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CH3551 MASS TRANSFER-II Vapor leaving the top of the column passes through a heat exchanger, the condenser, where it is
UNIT II-DISTILLATION partially or totally condensed. The liquid which results is temporarily held in the "accumulator" or reflux drum.
Vapour liquid equilibria - Raoult‘s law, vapor-liquid equilibrium diagrams for ideal and non-ideal systems, A liquid stream is withdrawn from the drum and returned to the top tray of the column as reflux (R or L) to
enthalpy concentration diagrams. Principle of distillation - flash distillation, differential distillation, steam promote separation.
distillation, multistage continuous rectification, Number of ideal stages by Mc.Cabe - Thiele method and The portion of the column above the feed tray is called the rectification section. In this section, the
Ponchan - Savarit method, Total reflux, minimum reflux ratio, optimum reflux ratio. Introduction to multi- vapor is enriched by contact with the reflux.
component distillation, azeotropic and extractive distillation The portion of the column below the feed tray is called the stripping section. The liquid portion of
********************************************************* the feed serves as the reflux for this section. The operating pressure of the column is typically controlled by
DISTILLATION adjusting heat removal in the condenser.
Distillation is a method of separating the components of a solution which depends upon the The base of the column is typically used as a reservoir to hold liquid leaving the bottom tray. A heat
distribution of the substances between a gas and a liquid phase, applied to cases where all components are exchanger, the reboiler, is used to boil this liquid. The vapor which results, the "boilup" (V) is returned to the
present in both phases. This unit operation is also termed as Fractionation or Fractional distillation. column on one of the bottom three or four trays.
Distillation is the most widely used separation process in the chemical industry. It is normally used to In normal operation, there are five "handles" that can be adjusted to manipulate the behavior of a
separate liquid mixtures into two or more vapor or liquid products with different compositions. distillation column - the feed flow, two product flows, the reflux flow, and the boil up flow (or) reboiler heat
Distillation is an equilibrium stage operation. In each stage, a vapor phase is contacted with a liquid input. A normal column has a temperature gradient and a pressure gradient from bottom to top.
phase and mass is from vapor to liquid and from liquid to vapor. The less volatile, "heavy" or "high boiling", CONCEPT OF DISTILLATION
components concentrate in the liquid phase; the more volatile, "light", components concentrate in the In distillation, the phase involved are liquid and vapour or gas and mass is transferred from both the
vapor. By using multiple stages in series with recycle, separation can be accomplished. phase to one another.
Distillation is commonly encountered in chemical and petroleum industries as a means of separating a. Vaporization from liquid phase.
the liquid mixture into its component parts. The separation of a mixture of ethanol and water, production of b. Condensation from vapour phase.
absolute alcohol from 95% ethyl alcohol using benzene, the separation of petroleum crude into gasoline, Boiling Point
kerosene, fuel oils, etc. are typical examples of distillation. For any given pressure, a pure liquid when heated will boil or vaporise at a certain single
Evaporation is concerned with the separation of a solution containing a non-volatile solute and a temperature known as boiling point of the liquid. Boiling point of a liquid increases with increase in
volatile solvent whereas distillation is concerned with the separation of solutions where all the components are pressure and vice versa. Boiling points at a given pressure vary greatly for different liquids.
appreciably volatile. The separation of a mixture of alcohol and water into its components is a distillation. For example, boiling point of water is 373K (100°C), that of toluene is 383.6K (110.6°C) and that of
Operating Principles methanol is 337.7K (64.7°C) at one atmosphere (101.325kPa).
The feed to a distillation column may be liquid, vapor, or a liquid-vapor mixture. It may enter at any In the binary mixture (two component system), the component with lower boiling point or
point in the column, although the optimal feed tray location should be determined and used. More than one component with higher vapour pressure at a given temperature, is termed as more volatile or lighter and
stream may be fed to the system, and more than one product may be drawn. the component with higher boiling point or with lower vapour pressure at a given temperature is termed as less
A column is divided into a series of stages. These correspond to a cascade of equilibrium stages. Liquid volatile or heavier.
flows down the column from stage to stage and is contacted by vapor flowing upward. Thus in case of binary mixture of methanol and water, methanol is more volatile component and
Traditionally, most columns have been built from a set of distinct "trays" or "plates", so these water is less volatile component. The whole mixture of methanol and water will boil somewhere between
terms end up being essentially interchangeable with "stages". Each tray in a distillation column is designed to 337.7K (64.7°C) and 373K (100°C) at atmospheric pressure (101.325kPa).
promote contact between the vapor and liquid on the stage. Equilibrium
Stages may be numbered from top down or bottom up. When analyzing a stage, flows and compositions Separation of components by distillation is that composition of vapour be different from the composition
take the number of the stage they leave. The text for this class calls the top tray of the column "Tray 1" and of the liquid which it is ‗equilibrium‘. Equilibrium refers to the absence of any tendency for a change to take
numbers downward-this is the convention we will use. It is also denoted for the streams between the column place or occur. It is a static condition in which the net transfer of material between the phases ceases for a
top and condenser with an "a" subscript and those at the bottom with "b". Generally prefer to let "Tray 1" be the given set of operating conditions.
bottom tray of the column, the reboiler "Tray 0" and number upward. Driving force
The product leaving the top of the column is called the overhead product, the "overhead", the When two phases (not at equilibrium) are brought into intimate contact, the phases will tend to approach
"top product", the distillate, or "distillate product". Distillate product may be liquid or vapor depending on equilibrium due to a tendency for a change to take place. The difference between the existing condition and the
the type of condenser used. Most of the time the distillate flow rate is assigned the symbol D, and the equilibrium condition is the driving force which causes a change. Concentration difference is the driving
composition xD (or) yD. force for mass transfer analogous.
The product leaving the bottom of the column is called the bottom product or "bottoms", and given the Equilibrium stage
symbol W, with composition xw. In some situations, notably petroleum refining, one or more intermediate or Equilibrium stage is defined as the one in which two insoluble phases not at equilibrium are
"sidedraw" products may be removed from the column. brought into contact, sufficient time is provided to attain equilibrium, the phases are separated and
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streams leave the stage in equilibrium. For a given set of operating conditions, an equilibrium stage gives Consider the upper curve provides the temperature – vapour composition (T-y*) relationship, the lower
maximum possible composition change, so it is also known as the ideal or theoretical stage. that of the temperature – liquid (T-x) relationship composition.
Mass transfer devices consist of a series of stages through which phases flow, from one to the other, in a
counter current fashion. A stage consists of two steps:
(i) Intimate contacting of two insoluble phases: Where by mass transfer occurs between the phases
tending to bring them to equilibrium.
(ii) Mechanical separation of the phases: Device or combination of devices wherein two insoluble phases
are first brought into intimate contact whereby mass transfer occurs between the phases and the phases
are then mechanically separated is referred to as a stage. A process carried out in this manner is a single-
stage process. For separations requiring greater changes in concentration, the phases flow counter
current to each through a series of stages and the process carried out in this manner is called a
multistage process. Such a multistage arrangement is called a cascade. In such a case for establishing a
standard to measure the performance, the equilibrium, ideal or theoretical stage concept is introduced.
Ideal Stages
The ideal or theoretical stage is the one from which the phases leaving (the effluent Phases) are in
equilibrium with each other, so that no additional change in the composition results by providing a further RAOULT’S LAW
time of contact between the phases. It is commonly used for predicting the vapour-liquid equilibrium for an ideal solution in equilibrium
Stages are built to maximize contact between the incoming vapor and the incoming liquid. During the with an ideal gas mixture from the pure component vapour-pressure data.
contact, some of the liquid component in the entering liquid is vaporized and leaves with the vapor; some of the *
It states that the equilibrium partial pressure PA of a component in a solution at a given
heavy component in the entering vapor condenses and leaves with the liquid. temperature is equal (or directly proportional) to the product of its vapour pressure ‘pA’ in the pure
By definition, an ideal stage is one where the vapor and liquid leave the stage in equilibrium. state and its mole fraction ‘x’ in the liquid phase.
Consequently, the vapor composition functionally depends on the liquid composition. Ideality is an *
Thus, for a binary (two component) system, if PA is the equilibrium partial pressure of A, pA is the
approximation, but stage efficiencies can be used to account for real cases. A key result of the ideal stage
assumption is that liquid streams leaving an ideal stage are assumed to be at their bubble point. Vapor streams vapour pressure of A in the pure state and xA the mole fraction of A in liquid phase, then
PA  p A x A
*
leave at their dew point.
When no azeotropes are present, both top and bottom products may be obtained in any desired purity-if For components B,
enough stages are provided and enough reflux is available. Theoretical limits on performance are imposed by
PB  pB xB
*
total reflux (minimum stages) and minimum reflux (infinite number of ideal stages).
PB  pB (1  xA ) ( x A  xB  1)
*
Vapour – liquid Equilibria (VLE)
Successful application of distillation method depends greatly upon an understanding of equilibrium Where,
existing between the vapour and liquid phase of the mixture encountered. *
PB - Equilibrium partial pressure of component B
The equilibrium in vapour-liquid systems is governed by phase rule. In case of a binary mixture
subjected to distillation, the components (C) involved are two, the phases (P) involved are two (vapour and pB - Vapour pressure of pure component B
liquid), so according to the phase rule [F = C - P + 2], the degree of freedom (F) or the number of intensive xB - Mole fraction of B in liquid phase
variables that can be varied independently are two. DALTON'S LAW
In distillation, there are four variables: temperature, pressure, vapour phase composition and liquid It states that the total pressure exerted by a gas or vapour mixture is equal to the sum of the partial
phase composition Thus, if the pressure is fixed then only one variable say, for example, the liquid phase pressures of the components present in it. Thus, it expresses the additive nature of partial pressures.
composition can be changed independently, and the temperature and vapour phase composition then follow. Mathematically, for a binary system,
P  PA  PB
* *
Constant-Pressure Vapour-Liquid Equilibria
Vapour-liquid equilibrium refers to systems where in a single liquid phase is in equilibrium with its Where, P is the total pressure.
vapour. We restrict our discussion to binary systems (systems containing two chemical species). Equilibrium in For ideal gas or vapour, the partial pressure is related to the mole fraction of the component in the gas or
vapour-liquid systems is usually expressed in terms of the mole fraction of the more volatile component in the vapour phase by the relation:
vapour phase (y) and the mole fraction of the same component in the liquid phase (x). Vapour-liquid Partial pressure = Mole fraction x Total pressure
equilibrium data for a binary system at constant total pressure are represented by means by Thus, for component A,
(i) The temperature-composition diagram (the T-x-y diagram or boiling point diagram).
PA  y A.P
*
(ii) The equilibrium curve (x-y plot/diagram or distribution diagram).
Where, yA is the mole fraction of A in the vapour phase.
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RELATIVE VOLATILITY Relative volatility is a measure of the separability by distillation. When α = 1, a separation by
Volatility is defined as the ratio of the partial pressure of A to the mole fraction of A in the liquid phase. distillation is not possible. The separation by distillation is possible for relative volatility values greater than
P
* one. Larger the value of the relative volatility, the easier is the separation by distillation.
Volatality of A  A METHODS OF DISTILLATION
xA
*
Basically distillation is carried out in two ways:
P
Similarly, Volatality of B  B 1. The liquid mixture is heated to create vapour. The vapours formed are condensed in condenser
xB and withdraw as a product. - No Reflux
Relative volatility of component A with respect to B is the ratio of the volatility of A (more volatile 2. The liquid mixture is heated to create vapour. The vapour formed are condensed in condenser
component) to that of B. It is also known as volatility of A with respect to B and is denoted by symbol αAB. part of the condensed liquid is returned to distillate system. - Reflux
*
PA xB Common methods used in distillation:
 AB  * 1. Differential or Simple distillation
PB x A

