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Distillation

Tigabu Hailelule Yemane is an instructor of chemical engineering at Defense University. This chapter discusses distillation, including vapor pressure, phase diagrams, vapor-liquid equilibrium, distillation columns, and analysis of binary distillation. Distillation is an important separation process that relies on differences in boiling points. Key concepts covered include relative volatility, ideal and non-ideal vapor-liquid equilibrium curves, and azeotropes.

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0% found this document useful (0 votes)
52 views69 pages

Distillation

Tigabu Hailelule Yemane is an instructor of chemical engineering at Defense University. This chapter discusses distillation, including vapor pressure, phase diagrams, vapor-liquid equilibrium, distillation columns, and analysis of binary distillation. Distillation is an important separation process that relies on differences in boiling points. Key concepts covered include relative volatility, ideal and non-ideal vapor-liquid equilibrium curves, and azeotropes.

Uploaded by

Fekadu Dagnaw
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PPTX, PDF, TXT or read online on Scribd
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Defense University, College of Engineering

Department of Chemical Engineering


Heat and Mass Transfer Unit Operation
Instructor Name: Tigabu Hailelule Yemane
Profile of Instructor:
1.B.Tech in Chemical Engineering and MSc in Chemical Process and
Product Design
2. BA in Business Management and MBA
Chapter Two
Distillation
The content of this chapter
‣ Introduction
‣ Vapor Pressure
‣ Phase Diagram
‣ Vapor-Liquid Equilibrium (VLE)
‣ Distillation columns and their process calculations
‣ Analysis of binary distillation in tray towers
‣ Introduction to Multicomponent Distillation
Introduction
‣ Distillation is method of separation of components from a liquid mixture which depends on the
differences in boiling points of the individual components and the distributions of the
components between a liquid and gas phase in the mixture.
‣ The liquid mixture may have different boiling point characteristics depending on the
concentrations of the components present in it.
‣ Therefore, distillation processes depends on the vapor pressure characteristics of liquid
mixtures.
‣ The vapor pressure is created by supplying heat as separating agent. In the distillation, the new
phases differ from the original by their heat content.
‣ During most of the century, distillation was by far the most widely used method for separating
liquid mixtures of chemical components (Seader and Henley, 1998).
‣ This is a very energy intensive technique, especially when the relative volatility of the
components is low. It is mostly carried out in multi tray columns.
‣ Packed column with efficient structured packing has also led to increased use in distillation.
Vapor Pressure
‣ The vaporization process changes liquid to gaseous state.
‣ The opposite process of this vaporization is called condensation.
‣ At equilibrium, the rates of these two processes are same.
‣ The pressure exerted by the vapor at this equilibrium state is termed as the vapor pressure of
the liquid.
‣ It depends on the temperature and the quantity of the liquid and vapor.
‣ From the following Clausius-Clapeyron Equation or by using Antoine Equation, the vapor
pressure can be calculated.
‣ Clausius-Clapeyron Equation:

where pv and pV1 are the vapor pressures in Pascal at absolute temperature T and T1 in K. λ is
the molar latent heat of vaporization which is independent of temperature.
Antoine Equation:

‣ Typical representative values of the constants A, B and C are given in the following Table 2.1 (Ghosal et al., 1993).
‣ Table 2.1: Typical representative values of the constants A, B and C
Phase Diagram
‣ For binary mixture phase diagram only two-component mixture, (e.g. A (more volatile) and B
(less volatile)) are considered.
‣ There are two types of phase diagram: constant pressure and constant temperature.
Constant Pressure Phase Diagram
‣ The Figure 2.1 shows a constant pressure phase diagram for an ideal solution (one that obeys
Raoult's Law).
‣ At constant pressure, depending on relative concentrations of each component in the liquid,
many boiling point temperatures are possible for mixture of liquids (solutions) as shown in
phase diagram (Figure 2.1).
‣ For mixture, the temperature is called bubble point temperature when the liquid starts to boil
and dew point when the vapor starts to condense.
‣ Boiling of a liquid mixture takes place over a range of boiling points. Likewise, condensation
of a vapor mixture takes place over a range of condensation points.
‣ The upper curve in the boiling point diagram is called the dew-point curve (DPC) while the
‣ At each temperature, the vapor and the liquid are in equilibrium.
‣ The constant pressure phase diagram is more commonly used in the analysis of vapor-liquid
equilibrium.

