Specific objectives:

● Determine the minimum reflux and operating conditions for obtaining 96% ethanol.
● Determine the concentration and temperature profiles inside the distillation column
● Evaluate the incidence of reflux on ethanol recovery in the distillate

3. Theoretical background

Continuous distillation

Distillation is one of the most common methods for the separation of liquids, but despite this it has several
limitations, which has led to other forms of separation. Even, modifications to the same distillation are
sought, making this form of separation the first option when separating liquids.

Distillation is a method of separation whose principle is the difference in relative volatilities between the
compounds, which is usually expressed in a difference of boiling points between these, usually one has a
very volatile component with respect to the other.

The distillation consists of a partial vaporization of a given mixture followed by a separate recovery of
steam and waste. In this method of separation the components are found in both liquid and gas phase, so
the separation depends on the distribution of these in the phases. Unlike absorption or desorption, where a
new substance is introduced to perform the separation, in distillation the creation of a new phase is carried
out from the initial solution by means of evaporation or condensation.

Distillation can be classified according to its method of operation into two types: distillation continuous or
discontinuous. Continuous operation refers to the fact that the feed is constant with respect to time and a
discontinuous operation refers to the fact that the feed is variable with respect to time.

On the other hand, it can be operated at atmospheric pressure or reduced pressure, this is determined
according to the compound and its boiling point, since at reducing the pressure decreases the boiling point
of the compounds. (Treybal R., 1980)

In addition to those mentioned above, there are other types of distillation:

● Simple distillation: This distillation was the first to be used in the industry, in this the vapor that is
withdrawn from the liquid sinus immediately passes to the condenser and then distilled liquid is collected.
By this method, binary mixtures are usually separated with a difference in boiling points of at least 60-80
°C. Through this is not possible to obtain high purity compounds.

● Fractional distillation: It is the combination of many successive simple distillations in a single operation in
which a vertical fractionation column is used, in which successive evaporations and condensations occur
until steam reaches the top of the column and condenses, obtaining the distillate. In each of these simple
distillations It is considered a theoretical stage of separation, this distillation is very effective, even for
separate components with a boiling point difference of one degree.

Following this, the more plates a fractional column has, the greater the degree of separation.

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● Azeotropic distillation: When it is not possible to carry out a distillation conventionally due to problems
that they occur when an azeotrope is formed between the compounds, azeotropic distillation is used,
which consists in breaking the azeotrope by changes in pressure or addition of a third component that
does not form azeotrope with the other components. It is also used extractive distillation in these cases, in
which a separating agent or solvent is added.

Distillation is done both in a column of dishes and in a packed column, however, the latter is very poorly
studied, because it’s modeling is more complicated.

Distillation advantages and disadvantages

The advantages of distillation are that it is not necessary to add other foreign substances that can make
the process much more cumbersome since the other phase is generated from the liquid fed, which does
not occur with liquid-liquid absorption or extraction. Another big advantage is the little space that the
equipment needs in comparison with other operations.

The main disadvantage is the amount of energy it is needed to generate the gas phase and then be
removed to generate the liquid phase, this means two more auxiliary equipment that are necessary to a
correct operation.

Packed distillation columns

Packed columns are used in a wide 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 to the fact 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 is 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.

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

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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 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:

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

Being NA the flux of the substance A, k’y and k’x 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:

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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:

Due to that these will be constant as well and the equation can be converted into:

With NtG and NtL being the number of transfer units. The mathematical procedure until here presented
corresponds to that developed by Treybal.

4. Materials, equipment and reactants

The equipment to use in this experiment is the LIQ continuous packed distillation tower. Column is
supported by a 1.18m stand, has a jacketed reboiler and a shell-tube condenser. The pack is Nutter Ring
type of stainless steel (1 in). Column pipeline network has been modified and new valves and bypasses
were installed, however, an approximate scheme of the equipment is shown in figure 2.

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​ chematic representation of the LIQ packed column equipment.