 P 
2. Flash or Equilibrium distillation
y x
 AB  A B A
*
 y A .P and PB  yB .P
*
3. Rectification or Fractionation
yB x A
1. Differential or Simple distillation
yA In this distillation technique, a known quantity of liquid mixture is charged into a jacketed kettle or still.
yB
 AB  The jacket is provided for heating the mass in the still with the help of a heating media such as steam. The
xA
xB charge is boiled slowly, vapours formed are withdrawn and fed to a condenser where they are liquefied and
Relative volatility is the ratio of the concentration ratio of A to B in one vapor phase to that in liquid collected in the receiver as a distillate. In early stage of distillation, vapours leaving the still are richest in the
phase and is a measure of separability. more volatile component and as the distillation proceeds the liquid in the still becomes lean with respect to
y x more volatile component. The composition of the less volatile component thereby increases and hence the
 AB  A B boiling point increases.
yB x A
The product (distillate) from such units can be collected in several receivers, called cuts to give products
y A (1  x A )
 AB   yB  (1  y A ) and xB  (1  xA ) of various purities over the length of distillation period. The distillation is continued till the boiling point of
(1  y A ) x A liquid reaches a predetermined value and the content of the still is finally removed as residual liquid containing
 AB (1  y A ) xA  y A (1  xA ) majority of less volatile component.
 AB x A Material balance-Binary mixtures:
yA 
1  ( AB  1) x A As the composition of vapour issuing from distillation and that of the liquid remaining in it changes
Dropping superscripts we get, during the course of operation, the mathematical approach should be differential.
Assumptions:
x
y 1. F = The Kmol of the liquid mixture (A+B) containing
1  (  1) x
2. xF = mole fraction of component A
y 3. D = Kmol of the distillate
(1  y )
Where,   4. W = Kmol of the residual liquid
x
(1  x) 5. yDavg and xw = mole fraction of A in distillate and bottom residual liquid
y(1  x) 6. L = Kmol of the liquid in still

x(1  y) 7. x = The mole fraction of A in liquid
From above equation, knowing α for a given binary system, x - y data (equilibrium data) can be
generated by taking x = 0, 0.1,….to 1 and evaluating the corresponding values of y (equilibrium vapour phase
composition).
For an ideal system, volatility is equal to the vapour pressure of the pure component. Therefore, the
relative volatility of two substances forming an ideal solution is the ratio of their vapour pressures.
p
Re lative volatalit y   AB    A
pB
The relative volatility of component A with respect to B is the ratio of the pure component vapor
pressure of A to that of B at the same temperature.
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Overall material balance at any time, Raoult's law, in other words, is nearly applicable to the substance present in very large concentrations.
L  ( L  dL)  dD ----------------- (1) This is the case for all substances except where association within the vapor or electrolytic dissociation
L  L  dL  dD within the liquid occurs. The distribution diagram (x vs. y*) for systems of this type appears much the same as
dL  dD ----------------- (2) that of Figure.
Individual material balance any time, Minimum-boiling mixtures-azeotropes
Lx  ( L  dL)(x  dx)  y.dD ----------------- (3) When the positive deviations from ideality are sufficiently large and the vapor pressures of the two
Lx  Lx  Ldx  xdL  dLdx  ydD components are not too far apart, the total-pressure curves at constant temperature may rise through a maximum
at some concentration, as in Figure. Such a mixture is said to form an azeotrope, or constant-boiling mixture.
dLdx being very small can be neglected,
0  Ldx  xdL  ydD ----------------- (4)
Substituting for dD from equation (2) into equation (4) becomes,
0  Ldx  xdL  ydL ----------------- (5)
Rearranging the above equation gives,
Ldx  ( y  x)dL
dL dx
 ---------------- (6)
L ( y  x)
Integrating the above equation between the limits,
When, L =F; x = xF
L = W; x = xw
F x
dL F dx
 L  x ( y  x)
W W

