Faculty of Engineering and Technology
Department of Chemical Engineering
Separation Processes-I
Chapter 04: Distillation
Lecturer: Sadak Mohamud Mohamed Abdo
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INSTRUCTIONALOBJECTIVES
After completing this chapter, you should be able to:
✓ Explain the need in distillation for a condenser to produce reflux and
a reboiler to produce boilup.
✓ Determine the five construction lines of the McCabe–Thiele method
using material balances and vapor–liquid equilibrium relations.
✓ Distinguish among five possible phase conditions of the feed.
✓ Apply the McCabe–Thiele method for determining minimum reflux
ratio, minimum equilibrium stages, number of stages for a specified
reflux ratio greater than minimum, and optimal feed-stage location,
given the required split between the two feed components.
✓ Use a Murphree vapor stage efficiency to determine the number of
actual trays from the number of equilibrium stages.
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Introduction
✓ The word distillation is derived from the Latin word
destillare, which means “dripping.”
✓ Distillation is a unit operation with the objective of
separation or fractionation, by vaporization, of a mixture of
miscible and volatile liquids into its components.
✓ Such fractionation is made possible by taking advantage of
the different vapor pressures of the components of the
mixtures at certain temperatures.
✓ When there is interaction between the liquid and vapor
phases, distillation is called rectification. When this
interaction is not present, the operation is called simple
distillation.
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Liquid–Vapor Equilibrium
✓ The transfer of material reaches a limit when
equilibrium between phases is achieved
✓ in order to reach a driving force for mass
transfer, equilibrium should be avoided.
✓ It is very important to know when equilibrium
between two phases occurs in order to evaluate
the driving forces.
✓ The composition of a vapor in equilibrium with a
liquid of a given composition is experimentally
determined by an equilibrium distiller, called
a boil-meter.
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Fig. 4.1 Temperature–composition diagram.
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✓ The mixture of composition x is known as Z
azeotropic mixture or, simply, azeotrope.
Fig. 4.2 T–X diagram for an azeotropic binary system.
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✓ Since industrial distillations take place basically at constant
pressure, it is more adequate to represent the liquid–vapor
compositions with a composition (x–y) diagram called an
equilibrium diagram
Fig. 4.3 y–x equilibrium diagram.
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Enthalpy Composition Diagram
✓ The molar or mass
fraction of the vapor
(y) and of the liquid (x)
are represented on the
abscissa, while the
enthalpies of vapor Hˆ
and of liquid hˆ are
represented on the
ordinate.
FIGURE Enthalpy–composition diagram.
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Distillation of Binary Mixtures
✓ There are different distillation methods for binary
mixtures.
✓ There are three main methods used in distillation
practice which all rely on this basic fact. These
are:
(a) Differential distillation.
(b) Flash or equilibrium distillation, and
(c) Rectification.
Rectification is much the most important, and it differs from the
other two methods in that part of the vapour is condensed and
returned as liquid to the still, whereas, in the other methods, all the
vapour is either removed as such, or is condensed as product.
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Industrial Example
• The purpose of the 25-sieve-
tray column, with a
condenser, reflux drum, and
reboiler, is to separate the
feed into a liquid distillate of
99 mol% benzene and a
liquid bottoms product of 98
mol% toluene.
Figure –Continuous distillation of a binary mixture of benzene and toluene.
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a) Differential distillation (Simple Distillation)
✓Works in a batch fashion in one stage only
✓A kettle is loaded with the mixture to be distilled and
vapors are formed by supplying heat.
✓Vapors are withdrawn continuously so that condensate
does not return to the kettle.
✓Initially, the vapors formed will contain a high
percentage of the most volatile component.
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✓ The composition of the mixture in the kettle varies
continuously so that the fraction of the heaviest
component increases and there is no steady state.
✓ Since heat is supplied to the kettle at a constant rate,
the boiling temperature of the load will increase as it
becomes poor in the most volatile component.
✓ Today, almost pure products are obtained by
continuous, multistage contacting.
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FIGURE Simple distillation.