Figure 2.1: Phase diagram of binary system at constant pressure


Constant temperature (isothermal) phase diagram
‣ The constant temperature phase diagram is shown in
Figure 2.2.
‣ The constant temperature phase diagram is useful in
the analysis of solution behavior.
‣ The more volatile liquid will have a higher vapor
pressure (i.e. pA at xA = 1.0)

Figure 5.2: Binary Phase


diagram at constant
Relative volatility
‣ Relative volatility is a measure of the differences in volatility between two components, and
hence their boiling points.
‣ It indicates how easy or difficult a particular separation will be.
‣ The relative volatility of component ‘A’ with respect to component ‘B’ in a binary mixture is
defined as

‣ where, yA = mole fraction of component ‘A’ in the vapor, xA = mole fraction of component ‘A’
in the liquid.
‣ In general, relative volatility of a mixture changes with the mixture composition. For binary
mixture, xB = 1-xA.
‣ where PA is the partial pressure of component A in the vapor, PB is the partial
pressure of component B in the vapor and P is the total pressure of the system.
‣ Thus if the relative volatility between two components is equal to one, separation
is not possible by distillation.
‣ The larger the value of α, above 1.0, the greater the degree of separability, i.e. the
easier the separation.
‣ Some examples of optimal relative volatility that are used for distillation process design are
given in Table 2.2.
Table 2.2: Some optimal relative volatility that are used for distillation process
Vapor-Liquid Equilibrium (VLE)
‣ It is useful for graphical design in determining the
number of theoretical stages required for a distillation
column.
‣ A typical equilibrium curve for a binary mixture on x-y
plot is shown in Figure 2.3.
‣ It contains less information than the phase diagram (i.e.
temperature is not included), but it is most commonly
used.
‣ The VLE plot expresses the bubble-point and the dew-
point of a binary mixture at constant pressure.
‣ The curved line in Figure 2.3 is called the equilibrium
Figure 2.3: Equilibrium line and it describes the compositions of the liquid and
diagram for a benzene-toluene vapor in equilibrium at some fixed pressure.
mixture at 1 atmosphere
Vapor-Liquid Equilibrium (VLE)
‣ This particular VLE plot (Figure 2.3) shows a binary
ideal mixture that has a uniform vapor-liquid
equilibrium that is relatively easy to separate.
‣ On the other hand, the VLE plots shown in Figure 2.4
represented for non-ideal systems.
‣ These non-ideal VLE systems will present more
difficult separation.
‣ The most challenging VLE curves are generated by
azeotropic systems. An azeotrope is a liquid mixture
which when vaporized, produces the same
composition as the liquid.
‣ Two types of azeotropes are known: minimum-boiling
Figure2.4:Vapor-liquid and maximum-boiling (less common).
equilibrium curve for non-ideal
systems
Vapor-Liquid Equilibrium (VLE)
‣ The most challenging VLE curves are generated by azeotropic systems.
‣ An azeotrope is a liquid mixture which when vaporized, produces the same composition as the
liquid.
‣ Two types of azeotropes are known: minimum-boiling and maximum-boiling (less common).
Ethanol-water system (at 1 atm, 89.4 mole %, 78.2 oC; Carbon-disulfide - acetone (61.0 mole
% CS2, 39.25 oC, 1 atm) and Benzene - water (29.6 mole% H2O, 69.25 oC, 1 atm) are
minimum-boiling azeotropes. Hydrochloric acid - water (11.1 mole% HCl, 110 oC, 1 atm);
‣ Acetone - chloroform (65.5 mole% chloroform, 64.5 oC, 1 atm) are the examples of
Maximum-boiling azeotropes.
‣ The Figure 2.5 shows two different azeotropic systems, one with a minimum boiling point
(Figure 2.5a) and one with a maximum boiling point (Figure 2.5b).
‣ The points of intersections of the equilibrium curves with the diagonal lines are called
azeotropic points.
‣ An azeotrope cannot be separated by conventional distillation. However, vacuum distillation
may be used as the lower pressures which can shift the azeotropic point.
Figure 2.5: VLE curves for azeotropic systems: (a) for maximum boiling point, (b) for minimum boiling point
‣ Although most distillations are carried out at atmospheric or near atmospheric pressure, it is
not uncommon to distill at other pressures.
‣ High pressure distillation (typically 3 - 20 atm) usually occurs in thermally integrated
processes.
‣ In those cases the equilibrium curve becomes narrower at higher pressures as shown in Figure
2.6. Separability becomes less at higher pressures.
Distillation columns and their process calculations
‣ There are many types of distillation columns each of which is designed to perform specific
types of separations.
‣ One way of classifying distillation column type is to look at how they are operated. Based on
operation, they are of two types: batch or differential and continuous columns.
Batch or differential distillation columns and their process calculation
‣ In batch operation, the feed is introduced batch-wise to the column. That is, the column is
charged with a 'batch' and then the distillation process is carried out.
‣ When the desired task is achieved, a next batch of feed is introduced. Consider a binary
mixture of components A (more volatile) and B (less volatile).
‣ The system consists of a batch of liquid (fixed quantity) inside a kettle (or still) fitted with
heating element and a condenser to condense the vapor produced as shown in Figure 2.7.
‣ The condensed vapor is known as the distillate.
‣ The distillate is collected in a condensate receiver. The liquid remaining in the still is known as
the residual.
‣ The process is unsteady state.
‣ The concentration changes can be analyzed using the phase diagram, and detailed
mathematical calculations carried out using the Rayleigh Equation.
‣ As the process is unsteady state, the derivation is based on a differential approach to changes in
concentration with time.
‣ Let L1 = initial moles of liquid originally in still, L2 = final moles of liquid remained in still,
x1 = initial liquid composition in still (mole fraction of A), x2 = final liquid composition in
still (mole fraction A).
‣ At any time t, the amount of liquid in the still is L, with mole fraction of A in the liquid being
x. After a small differential time (t + dt), a small amount of vapor dL is produced, and the
composition of A in the vapor is y (mole fraction).
‣ The vapor is assumed to be in equilibrium with the residue liquid.
‣ The amount of liquid in the still is thus reduced from L to (L - dL), while the liquid
composition changed from x to (x - dx).
‣ Then the material balance on A can be written as: Initial amount in still = Amount left in still +
Amount vaporized