xF

ln L
F
W 
dx
 ( y  x)
xW
Negative Deviations from Ideality
x When the total pressure of a system at equilibrium is less than the ideal value, the system is said to
 F  F dx
ln     --------------- (7) deviate negatively from Raoult's law. Such a situation is shown in Figure at constant temperature.
 W  xW ( y  x) Note that in this case, as with positive deviations, where neither vapor association nor liquid dissociation
(y is in equilibrium with x i.e. y is the vapour phase composition in equilibrium with liquid phase occurs, the partial pressures of the constituents of the solution approach ideality as their concentrations
composition (x)). approach 100 percent. The constant-pressure diagram for such a case has the same general appearance as the
This above equation (7) is known as Rayleigh equation. diagrams shown in Figure.
It is used to determine F, W, xF or xw when three of these are known. RHS of Equation (7) i.e. integral
on the RHS side is evaluated graphically by plotting 1/(y-x) as an ordinate and x as the abscissa and
determining the area under the curve between x = x F and x = xw. The required data for above procedure are
taken from vapour-liquid equilibrium relationship.
If yD,avg. is a composition of composited distillate, then,
Material balance of component A is:
xF F  y D ,avg D  xW W --------------- (8)
Though the simple or differential distillation as a method of separation is not effective, many such units
are used, especially where (i) the components to be separated have widely different boiling points and (ii)
methods giving sharp separations are not necessary.
Positive Deviations from Ideality
A mixture whose total pressure is greater than that computed for ideality is said to show positive
deviations from Raoult's law. Most mixtures fall into this category. In these cases the partial pressures of each
component are larger than the ideal, as shown in Figure.
It should be noted that as the concentration for each component approaches unity mole fraction, the
partial pressures for that substance approach ideality tangentially.
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Maximum-boiling mixtures—azeotropes The point of intersection of operating line and diagonal (x = y) is,
When the difference in vapor pressures of the components is not too great and in addition the negative  (1  f ) x xF
x  i.e, (x = y)
deviations are large, the curve for total pressure against composition may pass through a minimum, as in f f
Figure.  (1  f ) x  xF
This condition gives rise to a maximum in the boiling temperatures, as at point L (Figure), and a x
f
condition of azeotropism. The equilibrium vapor is leaner in the more volatile substance for liquids whose x is
xf   x  xf  xF
less than the azeotropic composition and greater if x is larger.
Solutions on either side of the azeotrope, if boiled in an open vessel with escape of the vapor, will x  xF
ultimately leave a residual liquid of the azeotropic composition in the vessel. and y  xF
2. Flash or Equilibrium distillation For f =1, feed totally vaporized,
Flash distillation is normally carried out in continuous manner. In this method, a liquid mixture is  (1  f )
Slope  0
partially vaporised, vapour and liquid are allowed to attain equilibrium and finally withdrawn separately f
Feed is heated in a tubular heat exchanger. The hot liquid mixture is then fed to a separator via pressure and hence the operating line is parallel to ‗x‘ axis through the point (xF,xF) on diagonal.
reducing valve whereby pressure is reduced and vapour is formed at the expense of liquid adiabatically. The For f = 0, - no feed is vaporized.
liquid is withdrawn from bottom of the separator and the equilibrium vapour leaves the separator from top Slope = ∞ and the operating line will be parallel to y-axis through point (xF,xF) on diagonal.
which is then liquified in a condenser. Flash distillation is commonly used in petroleum industry, handling The operating line for various values of ‗f‘ on equilibrium diagram is as shown in figure.
multicomponent system in the pipe stills.
Material balance-Binary mixtures:
Consider 1mole of liquid mixture having xF mole fraction of more volatile component is fed to flash
distillation unit.
Assumptions:
1. Let ‗F‘ can be fraction of feed or vaporized and composition ‗y‘.
2. Let ‗x‘ will be mole fraction of more volatile component.
3. Let (1-f) will be mole of residual liquid obtained.

The following figure shows method of obtaining equilibrium compositions of vapour (y1) and liquid (x1)
for a given f.

Material balance for more volatile component,

xF  f . y  (1  f ) x ----------------- (1)
f . y  (1  f ) x  xF ----------------- (2)
 (1  f ) x xF
y  ----------------- (3)
f f
Equation (3) is a material balance/operating line for flash distillation
with slope equal to - (1- f)/f and intercept equal to xF/f.
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3. Continuous Rectification –Binary System (Fractionating column)
Rectification is commonly encountered in industrial practice as it is possible to get almost pure product
by this method. The enrichment of the vapour stream as it passes through the column in contact with reflux is
termed as rectification.
In this separation method, part of the condensed liquid is returned back as a reflux and maximum
enrichment of more volatile component in vapour is obtained by successive partial vaporisation and
condensation by multistage contact of vapour and liquid. This is achieved in a single unit called as fractionating
column.

Material balance-Binary mixtures:

Consider that the column is fed with F moles/time of liquid mixture (feed) with x F mole fraction of more
volatile component.
Assumptions:
1. D moles/time of composition xD are withdrawn as a distillate.
2. W moles/time of composition xW is withdrawn as a bottom product.
Overall material balance
Feed  Distillate  Bottom Product
F  D  W ----------------- (1)
Material balance of more volatile compound (A) over fractionator
A in Feed  A in Distillate  A in Bottom Product
FxF  DxD  WxW ---------------- (2)
Eliminating ‘W’ from equation (1),
Fractionating column consists of: W  F  D ---------------- (3)
i. Cylinder shell divided into sections by a series of perforated trays Substitute eqn. (3) in eqn. (2) we get,
ii. Reboiler FxF  DxD  ( F  D) xW
iii. Condenser
FxF  DxD  FxW  DxW
The liquid mixture to be separated in introduced in the cylindrical column. The column itself is dived
into 2 sections FxF  D( xD  xW )  FxW
a) Rectification section F ( xF  xW )  D( xD  xW )
b) Stripping section D ( xF  xW )
a) Rectification section  ---------------- (4)
F ( xD  xW )
1. The section above the feed plate is called as Rectifying section.
Eliminating ‘D’ from equation (1),
2. The vapour is washed to remove the less volatile compound with the liquid return to column
D  F  W --------------- (5)
from top (known as Reflux).
3. The Rectifying section is also called the Enriching section. Substitute eqn. (5) in eqn. (2) we get,
4. The feed is enriched in this section, owing to which the top product/distillate is richer in the FxF  ( F  W ) xD  WxW
more volatile component than the feed. FxF  FxD  Wx D  WxW
b) Stripping section FxF  FxD  W ( xW  xD )
1. The portion below the feed plate including feed plate is called the stripping section wherein
F ( xF  xD )  W ( xW  xD )
liquid is stripped off more volatile component by rising vapour.
2. Perforated trays are nothing but gas-liquid contacting devices on which gas/vapour and liquid W ( xF  xD )
 --------------- (6)
streams are brought into intimate contact for mass transfer to occur. F ( xW  xD )
 P a g e | 13 P a g e | 14
Let ‗L‘ be (mole/ time) of liquid returned to the top of column then, b. Stripping section (Including Reboiler):
L
Reflux ratio  R 
D
This reflux ratio is also known as external reflux ratio.
Let ‗V‘ is the (mole/ time) molal flow rate of vapour leaving the top of column then,
L
Reflux ratio  R 
V
This reflux ratio is also known as internal reflux ratio.
a. Rectification section:

Overall Material Balance Over figure (above)