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A global molar balance is carried out:
where L and V are the molar quantities of liquid and vapor
respectively in the kettle, while D is the amount of distillate
obtained. The molar density of vapor is much lower than that of
liquid, and where V is not so high, the last equation can be
expressed as:
Balance of the volatile component:
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A differential time range is complied with:
This is a differential equation with separable variables. If one
begins with L0 moles of composition x0, the integration of this
equation yields the expression:
This expression is
called Rayleigh’s
equation.
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When the equilibrium relationship is linear, that is, if
y = mx + c is complied with, the integral term has an
analytical solution:
If the equilibrium relationship is y = Kx, the following
equation is obtained:
When it can be assumed that the relative volatility is
constant, the integral term also has an analytical solution,
obtaining the expression:
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b) Flash Distillation
✓ Flash distillation, also called closed or equilibrium
distillation, consists of the evaporation of a certain
amount of liquid in such a way that the vapor
generated is in equilibrium with the residual liquid.
✓ The vapor is withdrawn and condensed separately.
✓ A mixture with L0 mol and composition x0 is
introduced in a chamber where the pressure is lower
than that of the mixture. In this way, V mol of vapor
with composition y and L mol of liquid with
composition x are separated.
✓ The compositions y, x of the separated phases are in
equilibrium.
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FIGURE Flash distillation: (a) installation sketch; (b) operation on the equilibrium
diagram.
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The following expressions are obtained from the global
balance and the volatile component:
Where f = 0, no vapor stream is generated and the mixture is not separated.
If f = 1, the whole mixture is vaporized, obtaining only a phase change without
fractionation of the mixture.
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c) Continuous Rectification of Binary Mixtures
✓ The term rectification is derived from the Latin words
recte facere, meaning “to improve.”
✓ In every distillation process the vapor formed in the
kettle is richer in the more volatile component than in
the remaining liquid.
✓ The vapor contains a certain amount of both
components and the distillate is rarely a pure
substance.
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✓ In order to increase the concentration of the more volatile
component in the vapor and to separate the less volatile
one, the vapor is brought into contact with a stream of
boiling liquid that runs down the column.
✓ A stream of liquid with a high concentration of the volatile
component, called reflux, is introduced at the top of the
column.
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✓ The most volatile components are concentrated in
the vapor phase and the least volatile in the liquid
phase
✓ The separation achieved in the mixture between the
top and bottom products depends on the
1. relative volatilities of the components,
2. number of contact stages, and
3. reflux ratio.
✓ This process is called rectification and is performed
in fractionating columns that operate in a continuous
mode
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✓ The plate in which feed is introduced divides the
column into two parts;
• The top is the rectification, or enrichment,
zone and
• The bottom is the exhaust zone or Stripping-
Section .
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Figure. Continuous fractionating
column with rectifying and stripping
sections
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FIGURE Rectification column
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FIGURE Evolution of the concentrations of phases in a plate n.
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✓ On each tray the system tends to reach equilibrium
because:
a) Some of the less volatile component LVC
condenses from the rising vapour into the liquid
thus increasing the concentration of the more
volatile component MVC in the vapor.
b) Some of the MVC is vaporized from the liquid on
the tray thus decreasing the concentration of the
MVC in the liquid.
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Figure . Material balances at top and bottom of column
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Design and Analysis Factors
The following factors that influence the design or analysis of
a binary-distillation operation are:
1. Feed flow rate, composition, 9. Type of reboiler (partial or total)
temperature, pressure,and phase 10. Type of trays or packing
2. Desired degree of component 11. Column height
separation 12. Feed-entry stage
3. Operating pressure (which must
13. Column diameter
be below the critical pressure of
14. Column internals and materials of
the mixture)
construction
4. Pressure drop, particularly for
vacuum operation 15. Heat lability and chemical reactivity
of feed components
5. Reflux ratio
16. Corrosion and materials of
6. Number of equilibrium stages and
construction
stage efficiency or HETP
17. Toxicity and flammability
7. Type of condenser (total, partial, or
mixed)
8. Degrees of liquid reflux subcooling
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Calculation of the Number of Plates
1. Mathematical Model
where A, D, and R are the molar streams of the feed,
distillate, and waste, respectively.
The enthalpies of the vapor streams are represented by Hˆ ,
while those of liquid are indicated by hˆ.