Figure 2.7: Simple batch or differential distillation process


Example problem 2.1
A mixture of 40 mole % isopropanol in water is to be batch-distilled at 1 atm until 70 mole % of
the charge has been vaporized. Calculate the composition of the liquid residue remaining in the
still pot, and the average composition of the collected distillate. VLE data for this system, in mole
fraction of isopropanol, at 1 atm are (Seader and Henley, 1998):
Continuous distillation column
‣ In contrast, continuous columns process a continuous feed stream. No interruptions occur
unless there is a problem with the column or surrounding process units.
‣ They are capable of handling high throughputs. Continuous column is the more common of
the two types.
‣ Continuous columns can be further classified according to the nature of the feed that they are
processing:
‣ Binary distillation column: feed contains only two components
‣ Multi-component distillation column: feed contains more than two components the number of
product streams they have
‣ Multi-product distillation column: column has more than two product streams where the
extra feed exits when it is used to help with the separation
‣ Extractive distillation: where the extra feed appears in the bottom product stream
‣ Azeotropic distillation: where the extra feed appears at the top product stream the type of
column internals.
‣ Tray distillation column: where trays of various designs are used to hold up the liquid to
provide better contact between vapor and liquid, hence better separation.
‣ Packed distillation column: where instead of trays, 'packings' are used to enhance contact
between vapor and liquid.
A single-stage continuous distillation (Flash distillation):
‣ A single-stage continuous operation occurs where a liquid mixture is partially vaporized.
‣ The vapor produced and the residual liquids are in equilibrium in the process are separated and
removed as shown in Figure 2.8.
‣ Consider a binary mixture of A (more volatile component) and B (less volatile component).
The feed is preheated before entering the separator.
‣ As such, part of the feed may be vaporized.
‣ The heated mixture then flows through a pressure-reducing valve to the separator. In the
separator, separation between the vapor and liquid takes place.
‣ The amount of vaporization affects the concentration (distribution) of A in vapor phase and
liquid phase.
‣ The relationship between the scale of vaporization and mole fraction of A in
vapor and liquid (y and x) is known as the Operating Line Equation.
‣ Define f as molal fraction of the feed that is vaporized and withdrawn
continuously as vapor.
‣ Therefore, for 1 mole of binary feed mixture, (1- f) is the molal fraction of the
feed that leaves continuously as liquid. Assume, yD = mole fraction of A in vapor
leaving, xB = mole fraction of A in liquid leaving, xF = mole fraction of A in feed
entering.
‣ Based on the definition for f, the greater the heating is, the larger the value of f.
‣ If the feed is completely vaporized, then f = 1.0 Thus, the value of f can varies
from 0 (no vaporization) to 1 (total vaporization).
‣ The fraction f depends on the enthalpy of the liquid feed, the enthalpies of the
vapor and liquid leaving the separator.
Figure 2.8: Flash distillation process
Figure 2.9: Graphical presentation of flash vaporization
Multi-stage Continuous distillation-Binary system
‣ A general schematic diagram of a multistage counter-current binary distillation operation is
shown in Figure 2.10.
‣ The operation consists of a column containing the equivalent N number of theoretical stages
arranged in a two-section cascade; a condenser in which the overhead vapor leaving the top
stage is condensed to give a liquid distillate product and liquid reflux that is returned to the top
stage; a reboiler in which liquid from the bottom stage is vaporized to give a liquid bottom
products and the vapor boil off returned to the bottom stage;
‣ accumulator is a horizontal (usually) pressure vessel whereby the condensed vapor is collected;