Liquid flow to plate (m  1)  Vapour flow from plate (m  1)  Bottom product withdrawn
Lm  Vm1  W --------------- (12)
Similarly, material balance of more volatile component (A),
Lm xm  Vm1 ym1  WxW --------------- (13)
Rearranging the above equation,
Lm Wx
ym1  xm  W --------------- (14)
Vm1 Vm1
From equation (12),
Vm1  Lm  W
Therefore equation (14) becomes,
Lm WxW
ym1  xm  --------------- (15)
Lm  W Lm  W
Material balance around condenser
V  L  D --------------- (7) Equation (15) is known as the material balance line (or) operating line of the ‘Stripping section’.
L V D ANALYSIS OF FRACTIONATING COLUMN:
D V L The theoretical/ ideal stage/ plates required for given degree of separation can be obtained by:
Overall Material Balance Over figure (above) 1. McCabe - Thiele method
Vapour flow to plate (n)  Liquid flow from plate (n)  Distillate withdrawn 2. Lewis – Sorel method
3. Ponchon – Savarit method
Vn1  Ln  D --------------- (8)
1. McCabe - Thiele method
Similarly, material balance of more volatile component (A), It is a graphical procedure of obtaining theoretical plates.
Vn1 yn1  Ln xn  DxD --------------- (9) Assumptions:
Rearranging the above equation, i. Constant molal heat of vaporization.
L Dx ii. No heat losses.
yn1  n xn  D --------------- (10)
Vn1 Vn1 iii. No heat of mixing.
From equation (8), Consider any plate ‗n‘ in the rectifying section
Vn1  Ln  D
Therefore equation (10) becomes,
Ln DxD
yn1  xn  --------------- (11)
Ln  D Ln  D
Equation (11) is known as the material balance line (or) operating line of the ‘Rectifying section’.
 P a g e | 15 P a g e | 16
Thus the operating line of rectifying section to be drawn on equilibrium diagram through the point with
Heat Balance across plate ‗n‘ is the co-ordinates (xD, xD) on the 45o diagonal and with the slope of R/(R+1) and Intercept on y axis equal to
Ln1H Ln 1  Vn1HVn 1  Ln H Ln  Vn HVn  Heat Losses  Heat of mixture -------------- (1) xD / (R+1).
Heat losses are negligible for good insulation. The equation of the operating line of stripping section becomes:
L WxW
Heat of mixing is zero for ideal system. y x -------------- (5)
Then equation (1) becomes L  W L  W
Ln 1H Ln 1  Vn1HVn 1  Ln H Ln  Vn HVn  0  0 Here, point of intersection of operating line for stripping section and the 45o diagonal (x = y)
obtained as,
Ln1H Ln 1  Vn1HVn 1  Ln H Ln  Vn HVn -------------- (2)
L WxW
x x
Where, HL and HV - Enthalpies of liquid and vapour per mole. L  W L  W
If the molal heat of vaporization is constant than one mole of vapour Vn+1 on condensing, release Lx  Wx  Lx  WxW
sufficient heat to liberate one mole of vapour Vn. It follows that,
x  xW and y  xW
Vn  Vn 1
Thus the operating line of stripping section is to be drawn through the point having coordinates
H L n  H L n1 L
(xw, xw) on the diagonal and with the slope equal to
and HV n  HV n1 L  W
Substitute in equation (2) becomes, Stepwise procedure for obtaining theoretical plates by McCabe -Thiele method
Ln 1H Ln 1  Vn1HVn 1  Ln H Ln 1  Vn1HVn 1 1. By material balances, evaluate the terms D, W, L, etc.
2. Let xD , xF, and xw are the mole fraction of distillate ,feed and bottom product of the distillation column
Ln 1H Ln 1  Ln H Ln 1 3. To draw the distillation tower diagram and locate the mole fraction xD , xF, and xw
Ln1  Ln 4. Draw the equilibrium diagram with help of x – y data given in the problem. (or) If the relative volatility is
given, generate the x – y data.
So the moles of liquid reflux in this section are also constant. x
5. Generate the data using the following relation. (Assume the value of x from 0 to 1). y 
Ln and Vn+1 are constant is rectifying section. 1  x(  1)
Lm and Vm+1 are constant in the stripping section. 6. Draw the diagonal joining the points (0, 0) and (1, 1).
ie., The molal flow rate of vapour and liquid are constant is each section of column. 7. Locate xD , xF, and xw in the x-axis.
Ln  Ln1  L , Lm  Lm1  L 8. Draw a straight line from xD , xF, and xw to intercept the diagonal at this points a,b,c respectively.
9. Draw the feed line from the point ‗b‘ with the help of slope -q/(1-q), Where q- fraction of liquid in feed.
Vn  Vn1  V , Vm1  Vm  V  10. Let the point of intersection of feed line and equilibrium curve.
The above cited assumptions lead to a concept of constant molal vapour flow and constant molal liquid 11. Draw a straight line joining the point ‗a‘ and‗d‘.
flow in any section of the column. 12. The above line gives the intercept in the y-axis ;Let it be ‗emin ‗ xD
Intercept  emin 
In other words, for one mole of vapour condensed, one mole of liquid is vaporised. 13. Find RD min from the following relation. RD min  1
Thus Vn = Vn+1, Ln = Ln+1… etc., 14. Find RD act RD act = RD min x Multiplying factor, Where –Multiplying factor will be given in the
The subscripts n, n+1, m, m+1...etc., may be dropped and the operating lines then plotted on problem.
equilibrium diagram are straight. 15. Find the value of ‗eactual‗ from RD actual using the following. xD
Intercept  eact 
The operating line of the rectifying section becomes: 16. Locate the intercept value ‗eactual‗ in the y-axis. RDact  1

y
L
x
DxD 17. Join the points ‗eactual‗ and ―a‖ with a straight line.
-------------- (3)
LD LD 18. The above line is operating line of the rectifying section. This R oL Intercept the feed line at point F.
As R  L D , above equation becomes, 19. Joint the points ―F‖ and ―c‖. The Fc is he operating line of the stripping section.
20. The line aF and Fc serves as the operating line of the entire column of distillation.
R x
y x  D -------------- (4) 21. Draw stepwise construction between the operating line of the column and equilibrium line starting from
R 1 R 1 point ―a‖ and ending at point The number of theoretical plates in the column:
Here, point of intersection of operating line for rectifying section and 45o diagonal (x = y) obtained When Reboiler is used
as,
No % of plates= plates from graph -1
R x
x x D When Partial condenser is used
R 1 R 1
No % of plates= plates from graph -2
( R  1) x  Rx  xD
14. Actual plate = Theoretical plates/ % of efficiency.
x  xD and y  xD
 P a g e | 17 P a g e | 18
To calculate the change in phase flow rate by introduction of feed, factor ‘q‘ is introduced.
It (q) is a measure of thermal condition of feed and is defined as the number of moles of saturated liquid
resulting in the stripping section for each of feed is introduced.
For feed F, we get,
L  L  qF --------------- (1)
V  V   (1  q) F --------------- (2)
The values of ―q‖ for various thermal condition of feed are:
a) Cold Liquid : q>1
b) Liquid at its Bubble point : q =1
(Saturated liquid)
c) Partially Vaporized: (0<q<1)
Limitation of McCabe -Thiele method (Partially vapour/Partially liquid)
1. It is not used when relative volatility is less than 1.3 or greater than 5 (1.3<α>5). d) vapour at its Dew point : q=0
2. It is not used when more than 25 theoretical stages/plates are required. (Saturated vapour)
3. It is not used when the operating reflux ratio is less than 1.1 times the minimum reflux ratio. e) Super-heated vapour :q<0
Feed plate and Feed line The q value for any particular feed condition can be calculated from:
The plate on which feed is introduced is called feed plate. The feed to the column may be introduced as Energy to convert 1 mole of feed to saturated vapour
q
a) Cold liquid Molal latent heat of vaporization
b) Liquid at its bubble point (Saturated liquid) Liquid flow in stripping section is from equation (1),
c) Partially vaporized (Partially vapour/Partially liquid) L  L  qF --------------- (1)
d) Saturated vapour at its dew point
L  L  qF --------------- (3)
e) Super-heated vapour
Similarly vapour flow in rectifying section from equation (2),
The condition of feed introduced on the feed plate alters the phase flow rates.
a) Feed as a cold liquid and liquid at its bubble point- increases the liquid flow rate in the stripping V  V   (1  q) F --------------- (2)
section. V  V   (1  q) F --------------- (4)
b) Feed - partially vaporised increases the vapour flow rate in the rectifying section and also the Overall material balance for Upper section,
liquid flow rate in the stripping section. V  L  D --------------- (5)
c) Feed as a saturated vapour and a superheated vapour increases vapour flow rate in the rectifying Material balance of mole fraction component A,
section. Vy  Lx  DxD --------------- (6)
Phase flaw rates into and out of the feed plate for various feed conditions are shown diagrammatically in Overall material balance for Lower section,
following figures. V   L  W --------------- (7)
Material balance of mole fraction of component A,
V y  Lx  WxW --------------- (8)
Subtracting equation (8) from equation (6),
Vy  V y  Lx  Lx  DxD  WxW
(V  V ) y  ( L  L) x  DxD  WxW --------------- (9)
W.K.T,
FxF  DxD  WxW --------------- (10)
The equation (9) becomes,
(V  V ) y  ( L  L) x  FxF --------------- (11)
Substitute the equation (3) and (4) in equation (11),
y(1  q) F  x(qF )  FxF
y(1  q) F  F ( xq  xF ) --------------- (12)
q x
Figure: Feed through the feed plate for various feed conditions y x  F --------------- (13)
(1  q) (1  q)
 P a g e | 19 P a g e | 20
The equation (13) is known as feed line or q-line point of intersection of feed line and diagonal (y=x) is, Referring above Figure, we have:
q x 1. Theoretical plates including reboiler = n = 6.
yx x F
(1  q) (1  q) 2. Theoretical plates in column = n - 1 = 6 - 1 = 5.
x(1  q)   xq  xF 3. Feed plate = Third from top.
2. Ponchon - Savarit method
 ( x  xq)   xq  xF
There are three methods by which the design of the continuous fractionator can be established. Let us
 x  xF second consider Ponchon-Savarit method where it requires both enthalpy and concentration data.
 y  xF Envelope I: Condenser section
The feed line thus passes the point N (xF,xF) on the 45o diagonal and slope -q/(1-q) and intercept xF /(1-q) Envelope II: Full distillation unit
 For q = 1, slope = ∞ and hence the feed line is parallel to y-axis through the point N (xF, xF) on the Envelope III: Enriching/Rectifying section
diagonal on the equilibrium diagram Envelope IV: Stripping/Exhausting section
 For q = 0, slope = 0 and hence the feed line is parallel to the x-axis through the point N (xF,xF) on The numbering of plates or trays is accounted from the top to bottom. Suffix denotes the properties of
the diagonal. streams leaving a particular plate or tray. Let n and m, denote general plates in the enriching section and
Typical feed line or q-line constructions for the various values of 'q' are shown in following figure. stripping section respectively.