Figure 2. S

1. Packed section 6. Cooling water outlet


2. Direct feed to condenser pipeline 7. Cooling water inlet
3. Reboiler 8. Vapour inlet
4. Centrifugal pump 9. Bottoms outlet
5. Inlet flow-meter 10. Distillate outlet

A detailed PFD of the equipment is shown in annex 1. In this diagram it is shown that the column has
different taps in different heights in order to take samples to evaluate density

Reactants

● 40 L of ethanol solution 80% w/w


● 20 L of azeotropic ethanol (96% w/w)
● Water

Other materials and equipment

● Alcohol meter to measure density and calculate alcohol concentration


● Measuring buckets
● Probetes
● 4 thermometers (0 - 100°C)

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5. Experimental procedure

​ xperimental procedure flow diagram


Figure 3. E

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6. Variables and data collection

● Inlet pressure to the reboiler: ​Is the pressure given for the manometer at the reboiler inlet, it is
necessary to know the inlet enthalpy.
● Outlet saturated liquid flow from reboiler: K ​ nowing the outlet liquid is saturated, we can make an
energy balance if we know the mass flow, for that it is necessary to know the density and flow on
the outlet reboiler stream.
● Initial volume of mixture charged into the reboiler: ​It is necessary to stabilize the tower.
● Initial mixture concentration charged into the reboiler.
● Inlet water flow in the condenser: ​It is given for the flow-meter.
● Temperature of inlet water to the condenser: ​It is necessary to make the energy balance in the
condenser.
● Outlet temperature of condenser water: ​It can be measured with a thermometer at the condenser
outlet.
● Outlet water flow in the condenser: I​ t can be measured with a test tube and a chronometer in order
to compare it with the reported by the flow-meter.
● T1 - T6: G​ iven by the thermocouple, necessary to make the tower temperature profile.
● Total reflux: ​Once the tower is in steady state we can measured the total reflux with a rotameter.
● Real reflux: T​ he ratio of reflux we set.
● Inlet temperature of mixture to the tower: I​ t is measured in the boiler where the feed is charged.
● Inlet flow of mixture to the tower: I​ t is measured with a rotameter.
● Feeding plate: ​It is set by the users.
● Refraction index Tap 1- Top: N ​ ecessary to do the tower concentration profile.

6.1 Data collection

Table 1. ​Data collection format.


Inlet Outlet Initial Initial Inlet Tempe Outlet Outlet T1 (°C) T2 (°C) T3 (°C) T4 (°C) T5 (°C) T6(°C)
pressu saturat volume mixture water rature temper water
re to ed of concen flow in of inlet ature flow in
the liquid mixture tration the water of the
reboile flow charge charge conden to the conden conden
r (psig) from d into d into ser conden ser ser
the the the (L/min) ser water (L/min)
reboile reboile reboile (°C) (°C)
r r (L) r
(L/min) (%w/w)

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Table 2. ​Data collection format.


Total Real Inlet Inlet flow of Feeding Density Density Density Density Density Density
reflux reflux temperatu mixture to temperatur from from from from from from
(L/min) (L/min) re of the tower e (°C) sample sample sample sample sample sample
mixture to (L/min) Tap 1 Tap 2 Tap 3 Tap 4 Tap 5 Top
the tower
(°C)

6.2 Additional data

Figure 1. ​Temperature-composition diagram Ethanol-Water. Aspen Plus 9.0

Figure 2. ​X-Y diagram Ethanol-Water. Aspen Plus 9.0

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7. Costs

In this practice we have costs due to different causes than can be disaggregated as follows:
● Feed and service streams.
● Electricity.
● Operators wage.
● Equipment.

Feed and service streams.

Table 2. ​Associated costs to streams.


Stream Quantity to use Cost per unit Sub total

Steam 〜80kg/cicle 315 COP/kg 25.200

Ethanol 40L 17.000 COP/20L 680.000

Water 40L 6.311 COP/m3 252 COP

TOTAL 705.452 COP

Electricity.