Heat exchanger where the hot bottoms stream is used to heat up the feed stream before it enters
the distillation column.
‣ The feed enters the column at feed stage contains more volatile components (called light key,
LK) and less volatile components (called heavy key, HK). At the feed stage feed may be liquid,
vapor or mixture of liquid and vapor.
‣ The section above the feed where vapor is washed with the reflux to remove or absorb the
heavy key is called enriching or rectifying section.
‣ The section below the feed stage where liquid is stripped of the light key by the rising vapor is
called stripping section.
Analysis of binary distillation in tray towers: McCabe Thiele
Method
‣ McCabe and Thiele (1925) developed a graphical method to determine the theoretical number
of stages required to effect the separation of a binary mixture (McCabe and Smith, 1976).
‣ This method uses the equilibrium curve diagram to determine the number of theoretical stages
(trays) required to achieve a desired degree of separation.
‣ It assumes constant molar overflow and this implies that: (i) molal heats of vaporization of the
components are roughly the same; (ii) heat effects are negligible.
‣ The information required for the systematic calculation are the VLE data, feed condition
(temperature, composition), distillate and bottom compositions; and the reflux ratio, which is
defined as the ratio of reflux liquid over the distillate product.
‣ For example, a column is to be designed for the separation of a binary mixture as shown in
Figure 2.11.
Figure 5.11: Schematic of column for separation of binary mixture
‣ The feed has a concentration of xF (mole fraction) of the more volatile component, and a distillate
having a concentration of xD of the more volatile component and a bottoms having a concentration of
xB is desired.
‣ In its essence, the method involves the plotting on the equilibrium diagram three straight lines: the
rectifying section operating line (ROL), the feed line (also known as the qline) and the stripping
section operating line (SOL).
‣ An important parameter in the analysis of continuous distillation is the Reflux Ratio, defined as the
quantity of liquid returned to the distillation column over the quantity of liquid withdrawn as product
from the column, i.e. R = L / D.
‣ The reflux ratio R is important because the concentration of the more volatile component in the
distillate (in mole fraction xD) can be changed by changing the value of R.
‣ The steps to be followed to determine the number of theoretical stages by McCabe-Thiele Method:
1. Determination of the Rectifying section operating line (ROL).
2. Determination the feed condition (q).
3. Determination of the feed section operating line (q-line).
4. Determination of required reflux ratio (R).
6.Determination of number of theoretical stage.
Determination of the Rectifying section operating line (ROL)
‣ Consider the rectifying section as shown in the Figure 2.12.
‣ Material balance can be written around the envelope shown in Figure 2.12:
Figure 2.13: Representation of the rectifying operating line
Determination the feed condition (q)
‣ The feed enters the distillation column may consists of liquid, vapor or a mixture of both.
‣ Some portions of the feed go as the liquid and vapor stream to the rectifying and stripping
sections.
‣ The moles of liquid flow in the stripping section that result from the introduction of each mole
of feed, denoted as ‘q’. The limitations of the q-value as per feed conditions are shown in Table
2.3.
Table 2.3: Limitations of q-value as per feed conditions
Calculation of q-value
1. When feed is partially vaporized:
‣ Other than saturated liquid (q = 1) and saturated vapor (q = 0), the feed condition is uncertain.
In that case one must calculate the value of q.
‣ The q-value can be obtained from enthalpy balance around the feed plate. By enthalpy balance
one can obtain the q-value from the following form of Equation:

‣ where HF, HV and HL are enthalpies of feed, vapor and liquid respectively which can be
obtained from enthalpy-concentration diagram for the mixture.
2. When feed is cold liquid or superheated vapor:
‣ q can be alternatively defined as the heat required to convert 1 mole of feed from its entering
condition to a saturated vapor; divided by the molar latent heat of vaporization.
‣ Based on this definition, one can calculate the q-value from the following Equations for the
case whereby q > 1 (cold liquid feed) and q < 0 (superheated vapor feed) as
2.1.For cold liquid feed:

For superheated vapor feed:


Determination of the feed section operating line (q-line):
‣ Consider the section of the distillation column (as shown in Figure 2.11) at the tray (called feed
tray) where the feed is introduced.
‣ In the feed tray the feed is introduced at F moles/hr with liquid of q fraction of feed and vapor
of (1-f) fraction of feed as shown in Figure 2.14.
‣ Overall material balance around the feed

‣ Component balances for the more volatile component in the rectifying and stripping sections
are:
‣ For rectifying section:
‣ For stripping section:
‣ At the feed point where the two operating lines intersect can be written as:

Figure 2.14: Feed tray with fraction of liquid and vapor of feed
‣ From component balance around the entire column, it can be written as

‣ one can get the q-line Equation after rearranging as:

‣ For a given feed condition, xF and q are fixed, therefore the q-line is a straight line with slope -
q / (1-q) and intercept xF/(1-q). If x = xF , then from Equation above y = xF.
‣ At this condition the q-line passes through the point (xF, xF) on the 45 diagonal.
‣ Different values of q will result in different slope of the q-line.
‣ Different q-lines for different feed conditions are shown in Figure 2.15.
Figure 2.15: Different q-lines for different feed conditions
Determination of the stripping section operating line (SOL)
‣ The stripping section operating line (SOL) can be obtained from the ROL and qline without
doing any material balance.
‣ The SOL can be drawn by connecting point xB on the diagonal to the point of intersection
between the ROL and q-line.
‣ The SOL will change if q-line is changed at fixed ROL.
‣ The change of SOL with different q-lines for a given ROL at constant R and xD is shown in
Figure 2.16.

Figure 2.16: Stripping section operating line with different q-lines


‣ The stripping section operating line can be derived from the material balance around the stripping
section of the distillation column.
‣ The stripping section of a distillation column is shown in Figure 2.17.
‣ The reboiler vapor is in equilibrium with bottoms liquid which is leaving the column.
Determination of number of theoretical stage
‣ Suppose a column is to be designed for the separation of a binary mixture where
the feed has a concentration of xF (mole fraction) of the more volatile component
and a distillate having a concentration of xD of the more volatile component
‣ whereas the bottoms having a desired concentration of xB.
‣ Once the three lines (ROL, SOL and q-line) are drawn, the number of theoretical
stages required for a given separation is then the number of triangles that can be
drawn between these operating lines and the equilibrium curve.
‣ The last triangle on the diagram represents the reboiler.
‣ A typical representation is given in Figure 2.18.