Plotting the feed line and operating lines to determine the number of stages:
1. Draw the feed line on the equilibrium diagram.
2. Draw the operating line of the rectifying section as usual; it will cut the feed line at certain point.
3. The operating line of the stripping section can be easily plotted.
This line is to be plotted through the point M (xW, xW) on the diagonal and it will pass through the point
of intersection of the feed line and the operating line of the rectifying section. When molar latent heat is not constant and there is a substantial heat of mixing, then for establishing the
The point of intersection of lines - 1, - 2 and 3 falls in a triangle which represents a feed plate. The relationship between number of plates, product composition and liquid/vapour ratio, we have to adopt the
triangle representing the feed plate has one corner on the operating line of the rectifying section and one on the method developed by Ponchon and Savarit.
operating line of the stripping section. Feed should be introduced at any point between A and B but at the same Determination of the number of plates by this method is applicable for both constant and varying molar
time we have to keep in mind the maximum enrichment and minimum number of plates. overflow situations. The Ponchon-Savarit method is based on the use of an enthalpy-composition diagram and
Introduction of the feed near A or B unnecessarily results into a large number of plates in the rectifying it therefore requires detailed enthalpy data.
or stripping section. The optimum location will be the one at which the liquid phase composition value crosses The enthalpy-composition diagram consists of the dew-point curve (H v/s y), the bubble-point curve (H
the feed composition value xF. v/s x) and the tie lines joining these curves.
A continuous distillation unit to which F moles of feed of composition x F is fed continuously and from
which D moles of distillate of composition xD and W moles of bottom product xW are continuously withdrawn
on per unit time basis is shown in above figure.
Stepwise Procedure for Determination of Number of ideal plates using Ponchon-Savarit Method
1. Plot the Hxy diagram and the xy diagram as shown in Fig. 1.42.
2. Locate the point F on the Hxy diagram. Coordinates of F are (xF, HF). F represents the condition of a feed.
In Fig. 1.42, F is located on the saturated liquid curve which indicates that the feed is a saturated liquid.
3. Locate abscissas x = xD and x = xW, by drawing verticals, through them, representing the top and bottom
compositions.
 P a g e | 21 P a g e | 22
4. Locate ΔD vertically on vertical line through x = xD, i.e. locate ΔD on the ordinate at x = xD. The
coordinates of ΔD are (xD, Q'). Locate ΔD at H = Q' on the ordinate at x = xD.
5. We know that ΔD, F and ΔW lie on the same straight line. Join ΔD - F and extend this line to intersect the
vertical line x = xW in the desired point ΔW. Locate ΔW at which the extension of line ΔD F cuts the
ordinate at x = xW.
6. Locate V1 on the saturated vapour curve at which the ordinate through x = x D (i.e. vertical line x = xD)
intersects the curve, i.e., locate V1 at the intersection of the vertical line x = x D with the saturated vapour
curve. V1 represents the condition of vapour leaving the top plate and has coordinates (y1, HV1).
7. Now, we have to make use of the xy diagram, i.e., the equilibrium curve to draw tie lines LIVI, L2V2, etc.
8. We have to locate L1 (x1, HL1) on the saturated liquid curve. Through x = xD on the Hxy diagram, drop a
vertical to cut the diagonal (y = x) on the xy diagram at point A. Through A, proceed horizontally to get
point B on the equilibrium curve and then through B, draw a vertical on the Hxy diagram to cut the
saturated liquid curve at L1. Join V1 L1 which is a tie line representing an equilibrium stage (1). Similar
procedure is to be adopted for getting L2, L3 ... and drawing tie lines V2L2, V3L3 .... (L1 represents the
condition of liquid on top plate).
9. L1, V2 and ΔD will lie on the same straight line. So join (ΔD - L1) and mark V2 (y2, HV2) at which line (ΔD-
L1) intersects the saturated vapour curve. (V2 represents the condition of vapour on the second plate). The
same procedure is adopted for locating V3, V4 ... on the saturated vapour curve (as Ln, Vn+1 and ΔD lie on
the same straight line).
10. Through V2, drop a vertical on the xy diagram to cut the diagonal, from there move horizontally to the
equilibrium curve and from that point on the equilibrium curve, draw a vertical to cut the saturated liquid
curve at L2. Join (L2 - V2) which is a tie line representing the second ideal plate in the column from the
top.
11. L2, V3 and ΔD will lie on the same straight line. Join (L2- ΔD) to cut tin vapour curve at V3.
12. Repeat the above mentioned procedure for further construction of the number of theoretical plates till the
feed plate is reached. Use ΔD for construction till the feed plate is reached. The tie line which crosses the
line ΔD – F – ΔW represents a feed plate.
13. Make use of ΔW for the further construction work when any such tie line constructed crosses the line
joining ΔD – F – ΔW.
14. Suppose as an example (not true in Fig. 1.42) a tie line (V7 – L7) crosses the line through points ΔW, F and
ΔD, the plate 7th from the top is the feed plate Afterwards join ΔW to L7 and extend it to cut the saturated
vapour curve at V8 (ΔW,V8 and L7 lie on the same straight line). In Fig 1.43 a tie line V3L3 crosses the
line through points ΔD, F and ΔW, so the plate 3rd from the top is the feed plate. Afterwards L3 is joined to
ΔW and ΔW L3 is extended to meet the saturated vapour curve at V4.
15. For the stripping section, adopt the same procedure of construction of the equilibrium stages (tie lines) as
is given for the rectifying section and continue the construction work using ΔW till ΔW (xW, Qn) is exactly
reached or covered. Count the number of tie lines. The number of tie lines counted from x D to xW
represent the number of ideal plates including reboiler (i.e., n+1), so the number of ideal plates required in
the column will be n.
 P a g e | 23 P a g e | 24
PROBLEMS From graph,
i. A mixture containing ethanol and water contains 32% (mole %) of alcohol is to be separated in a 1. Number of theoretical stages including reboiler, n = 9
fractionating column using indirect stream as the source of heat. The fractionation is carried out at 1atm 2. Feed plate = 6
pressure to obtained to give product containing 97% alcohol is overhead product and bottom product 3. Number of theoretical stages required, (n-1) = (9-1) = 8
containing 1.5% . Calculate the minimum reflux ratio. Find out the number of theoretical stages required if ii. A Continuous fractionating column is to designed to separate 30000kg/hr of a mixture of 40% benzene and
reflux ratio of 1.78 times the minimum is used. Feed is a saturated liquid. VLE for the system. 60% of toluene into an overhead product containing 97% benzene and bottom product contains 98%toluene are
by weight. A reflux ratio (RD) of 3.5 moles to 1 mole of products to be used. Benzene and toluene from ideal
x 0 0.02 0.04 0.06 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
system with a relatively volatility of about 2.5, the feed has a boiling point of 95oC at a pressure of 1atm.If the
y 0 0.13 0.23 0.30 0.41 0.57 0.66 0.72 0.77 0.82 0.87 0.91 0.95 1 feed is a mixer of 2/3 vapor and 1/3 liquid
a) Calculate the moles of overhead product and bottom product per hour.
Data Given: b) Determine the no/. of ideal plates and the position of the feed plates.
xF, = 32mole% = 0.32 i. If the feed is liquid and its boiling point.
xD = 97mole% = 0.97 ii. If the feed is liquid mixture of 2/3 vapor and 1/3 liquid.
xw = 1.5mole% = 0.015 Data Given:
Pressure = 1atm F = 30000kg/hr=30000/86.4=347.222Kmole/hr
RD act = RD min x 1.78 Benzene in feed = 40%=0.40
q =1 (saturated liquid) Toluene in feed = 60%=0.60
Minimum reflux ratio, RDmin = ? Distillate = 97% benzene
Number of theoretical stages = ? Bottom Product = 98%toluene
Solution: Reflux ratio (RD) = 3.5 moles to 1 mole
Feed is a saturated liquid: q = 1 Relatively volatility, α = 2.5
q Boiling point, Tb = 95oC
Slope of feed line 
(1  q) Pressure = 1atm
1 Feed is liquid and its boiling point
Slope  
(1  1) Feed is a mixer of 2/3 vapor and 1/3 liquid
Plot a graph between x & y Moles of overhead product and bottom product per hour = ?
From graph, Number of ideal plates and the position of the feed plates = ?
Interceptmin = emin = 0.55 Solution:
xD Mol. weight of Benzene, (C6H6) = 78
Intercept min  emin 
RD min  1 Mol. weight of Toluene, (C6H5 CH3) = 92
Average molecular weight of Feed = (0.4 x 78) + (0.6 x 92) = 86.4 Kg/Kmol
0.97
0.55  Average molecular weight of Residual = (0.98x 92) + (0.02 x 78) = 91.72 Kg/Kmol
RD min  1
Average molecular weight of Distillate = (0.97 x 78) + (0.03 x 92) = 78.42 Kg/Kmol
0.97
RD min  1 
0.55 40 78
RD min  0.7636 xF 
40 78  60 92  0.4398
RDact  RD min 1.78
RDact  0.7636 1.78
2 
78