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Description Power Cost per unit Sub total

3 centrifugal pumps 1 hp 〜500 COP/kWh 4.470 COP

TOTAL 4.470 COP

Operators wage.

Table 4.​ ​Operators wage.


Description Cost [COP] Hour Number of persons Sub total

Engineer hour 150.000 4 1/3 200.000

Laboratorist 1/8 (Taking into account all the


60.000 4 30.000
hour practices in charge of the laboratorist)

Student hour 60.000 4 4 960.000

TOTAL 1’190.000

The greatest cost linked to this practice is the wage of operators, but in a real plant where this process be
carry on, the personal would be in charge of very equipment and due to that the associated costs would be
minors.

8. Work planning

On the following tables is presented the expected activities distribution on the two days of the experiment
(October 23​rd​ and 30​th​)

Table 5. ​Activities Wednesday 23 Octubre

October 23rd
Hour
Task Attendant
1:00 1:30 2:00 2:30 3:00 3:30 4:00 4:30
Request work material, helmets and keys Laura
Prepare solutions ethanol-water of known
Camilo
concentratión
Density measure Daniel
Calibration curve Carol
Equipment adequacy Juan Antonio
Load equipment, on PLC and purge Alejandra
Supply steam, pressure 7ps, open reflux Daniel

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valve
Waiting the concentration Carol
Start up equipment Laura
Open food valve, PLC temperature and
Camilo
level control
Distillate and Waste flow Alejandra
Ending equipment Juan Antonio

Table 6. ​Activities Wednesday 30 October

October 30th
Hour
Task Attendant
1:00 1:30 2:00 2:30 3:00 3:30 4:00 4:30
Request work material, helmets and keys Carol
Prepare solutions ethanol-water of known
Camilo
concentratión
Density Measure Juan Antonio
Equipment adequacy Kristal
Load equipment, on PLC and purge Daniel
Supply steam, pressure 7ps, open reflux
Daniel
valve
Waiting the concentration Carol
Start up equipment Camilo
Open food valve, PLC temperature and
Alejandra
level control
Distillate and Waste flow Kristal
Ending equipment Juan Antonio

9. Sample calculation

Then we will use an approximate method such as McCabe-Thiele. First, we determine the approximate
value of the theoretical minimum reflux that could be worked in the column. This is possible with the use of
the concentration of the food that we will use(40% volume), and the concentration of distillate that we want
to get (96% volume), assuming that a food is entered as a saturated liquid.

In this way the molar composition of the food is:

(C i * þi )/(P M i )
Where:
C i = C oncentration in vol/vol

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þi = Density
P M i = M olecular weight

0, 4 * 0, 79/46, 1 = 0, 171 mol ethanol in liq phase/mol total

0, 6 * 0, 98/18 = 0, 829 mol water in liq phase/mol total


Then, ​intercepting the distillate line and cutting the line q (saturated liquid) with equilibrium, the minimum
reflux was found as follows:

According to the following equation:

b = X D / (Rmin + 1)

Rmin = (0, 89/0, 2822) − 1

Rmin = 2, 1537

Now, we determine operation reflux, it was proposed that it be 1.5 times the minimum, this corresponds to:

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Rope = 1, 5 * 2, 1537
Rope = 3, 23

Then, we determine the operation line with the expression:

b = X D / (Rope + 1)

b = 0, 88/ 3, 23 + 1

b = 0, 208
And the slope:

m = Rope/(Rope + 1)

m = 3, 23/(3, 23 + 1 )

m = 0, 7635
Finally, assuming the composition of ethanol in funds, the operation line of the enrichment and depletion
section is obtained:

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And the theoretical plates:

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10. Industry application:

Continuous distillation is widely used in chemical industry, due to its ease operation, high purity products
and the fact that it is not needed the use of a third component (i.e. solvents). However, it should not been
used in cases where concentration is too low or any interest compound is thermolabile.

Random packing distillation columns are usually used in distillation process with liquid rate above 50
m3/h/m2, where low pressure drop is desired. Besides, it is not expected presence of solids or fouling
(Pilling & Holden, 2009).