Figure 2.18: A typical representation of identifying number of theoretical stages
Reflux Ratio, R
‣ The separation efficiency by distillation depends on the reflux ratio.
‣ For a given separation (i.e. constant xD and xB) from a given feed condition (xF and q), higher
reflux ratio (R) results in lesser number of required theoretical trays (N) and vice versa.
‣ So there is an inverse relationship between the reflux ratio and the number of theoretical
stages. At a specified distillate concentration, xD, when R changes, the slope and intercept of
the ROL changes (Equation (5.19)).
‣ when R increases (with xD constant), the slope of ROL becomes steeper, i.e. (R/R+1) and the
intercept (xD/R+1) decreases.
‣ The ROL therefore rotates around the point (xD, xD). The reflux ratio may be any value
between a minimum value and an infinite value.
‣ The limit is the minimum reflux ratio (result in infinite stages) and the total reflux or infinite
reflux ratio (result in minimum stages). With xD constant, as R decreases, the slope (R/R+1) of
ROL decreases, while its intercept (xD/R+1) increases and rotates upwards around (xD, xD) as
shown in Figure 5.19.
Figure 2.19: Representation of minimum reflux ratio
‣ At this point of intersection the driving force for mass transfer is zero.
‣ This is also called as Pinch Point. At this point separation is not possible.
‣ The R cannot be reduced beyond this point. The value of R at this point is known as the
minimum reflux ratio and is denoted by Rmin.
‣ For non-ideal mixture it is quite common to exhibit inflections in their equilibrium curves as
shown in Figure 2.20 (a, b). In those cases, the operating lines where it becomes tangent to the
equilibrium curve (called tangent pinch) is the condition for minimum reflux.
‣ The ROL cannot move beyond point P, e.g. to point K.
‣ The condition for zero driving force first occurs at point P, before point K which is the
intersection point between the qline and equilibrium curve.
‣ Similarly it is the condition SOL also. At the total reflux ratio, the ROL and SOL coincide
with the 45 degree diagonal line.
‣ At this condition, total number of triangles formed with the equilibrium curve is equal
minimum number of theoretical stages.
‣ The reflux ratio will be infinite.
Figure .20 (a): Representation of minimum Figure .20 (b): Representation of minimum
reflux ratio for non-ideal mixture reflux ratio for non-ideal mixture
Tray Efficiency
‣ For the analysis of theoretical stage required for the distillation, it is assumed that the the vapor
leaving each tray is in equilibrium with the liquid leaving the same tray and the trays are
operating at 100% efficiency. In practice, the trays are not perfect.
‣ There are deviations from ideal conditions.
‣ The equilibrium with temperature is sometimes reasonable for exothermic chemical reaction
but the equilibrium with respect to mass transfer is not often valid.
‣ The deviation from the ideal condition is due to: (1) Insufficient time of contact (2)
Insufficient degree of mixing.
‣ To achieve the same degree of desired separation, more trays will have to be added to
compensate for the lack of perfect separability.
‣ The concept of tray efficiency may be used to adjust the actual number of trays required.
Overall Efficiency
 The overall tray efficiency, EO is defined as:

‣ It is applied for the whole column. Every tray is assumed to have the same efficiency.
‣ The overall efficiency depends on the (i) geometry and design of the contacting trays, (ii) flow
rates and flow paths of vapor and liquid streams, (iii) Compositions and properties of vapor
and liquid streams (Treybal, 1981; Seader and Henley, 1998).
‣ The overall efficiency can be calculated from the following correlations:
‣ The Drickamer-Bradford empirical correlation:
Murphree Efficiency
‣ The efficiency of the tray can also be calculated based on semi-theoretical models which can
be interpreted by the Murphree Tray Efficiency EM.
‣ In this case it is assumed that the vapor and liquid between trays are well-mixed and have
uniform composition.
‣ It is defined for each tray according to the separation achieved on each tray based on either the
liquid phase or the vapor phase. For a given component, it can be expressed as:
‣ Based on vapor phase:

‣ Based on liquid phase:


Example problem 2.2:

A liquid mixture of benzene toluene is being distilled in a fractionating column at 101.3 k Pa


pressure. The feed of 100 kmole/h is liquid and it contains 45 mole% benzene (A) and 55 mole%
toluene (B) and enters at 327.6 K. A distillate containing 95 mole% benzene and 5 mole% toluene
and a bottoms containing 10 mole% benzene and 90 mole% toluene are to be obtained. The
amount of liquid is fed back to the column at the top is 4 times the distillate product. The average
heat capacity of the feed is 159 KJ/kg mole. K and the average latent heat 32099 kJ/kg moles.
Calculate
i. The kg moles per hour distillate, kg mole per hour bottoms
ii. No. of theoretical stages at the operating reflux.
iii. The minimum no. of theoretical stages required at total reflux
iv. If the actual no. of stage is 10, what is the overall efficiency increased at operating condition
compared to the condition of total reflux?
The equilibrium data:

Figure E1: Graph representing the example problem 2.2.


Analysis of binary distillation by Ponchon-Savarit Method
Background Principle:
‣ The method is concerned with the graphical analysis of calculating the theoretical stages by
enthalpy balance required for desired separation by distillation process (Hines and Maddox,
1984).
‣ In this method, the enthalpy balances are incorporated as an integral part of the calculation
however it is not considered in the analysis separation by distillation process by McCabe-Thele
method.
‣ This procedure combines the material balance calculations with enthalpy balance calculations.
This method also provides the information on the condenser and reboiler duties.
‣ The overall material balance for the distillation column is as shown in Figure 2.11.
‣ The points represented by the feed, distillate and bottom streams can be plotted on the
enthalpy-concentration diagram as shown in Figure 2.21.
‣ The overall material balance for the distillation Colum:
‣ For any component the material balance around the column can be written as:
‣ Overall enthalpy balance for the column yields:
‣ where H is the enthalpy of the liquid stream, energy/mol, QR is the heat input to the reboiler,
J/s and QC is the heat removed from condenser, J/s. The heat balance on rearrangement of
gives

‣ The points represented by the feed, distillate and bottom streams can be plotted on the
enthalpy-concentration diagram as shown in Figure 2.21.


Figure 2.21: Representation of feed, distillate and bottom streams on the enthalpy-concentration
Analysis of binary distillation by Ponchon-Savarit Method
‣ Comparing the last Equation with the points plotted on Figure (2.21), it is found that the left hand side of the last
Equation represents the slope of the straight line between the points (xB, HB-QR/B) and (xF, HF).
‣ The right hand side of the Equation represents the slope of the straight line passing through the points (xF, HF)
and (xD, HD-QC/D).
‣ From this it can be said that all three points are on a same straight line.
‣ The amount of distillate as per Equation is proportional to the horizontal distance and the amount of bottoms is
proportional to the horizontal distance FD xx , then from the overall material balance it can be interpreted that the
amount of feed is proportional to the horizontal distance BD xx .
‣ This leads to the inverse lever rule. Based on this principle, the analysis of distillation column is called Enthalpy-
composition analysis or Ponchon-Savarit analysis of distillation column.

Analysis of tray column


‣ Consider the theoretical stage shown in Figure 2.12 and the principle by which it operates is described in the
enthalpy-composition diagram as shown in Figure 2.22.
‣ The vapor entering to the tray (n), Vn+1 is a saturated vapor of composition yn+1 whereas the liquid entering to
the tray is Ln-1 of composition xn-1. The point P in the Figure 2.22 represents the total flow to the tray.
‣ The point P lies in a straight line joining xn-1 and yn+1.
Stepwise procedure to determine the number of theoretical trays:
Step 1: Draw the equilibrium curve and the enthalpy concentration diagram for the mixture to be
separated
Step 2: Calculate the compositions of the feed, distillate and bottom products. Locate these
compositions on the enthalpy-concentration diagram.
Step 3: Estimate the reflux rate for the separation and locate the rectifying section difference
point as ΔR as shown in Figure 5.23. Point y1 is the intersection point of line joining point xD
and ΔR and HV-y curve.
Step 4: Locate the stripping section difference point Δs. The point Δs is to be located at a point
where the line from ΔR through xF intersects the xB composition coordinate as shown in Figure
4.23.
Step 5: Step off the trays graphically for the rectifying section. Then the point of composition x1
of liquid of top tray is to be determined from the equilibrium relation with y1 of vapor which is
leaving the tray and locate it to the HL-x curve. Then the composition y2 is to be located at the
point where the line of points ΔR and x1 intersects HV-y curve. This procedure is to be continued
until the feed plate is reached.
‣ The distance is proportional to the quantity Ln-1 and the distance is proportional to
the quantity Vn+1 as per lever rule.
‣ So