RDact  1.3592
xW 
 78  98 92  0.0234
2

Intercept act  eact 

xD 97 
78
RDact  1
xD 
 78  392  0.9741
97
0.97
eact  a) Moles of overhead product and bottom product per hour,
1.3592  1 F x D  xW
eact  0.4111 
D xF  xW
 P a g e | 25 P a g e | 26
F 0.9741  0.0234 From graph,

D 0.4398  0.0234 1. Number of theoretical stages including condenser, n = 10
347.222 0.9741  0.0234 2. Feed plate = 5

D 0.4398  0.0234 3. Number of theoretical stages required, (n-1) = (10-1) = 9
D  152.156 Kmole / hr b) ii. The feed is liquid mixture of 2/3 vapor and 1/3 liquid,
Material balance, 1
Substitute, q 
F  D W 3
W  F D q
Slope of feed line 
W  347.222  152.156 1  q 
W  195.064 Kmole / hr 1
3  0.4995
b) i. The feed is liquid and its boiling point,
Feed is a saturated liquid, q = 1
Slope 

1 1
3

q Plot a graph between x & y
Slope of feed line 
(1  q) From graph,
1 Interceptmin = emin = 0.31
Slope   xD
(1  1) Intercept min  emin 
RD min  1
Equilibrium Relation,
x 0.974
y 0.31 
1  x(  1) RD min  1
Relatively volatility, α = 2.5 0.974
RD min  1 
2.5x 2.5 x 0.31
y 
1  x(2.5  1) 1  1.5 x RD min  2.142
RDact  RD min  3.5
x 0 0.2 0.4 0.6 0.8 1.0
y 0 0.384 0.625 0.789 0.909 1.0 RDact  2.142  3.5
RDact  7.497
Plot a graph between x & y
From graph, xD
Intercept act  eact 
Interceptmin = emin = 0.41 RDact  1
xD 0.974
Intercept min  emin  eact 
RD min  1 7.497  1
0.974 eact  0.1146
0.41 
RD min  1 From graph,
0.974 1. Number of theoretical stages including reboiler, n = 10
RD min  1 
0.41 2. Feed plate = 6
RD min  1.376 3. Number of theoretical stages required, (n-1) = (10-1) = 9
iii. 1000Kmol /hr of ethanol – Propanol mixture containing 65mole % ethanol is to be separated in a
RDact  RD min  3.5
continuous plate column operating at 1atm pressure. The desired terminal composition for ethanol are xD =
RDact  1.376  3.5 0.92 and xw = 0.07 .The feed is a saturated vapour and a total condenser is used. When the reflux ratio is four
RDact  4.815 times the amount of top product , find the number of theoretical plates required for the separation .Data given
xD relative volatility = 2.10.
Intercept act  eact 
RDact  1
Data Given:
0.974
eact  xF, = 65mole% = 0.65
4.815  1
xD = 0.92
eact  0.1675 xw = 0.07
 P a g e | 27 P a g e | 28
RD act = RD min x 4 iv. A benzene – toluene solution containing 55 % benzene is to be fractionated continuously in a distillation
q = 0 (saturated vapour) column to get atop product of 85% and bottom product of 10% benzene. The feed is at its bubbles point. The
Relatively volatility, α = 2.10 relative volatility is 2.5. Find
Number of theoretical stages = ? i. The no/ of plates required for a reflux ratio is 2.5.
Solution: ii. Minimum no of plates.
Feed is a saturated vapour, q = 0 Data Given:
q xF, = 55% = 0.55
Slope of feed line 
(1  q) xD = 85% = 0.85
0 xw = 10% = 0.10
Slope  0 RD act = RD min x 2.5
(0  0)
q = 1 (saturated liquid)
Equilibrium Relation,
Relatively volatility, α = 2.5
x
y Number of theoretical stages = ?
1  x(  1)
Solution:
Relatively volatility, α = 2.10 Feed is a saturated liquid, q = 1
2.10 x 2.10 x q
y  Slope of feed line 
1  x(2.10  1) 1  1.10 x (1  q)
1
x 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 Slope  
(1  1)
y 0 0.189 0.344 0.474 0.583 0.677 0.759 0.831 0.894 0.949 1.0 Equilibrium Relation,
x
Plot a graph between x & y y
1  x(  1)
From graph,
Relatively volatility, α = 2.10
Interceptmin = emin = 0.35
2.5x 2.5 x
xD y 
Intercept min  emin  1  x(2.5  1) 1  1.5 x
RD min  1
0.92
0.35  x 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
RD min  1
0.92 y 0.217 0.385 0.517 0.625 0.714 0.789 0.854 0.909 0.957 1.0
RD min  1 
0.35
Plot a graph between x & y
RD min  1.6286 From graph,
RDact  RD min  4 Interceptmin = emin = 0.57
RDact  1.6286  4 Intercept min  emin 
xD
RD min  1
RDact  6.5143
0.85
xD 0.57 
Intercept act  eact  RD min  1
RDact  1
0.85
0.92 RD min  1 
eact  0.57
6.5143  1
RD min  0.4912
eact  0.1224
RDact  RD min  2.5
From graph,
1. Total number of theoretical stages, n = 9 RDact  0.4912  2.5
2. Feed plate = 4 RDact  1.2281
3. Number of theoretical stages required, (n-1) = (9-1) = 8
 P a g e | 29 P a g e | 30
xD W  157.64  63.056
Intercept act  eact 
RDact  1 W  94.584 kmole / hr
0.85
eact  Plot a graph between x & y
1.2281  1
From graph,
eact  0.3815
Interceptmin = emin = 0.32
From graph,
xD
1. Total number of theoretical stages with reboiler, n = 7 Intercept min  emin 
RD min  1
2. Feed plate = 3
0.97
3. Number of theoretical stages required, (n-1) = (7-1) = 6 0.32 
v. A continuous fractionating column is to be designed to separate 13,620 Kg/hr of mixture of 40% benzene, RD min  1
60% toluene in to an overhead product contains 97% benzene and bottom products containing 98% toluene 0.97
RD min  1 
are by weight. Reflux ratio of 3.5:1 of product is to be used. The molar latent heat of benzene, toluene are 0.32
7360 and 7960 cal/ mole. Calculate moles of overhead product and bottom product. Determine the number of RD min  2.0313
ideal theoretical plates and position of the Feed plate if Feed is liquid at its boiling point. Feed at 1.36 atm RDact  RD min  3.5
gauge is used for heating, how much steam is required / hr. for each of the above cases. λ = 522 Kcal / Kg.
Cooling water enters the condenser at 26.7oC and leaves at 65.5oC. How Much cooling water is required?
RDact  2.0313  3.5
Mole fraction of benzene in liquid 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 RDact  7.1094
Mole fraction of benzene in vapour 0.0 0.2 0.38 0.51 0.63 0.71 0.78 0.85 0.91 0.96 1.0 xD
Data Given: Intercept act  eact 
RDact  1
F = 13620 Kg /hr
0.97
xF, = 40% = 0.40 (benzene) eact 
7.1094  1
xD = 97% = 0.97 (benzene)
xw = 2% = 0.02 (benzene) eact  0.1196
RD act = 3.5:1 From graph,
q = 1 (Feed and its boiling point) Total number of theoretical stages with reboiler, n = 11
Number of theoretical stages = ? 1. Feed plate = 5
Solution: 2. Number of theoretical stages required, (n-1) = (11-1) = 10
Average molecular weight of feed = (0.4 x 78) + (0.6 x 92) = 86.4 vi. It is desired to distill a plate column for separating a equimolal feed mixture of A and B to get a product of
Molal flow rate of feed, F = 13620/86.4=157.64 kmole/hr 95% A and 5%A in the distillate and residue respectively. The reflux enters the column at its bubble point and
Material balance equations: a reflux ratio of 1.5 times the minimum is to be used. Estimate the number of plates needed if the plate
F  D W efficiency is 80%.
FxF  DxD  WxW XA 0 0.16 0.31 0.49 0.66 1.0
Where F = feed; D = distillate; W = residue YA 0 0.28 0.49 0.67 0.81 1.0
Substituting for the known quantities, Data Given:
157.64  0.4  0.97 D  0.02W xF, = 50% = 0.5 (Equimolal feed)
xD = 95% = 0.95
63.056  0.97D  0.02( F  D)
xw = 5% = 0.05
63.056  0.97 D  0.02 F  0.02 D
RD act = 1.5 RDmin
63.056  0.95D  0.02(157.64)
q = 1 (Feed and its bubble point)
63.056  3.153  0.95 D Number of theoretical stages = ?
59.903  0.95 D Solution:
59.903
D  63.056kmole / hr Plot a graph between x & y
0.95 From graph,
Substituting for the known quantities, Interceptmin = emin = 0.35
F  D W xD
Intercept min  emin 
W  F D RD min  1
 P a g e | 31 P a g e | 32
0.95 At (n = 1) in equation (6),
0.35 
RD min  1 x1
  AB
x2  -------------------- (7)
0.95 1  x1 (1  x2 )
RD min  1 
0.35 At (n = 2) in equation (6),
RD min  1.7143 x2  x3 
  AB -------------------- (8)
RDact  RD min 1.5 1  x2 (1  x3 )
Let, n = (n-1) in equation (6),
RDact  1.7143 1.5
x n 1 xn
RDact  2.5714   AB -------------------- (9)
1  ( x n 1 ) 1  xn
xD
Intercept act  eact  At, n = 0 in equation (5),
RDact  1 y1 x1 
  AB -------------------- (10)
eact 
0.95 1  y1 (1  x1 )
2.5714  1 Let, y1 = xD (Total condenser, Total reflux)
eact  0.2660 xD x1  -------------------- (11)
From graph,   AB
1  xD (1  x1 )
1. Total number of theoretical stages with reboiler, n = 14
Multiplying the equation (7), (8), (9), and (11) we get,
2. Feed plate = 5
3. Number of theoretical stages required, (n-1) = (14-1) = 13  xD  x1   x2    x   x1   x2   x3    xn 
   ........... n 1    n AB    ..... 
FENSKE EQUATION  1  xD  (1  x1 )  (1  x2 )   1  xn 1   (1  x1 )  (1  x2 )  (1  x3 )   1  xn 
This equation can be used to theoretically calculate the minimum no/. of trays ,if the relative volatility
xD  x 
remains constant.   n AB  n 
1 xD  1  xn 
y /1  y A 
 A ------------------- (1)
x A / 1  x A  Let n = Nmin+1 and xn = xD we get,
xD  x 
yA x   N min 1 AB  W 
  A ---------------------- (2) 1  xD
1  yA 1  xA  1  xW 
Operating line equation for rectifying section in terms of (n+1),  xD 
 