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Balances around the condenser:
is the latent heat of condensation of the vapor
mixture that reaches the condenser.
The amount of heat eliminated
in the condenser is:
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➢ Condenser
➢ At the top of column, three type of condenser:
a) Total condenser: takes the overhead vapor from the column
and liquefies it completely and split it into two portions:
1. Distillate which is called overhead product.
2. Reflux which return back to the top plate.
Overhead V Condenser
vapour
accumulator
L
D
Reflux
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b) Partial condenser: takes the over head vapor from the column and
liquefies a portion of it to return to the top plate as reflux, while the
other portion is vapor product or distillate.
c) Mixed condenser
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Balances around the kettle:
The heat that should be supplied
to the kettle is:
The enthalpies of the different streams that appear in the last equation depend not
only on temperature, but also on composition.
When the enthalpy of the
liquid is only a function of
temperature, assuming the
sensible heats as negligible
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Balances around the enrichment zone:
Balances around the exhaust zone:
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Balances around the feed plate:
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Solution of the Mathematical Model:
Method of McCabe–Thiele
➢ Once the mathematical model is set up, the next
step is to solve it with the corresponding data.
➢ Generally, data include feed flow A and the
compositions of feed x , of the waste x , and of
A R
the distillated x . D
➢ There are three solution methods for the
mathematical model.
1) Ponchon–Savarit method (enthalpy diagram is
employed)
2) The Lewis–Sorel method (analytically determines
the number of theoretical stages by step-by-step calculation)
3) McCabe–Thiele method
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✓ In order to apply the method of McCabe–Thiele to
calculate the number of theoretical plates of a
distillation column, the following hypotheses must
be verified:
• The specific heats of all liquids and vapors are
constant and equal.
• The latent heats of vaporization are constant and
equal.
• The mixing heats are null (Heat of mixing are negligible
compared to latent heat changes)
• The column works in an adiabatic form so heat
loss is negligible..
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✓ In general, Vn and Ln are constant in the enrichment
zone, and Vm and Lm are constant in the exhaust zone.
✓ Feed condition is an important datum in distillation
operations.
✓ The fraction of feed in liquid form is defined as q.
Therefore, when feed enters into the feed plate, the
fraction q.A will join the liquid stream that goes down
the column.
✓ If the hypotheses stated before are taken into account,
then the following is obtained when performing a
balance in this plate:
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The enthalpy balance in this plate yields
When it is complied that the liquid and vapor streams
are constant in each zone, and from the previous
equations, it is obtained that:
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Rectifying- Section Operating Line (Top)
This expression is the equation of a straight line in the y – x
equilibrium diagram, known as the enrichment line. This
straight line relates the composition of the vapor in plate n
with that of the liquid of the above plate n + 1
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The ratio LD/D, that is the ratio of the top overflow to the
quantity of product, is denoted r
Another way to express the enrichment line can be as:
In the x–y diagram, this straight line passes through points (xD, xD) and
(0, DxD/VD), and has slope LD/VD.
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McCabe–Thiele operating line for the rectifying section.
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Stripping- Section Operating Line
This expression is the equation of a straight line in the x–y
equilibrium diagram that passes by the point (xR, xR) and has
a slope equal to Lm/Vm.
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Feed - Stage Considerations—the q-Line
where the equation of a straight line represents the
geometric place where the operating lines intersect as a
function of the condition q of the feed. equation is called
line q.
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• Line q passes over the point (xA, xA) and has a
slope m = q/(q – 1).
• Therefore, if the enrichment operating line is
known when joining the point of intersection of the
enrichment line on line q with the point (xR, xR), the
exhaust operating line is obtained.
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q x
y= x+ F
q −1 1− q
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Depending on the condition of the feed, the value
of q as well as the slope of line q will be different:
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FIGURE Calculation of the number of plates by the McCabe–Thiele method.
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Figure. Possible feed
conditions:
(a)bubble-point liquid;
(b)dew-poin tvapor;
(c)subcooled liquid; (d)partially
vaporized; (e)superheated
vapor.
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Construction of operating lines
q x
1. Locate the feed line ( y= x+ F ) according to the feed
q −1 1− q
conditions.