‣ The sum of the liquid and vapor leaving the plate must equal the total flow to the plate. So the
tie line must pass through the point P which represents the addition point of the vapor Vn and
liquid Ln leaving the tray.
‣ The intersection of the tie line with the enthalpy-composition curves will represent the
compositions of these streams.
‣ The distance is proportional to the quantity Ln-1 and the distance is proportional to
the quantity Vn+1 as per lever rule.
‣ So

‣ The sum of the liquid and vapor leaving the plate must equal the total flow to the plate. So the
tie line must pass through the point P which represents the addition point of the vapor Vn and
liquid Ln leaving the tray.
‣ The intersection of the tie line with the enthalpy-composition curves will represent the
compositions of these streams.
Figure 2.22: Operation principle of stage-wise binary distillation on enthalpy-concentration
diagram
Introduction to Multicomponent Distillation
‣ In industry, most of the distillation processes involve with more than two components. The
multicomponent separations are carried out by using the same type of distillation columns,
reboilers, condensers, heat exchangers and so on.
‣ However some fundamental differences are there which is to be thoroughly understood by the
designer. These differences are from phase rule to specify the thermodynamic conditions of a
stream at equilibrium.
‣ In multicomponent systems, the same degree of freedom is not achieved because of the
presence of other components.
‣ Neither the distillate nor the bottoms composition is completely specified. The components
that have their distillate and bottoms fractional recoveries specified are called key components.
‣ The most volatile of the keys is called the light key (LK) and the least volatile is called the
heavy key (HK).
‣ The other components are called non-keys (NK). Light no-key (LNK) is referred when non-
key is more volatile than the light key whereas heavy non-key (HNK) is less volatile than the
heavy key. Proper selection of key components is important if a multicomponent separation is
‣ Several short-cut methods are used for carrying out calculations in multicomponent systems.
‣ These involve generally an estimation of the minimum number of trays, the estimation of
minimum reflux rate and number of stages at finite reflux for simple fractionators.
‣ Although rigorous computer methods are available to solve multicomponent separation
problems, approximate methods are used in practice.
‣ A widely used approximate method is commonly referred to as the Fenske-Underwood-
Gilliland method.
Estimation of Minimum number of trays: Fenske Equation
‣ Fenske (1932) was the first to derive an Equation to calculate minimum number of trays for multicomponent distillation at
total reflux.
‣ The derivation was based on the assumptions that the stages are equilibrium stages.
‣ Consider a multicomponent distillation column operating at total reflux as shown in Figure 5.24.
‣ Equilibrium relation for the light key component on the top tray is
Figure 2.24: Multicomponent column at minimum trays
Minimum Reflux: Underwood Equations
‣ For multi-component systems, if one or more of the components appear in only one of the
products, there occur separate pinch points in both the stripping and rectifying sections.
‣ In this case, Underwood developed an alternative analysis to find the minimum reflux ratio
(Wankat, 1988).
‣ The presence of non-distributing heavy non-keys results a pinch point of constant composition
at minimum reflux in the rectifying section whereas the presence of non-distributing light non-
keys, a pinch point will occur in the stripping section.
‣ Let us consider the pinch point is in the rectifying section.
‣ The mass balance for component i around the top portion of the rectifying section as illustrated
in Figure 5.24 is
Analysis of binary distillation by Ponchon-Savarit Method
Analysis of binary distillation by Ponchon-Savarit Method
Analysis of binary distillation by Ponchon-Savarit Method

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