L Dx D  1  xD 
y n 1  n x n  ------------------ (3)  N min 1 AB  -------------------- (12)
Vn 1 Vn 1  xW 
 
At total reflux ratio,  1  xW 
L L Taking log on both sides on above equation (12) we get,
D = 0, RD = 1; RD   1
D V  xD 
 
From equation (3), we get
 1  xD 
L ( N min  1) ln  AB  ln -------------------- (13)
y n 1  n x n  xW 
Vn 1  
 1  xW 
y n 1  x n -------------------- (4)
 xD 
 
1  xD 
From equation (2), for (n+1) tray,

y n 1 xn1  ln
  AB -------------------- (5)  xW 
1  y n 1 (1  x n 1 )  
 1  xW 
Sub equation (4) in (5), N min  1  -------------------- (14)
ln  AB
xn xn1 
  AB -------------------- (6)
1  xn (1  x n 1 ) 1  xD  (1  xD ) 
Rmin     -------------------- (15)
  1  x f (1  x f ) 
The above equation (14) is known as Fenske Equation.
 P a g e | 33 P a g e | 34
HEATING AND COOLING REQUIREMENTS Types of plate efficiency
When the saturated steam is used as the heating medium, Steam requirements given by this formula, i. Overall efficiency/overall plate efficiency - pertains to the entire column.
v ii. Murphree efficiency - pertains to any single plate.
ms 
s iii. Murphree local/point efficiency - pertains to a specific location on a given plate.
Where, i. Overall efficiency/overall plate efficiency:
ms – Steam consumption Overall efficiency is the ratio of number of ideal plates required to produce a given degree separation to
v – Vapour rate from the reboiler the number of actual plates required to effect the same separation.
 s – Latent heat of steam Theoritica l ideal plates required
o  100
 – Molal latent heat of mixture Actual plates required
If the water is used as the cooling medium in the condenser and the condensate is not sub cooled, the For example, if we need six theoretical plates to effect the desired separation and the overall efficiency
cooling water requirement. is 60% then the number of actual plates required are 6/0.60 = 10. The overall efficiency may vary from 30 to
v 100 percent.
mw 
T2  T1 ii. The Murphree plate efficiency:
It is the efficiency of any single plate based on vapour phase composition. For the n th plate in the
Where,
column, the Murphree efficiency is given by,
mw – Water consumption
(T2-T1) – Temperature rise of the cooling water y y
 M  n* n 1
Note: The feed is a mixer of vapour and liquid. y n  y n 1
Then q = (1-F), where f – fraction of original steam vapour. Where,
If the feed is cold yn – The average composition of vapour leaving plate.
1  C pL (Tb  T f ) yn+1 – The average composition of vapour entering plate.
q yn* – The composition of vapour in equilibrium with liquid leaving plate.

Where, It applies to an individual plate in a column and is defined as the actual change in average vapour
 – Latent heat of vaporization composition achieved by a given plate divided by the change in average vapour composition if the vapour
CpL – Specific heat of liquid leaving the plate were in equilibrium with the liquid leaving the plate.
Tf – Temperature of feed This efficiency is less convenient to use as it involves plate to plate compositions rather than the
Tb – Bubble point of feed terminal compositions.
For superheated vapor, q is given by iii. Point/Local efficiency:
It pertains to a particular place on the plate surface (applies to single location on a given plate). It is
 C pv (T f  Td )
q defined by,

y y
Where,    n*, local n 1, local
Cpv – Specific heat of vapor yn , local  yn 1, local
Tf – Dew point of feed Where,
PLATE EFFICIENCY yn,local – The composition of vapour leaving specific location on plate n.
By using either the McCabe-Thiele method or the Ponchon-Savarit method, we obtain the number of Yn+1,local – The composition of vapour entering plate n at the same location.
ideal/theoretical/equilibrium stages required for achieving the desired degree of separation. In case of an ideal ylocal* – The composition of vapour in equilibrium with the liquid at the same location (i.e. in
stage, the vapour leaving the plate is in equilibrium with the liquid which leaves it. equilibrium with xlocal).
In actual practice, complete equilibrium is never reached on any plate. This is due to short contact time To obtain satisfactory plate efficiencies, it is highly necessary that the plates must operate properly.
and incomplete mixing on any plate. The vapour leaving an actual plate is usually weaker in more volatile Adequate and intimate contact between vapour and liquid is essential. Each of the unfavourable phenomena
component than vapour in equilibrium with the liquid leaving it. Thus, for achieving desired degree of such as entrainment, excessive foaming, weeping, short-circuiting and flooding lower the plate efficiency.
separation in actual practice, we require more number of plates than ideal plates. To apply either of the methods
to an actual case, it is necessary to convert the number of ideal plates to actual plates. TYPES OF DISTILLATION COLUMNS
The factor that is used for converting ideal plates into actual plate is the plate efficiency. The reboiler Based on the nature of operation, distillation columns have been classified as batch and continuous
delivers vapour directly from the boiling liquid and is thus considered as a perfect plate. columns as shown in following figure.
 P a g e | 35 P a g e | 36
When the sum of the vapour pressures is equal to the total pressure, the mixture boils. With vapour
pressure data of the individual components, one can also estimate the temperature at which such distillations
take place.
PT = PA + PB
This type of distillation takes place at a temperature which will be even less than that of the boiling
point water. This method suffers from poor efficiency in its operation, as large quantity of water has to be
evaporated. However, one can introduce the effectiveness in such operations by
 Operating at different total pressures in which case the ratio of vapour pressure of the substances
may be more favourable.
 Sparging the mixture with superheated steam or other insoluble gas.