11. Experiment desired outcomes

Through the use of a continuous pilot scale column, we seek to strengthen the knowledge obtained
theoretically in previous courses regarding separation operations, specifically continuous distillation,
which has a wide industrial applicability.
It seeks to determine the degree of separation that can be opted with the tower for certain conditions to
later analyze and conclude the reason why these results are obtained.
With this practice it is also expected to obtain some knowledge regarding work at heights and the

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precautions that should be taken in these cases and the precautionary measures that must be taken into
account to ensure proper functioning of the tower.

12. Identification and assessment of risks along practice

Chemical Risks:

Additional risks
Substance H and P phrases Protocols used
classification

● Provide adequate general and local


exhaust ventilation.
● Wear protective gloves.
Water None known or appliable. None known.
● Chemical goggles or safety glasses.
● Do not eat, drink or smoke during use.

● H225 Highly flammable liquid


and vapour.
● Precautionary statements
P210 Keep away from
● Provide adequate ventilation. Observe
heat/sparks/open flames/hot
Occupational Exposure Limits and
surfaces. – No smoking.
● minimise the risk of inhalation of
● P233 Keep container tightly
vapours. Protective gloves and
closed.
goggles are
● P240 Ground/bond container
● recommended. Provide eyewash,
and receiving equipment.
quick drench.
● P241 Use explosion-proof
● Respiratory protection must be used if
electrical/ventilating/lighting//eq
air contamination exceeds acceptable
uipment.
● level. Use respiratory equipment with
● P242 Use only non-sparking
gas filter, type A2.
Ethanol tools. None known.
● Use protective gloves. Chemical
● P243 Take precautionary
resistant gloves required for
measures against static
prolonged or
discharge.
● repeated contact. Gloves of nitrile
● P280 Wear protective
rubber, PVA or Viton are
gloves/protective clothing/eye
recommended.
protection/face protection.
● Use safety goggles or face shield in
● P303 + P361 + P353 IF ON
case of splash risk.
SKIN (or hair): Remove/Take
● Wear appropriate clothing to prevent
off immediately all
any possibility of skin contact.
● contaminated clothing. Rinse
● Wash hands after contact.
skin with water/shower.
● P370 + P378 In case of fire:
Use for extinction.
● P403 + P235 Store in a

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well-ventilated place. Keep


cool.
● P501 Dispose of
contents/container to

Other risks:

The assessment of other kinds of risks (i.e. physical, biomechanical) is shown in Appendix 1. Practice
Risks Assessment Matrix. It was developed following the guides disposed by GTC-45 (2010), which is the
colombian technical guide applicable for this purpose.

According to this matrix, the levels of risk for the studied hazards were III and IV. Therefore, the risk levels
are acceptable while controls disposed by both LIQ and matrix are fulfilled.

BIBLIOGRAFÍA

Robert E. Treybal (1998). Operaciones de Transferencia de Masa. Mc-Graw Hill. 2 Ed.


Cap. 9 Destilación.

Otsuki, H., & Williams, F. C. (1953, January). Effect of pressure on vapor-liquid equilibria
for the system ethyl alcohol-water. In Chem Eng Progr Symp Ser (Vol. 49, No. 6, pp. 55-67).

Federación nacional de biocombustibles. (2018). Sitio


Web:http://www.fedebiocombustibles.com/v3/estadistica-precios-titulo-Alcohol_Carburante_(Etanol).h

Bello Hernandez, Forero Quimbaya, Lancheros Castañeda &Tibocha Bonilla (2016).


Evaluación del estado de la columna de destilación reactiva ubicada en la planta piloto del
laboratorio de ingeniería química. National University of Colombia. (Laboratory report).

Pilling, M., & Holden, B. S. (September, 2009). ​Razifar. Obtained from


http://www.razifar.com/cariboost_files/Choosing_20Trays_20and_20packings_20for_20distillation.p
df

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