2. Locate the rectifying line ( ). This line croces
xD
the diagonal at (xD, xD) and of intercept ( )
r +1
3. Draw the stripping line through point (xB, xB( an the
intersection of rectifying line with the feed line.
Note: xF, xB , xD, L,D are constant
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➢ Plate Feed Location
The feed plate is always represented by the triangle that has one
corner on the rectifying line and one on the stripping line
Note:
1. The number of plates = number of
plates + re-boiler plate.
2. The liquid on the feed plate does not
have the same composition as the
feed.
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Example 4.1 The McCabe-Thiele Method
A mixture of benzene and toluene containing 40 mole per cent
benzene is to be separated to give a product containing 90
mole per cent benzene at the top, and a bottom product
containing not more than 10 mole per cent benzene. The feed
enters the column at its boiling point, and the vapour leaving
the column which is condensed but not cooled, provides reflux
and product. It is proposed to operate the unit with a reflux
ratio of 3 kmol/kmol product. It is required to find the number of
theoretical plates needed and the position of entry for the feed.
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Solution
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LD is Ln This is thee equation of the top operating line
Thus, the line AB is drawn through the two points A (0.9, 0.9)
and B (0, 0.225).
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This is the equation of the bottom operating line
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Figure . Determination of number of plates by the McCabe–Thiele
method (Example 4.1)
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Plate Efficiency
✓ It is assumed that the streams leaving each plate
are in equilibrium, which is not true.
✓ For this reason, a greater number of plates will be
required to carry out the proposed distillation.
✓ For calculation of the real number of plates or
stages, three types of efficiency can be used:
1. global
2. Murphree’s or
Local efficiency is defined similarly to Murphree’s
3. local efficiency, but considering only one point of the plate.
Local efficiency is scarcely used in practice
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Number of Plates for Total Reflux
The number of theoretical plates N for the case of binary
mixtures with two components A and B is obtained from the
expression
The method of Fenske
N: is the required number of theoretical plates in the column.
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Example 4.2
For the separation of a mixture of benzene and toluene,
considered in Example 4.1, x d= 0.9, xw=0.1, and xf = 0.4. If
the mean volatility of benzene relative to toluene is 2.4, what
is the number of plates required at total reflux? Use Fenske’s
method
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Questions
1. What equipment is included in a typical distillation
operation?
2. What determines the operating pressure of a distillation
column?
3. Under what conditions does a distillation column need to
operate under vacuum?
4. Why are distillation columns arranged for counter current
flow of liquid and vapor?
5. Why is the McCabe–Thiele graphical method still useful
in this era of more rigorous, computer-aided algebraic
methods used in process simulators?
6. Under what conditions does the McCabe–Thiele
assumption of constant molar overflow hold?
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7. What is meant by reflux ratio?
8. What is the q-line and how is it related to the feed
condition?
9. What are the five possible feed conditions?
10.In the McCabe–Thiele method, are the stages stepped off
from the top down or the bottom up? In either case, when
is it best,
11.What is meant by subcooled reflux? How does it affect
the amount of reflux inside the column?
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12. In a single-stage, continuous distillation column used for
enriching alcohol/water mixtures, the feed contains 12% of
alcohol, and 25% of the feed passes out with the top
product (the "vapour" stream) from the still. Given that, at a
boiling temperature of 95.5°C, 1.9 mole% of alcohol in the
liquid is in equilibrium with 17 mole % of alcohol in the
vapour, estimate the concentration of alcohol in the product
from the still.
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14.Four hundred and fifty lbmol∕h(204 kmol∕h) of amixture of
60 mol% benzene (LK) and 40mol% toluene (HK) is to be
separated into a liquid distillate anda liquid bottoms
product of 95mol% and 5mol% benzene, respectively.The
feed enters the column with a molar percent vaporization
equal to the distillate-to-feed ratio. Use the McCabe–Thiele
method to compute, at 1atm (101.3kPa): (a) Nmin, (b) Rmin,
and (c) number of equilibrium stages N, for R/Rmin=1.3,
and the optimal feed-stage location. Also, compare the
results with those from a process simulator. Use Raoult’s
law to compute vapor–liquid equilibria
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