1. BATCH COLUMNS
In batch columns, the feed to the column is introduced batch wise and the distillation is carried. When
the desired quality is reached or when the desired quantity is distilled out, the operation is stopped and next
batch of feed is introduced.
i. Steam distillation
Steam distillation is a special type of distillation (a separation process) for temperature
sensitive materials like natural aromatic compounds. Applications:
Separation by normal distillation, steam is introduced into the distillation apparatus. The Liquid mixture 1. Steam distillation is employed in the manufacture of essential oils, for use in perfumes.
(substances) to be distilled are very sensitive to heat, steam distillation can also be combined with vacuum 2. Eucalyptus oil and orange oil are obtained by this method on the industrial scale.
distillation. After distillation the vapors are condensed as usual. 3. Steam distillation is also sometimes used to separate intermediate or final products during the
Some systems have very high boiling points and some of these substances are unstable at high synthesis of complex organic compounds.
temperatures. Especially when such systems are completely insoluble with each other, steam distillation can be 4. Steam distillation is widely used in petroleum refineries.
a useful method of separating such mixtures. 5. Steam distillation is also used in petrochemical plants.
Working Procedure: ii. Simple Distillation
When a mixture of two practically immiscible liquids are heated while being agitated to expose the i. Simple Distillation is a chemical process where two or more liquids with different boiling points
surfaces of both the liquids to the vapor phase, each constituent independently exerts its own vapor pressure as can be separated from each other.
a function of temperature .Consequently, the vapor pressure of the whole system increases. Boiling begins ii. The liquids are heated until one of them boils and evaporates (turns to a gas).
when the sum of the partial pressures of the two immiscible liquids just exceeds the atmospheric pressure. iii. The vapor is then fed into a condenser, which cools the vapour and condenses it back to a liquid.
iv. What remains in the original container is called the residue.
v. A fractionating column can be used to improve the separation.
vi. Distillation can be used for making dirty water cleaner.
vii. Fractional distillation can be used to purify crude oil so that it can become useful and can be used
for various things.
viii. The vaporized and condensed component is called distillate and the other component as the
residue.
ix. This has been used for a long time, to distill alcohol, pond water, and certain brands of coffee, and
produce distilled beverages.
x. Distillation is a commonly used operation in oil industry, where it is used to separate various fuels
For example, consider a mixture of hydrocarbon and water which are immiscible. The vapour pressure and raw materials from crude oil.
of either component cannot be influenced by the presence of the other component and each exerts its own
vapour pressure at the prevailing temperature.
 P a g e | 37 P a g e | 38
Working Procedure:
i. The feed is pumped through a heater at a certain pressure.
ii. The temperature of the liquid is raised in the heating chamber but the liquid does not boil under
high pressure (because boiling point increases).
iii. When the liquid enters into the vapor-liquid separator, due to drop in pressure, the liquid reaches
the boiling point under that reduced pressure and the liquid suddenly boils.
iv. The vapor flashes out from the hot liquid.
v. Since the vapor takes the latent heat, the liquid gets cooled down.
vi. The less volatile component of the vapor is condensed and the more volatile component remains in
the vapor phase.
vii. The mixture is allowed for sufficient time so that vapor and liquid come to equilibrium.
viii. The vapor is separated through an outlet provided at the top and the liquid is collected at the
Applications: bottom.
Simple distillation can be applied in four groups: Applications:
i. Laboratory scale, and It is used through all the common processes of petroleum refining such as:
ii. Industrial distillation, i. Crude Oil Distillation.
iii. Distillation of herbs for perfumery and medicinal (herbal distillate), ii. Hydrotreating, Reforming, Isomerization.
iv. Food processing. iii. Alkylation, Steam Cracking.
ii. Flash Distillation iv. Fluid Catalytic Cracking.
Principle: v. Coking.
i. When a hot mixture is allowed to enter from a high-pressure zone into a low pressure zone, the entire vi. Acid gas treatment.
liquid mixture is suddenly vaporized. This process is known as flash vaporization. 2. CONTINUOUS COLUMNS
ii. During this process, the chamber is cooled. These columns have a continuous feed stream and are capable of handling high throughputs. These are
iii. The less volatile fraction is condensed and the more volatile component remains in the vapor phase. further classified on the basis of,
iv. This process requires time, hence liquid and vapor are kept in intimate contact until equilibrium is a. The nature of the feed they are further processing
achieved. i. Binary columns—Feed has only two components
v. Flash distillation is also called equilibrium distillation because separation of two liquids takes place ii. Multicomponent column—Feed has more than two components
when liquid and vapor phases are at equilibrium. b. The number of product streams they have
Construction: i. Two product streams
i. It consists of a pump, which is connected to a feed reservoir. ii. Multi product streams
ii. Pumps help in pumping the feed into the heating chamber. c. The use of additional components in distillation
iii. The heating chamber is heat supplied by steam. i. Azeotropic distillation—use of entrainer
iv. The other end of the pipe is directly introduced into the vapor-liquid separator through a reducing ii. Extractive distillation—use of solvent
valve. d. The type of columns
v. The vapor outlet is provided at the top of the separator and liquid outlet is provided at the bottom. i. Tray columns—use of sieve plate columns/Bubble cap trays/valve trays for better vapour—liquid
contacting
ii. Packed towers—use of packings in columns for better vapour—liquid contacting.
i. Azeotropic distillation
Azeotropes: An azeotrope is a liquid mixture with an equilibrium vapour of the same composition as the liquid.
As the dew point and the bubble point are identical (same) at the azeotropic composition, the azeotropes are
called constant boiling mixtures (As the liquid and vapour compositions are the same, the boiling point of the
liquid mixture remains constant as the vapour is generated from it).
Close boiling components showing small deviations from ideality (Raoult's law) may form an azeotrope.
An azeotrope exhibits a maximum or a minimum boiling point relative to boiling points of the pure liquids and
thus are classified as maximum boiling and minimum boiling azeotropes.
 P a g e | 39 P a g e | 40
A minimum boiling azeotrope will boil at a temperature lower than the boiling points of the pure Choice of Entrainer:
components and a maximum boiling azeotrope will boil at higher temperature than the boiling points of pure 1. Entrainer should from a low boiling azeotrope with only one of the constituents of the binary
components. mixture.
In such cases, complete separation by ordinary fractionation may be impossible. The constituents of a 2. The new azeotrope formed must be sufficient volatility in order to make it readily separable from
binary azeotrope are separated completely by – the remaining constituent.
(1) Adding a third component to the binary mixture and 3. Cheap and readily available.
(2) Changing the system pressure. 4. Chemically stable.
The third component added (which is relatively volatile) to a binary azeotrope usually form a low 5. Non-corrosive.
boiling azeotrope with one or both of the feed components and this low boiling azeotrope is usually withdrawn 6. Non-toxic.
as the overhead product/distillate. 7. Low latent heat of vaporization.
The third component added to break the binary azeotrope to effect its separation into pure 8. Low freezing point to facilitate storage and handling.
components is called as the entrainer/azeotrope breaker. 9. Low viscosity to provide high tray efficiency and minimum pumping cost.
Azeotropic distillation is a distillation technique wherein a third component is added to a binary ii. Extractive distillation
azeotrope (feed) to effect the complete separation by forming an azeotrope with one or both of the feed Extractive distillation is defined as distillation in the presence of a miscible, high boiling, relatively
components and removing the azeotrope thus formed usually as the overhead product. non-volatile component, the solvent, that forms no azeotrope with the other components in the mixture.
Extractive distillation refers to the distillation process wherein a high-boiling solvent is added to alter
the relative volatilities of the constituents of a feed mixture.
It is necessary to alter the relative volatility of the original constituents because of similarities of the
vapour pressures of the constituents or the presence of an azeotrope.
The solvent selected is less volatile than either of the two constituents (of a binary mixture) and so as to
maintain a high concentration of the solvent throughout the column it is usually introduced a few stages below
the top stage.
An example of extractive distillation is the separation of toluene (b.p. = 110.8°C) from iso-octane (b.p. =
99.3°C) using phenol as an extractive solvent. In the presence of phenol, the relative volatility of isooctane
increases.

Working Procedure:
i. This is a special case of multicomponent distillation used for separation of binary mixture.
ii. Azeotropic distillation is either difficult or impossible to separate by ordinary fractionation.
iii. Under this circumstances third component, sometimes called an Entertainer may be added to binary
mixture to form a new boiling azeotropic with one of the original constituents.
iv. By this process volatility is easily occur and it can easily be separated from the other original
constituent.
v. Acetic acid can be separated from water by azeotropic method.
vi. To add butyl acetate is added to top of column.
vii. Azeotrope can readily be distillated from the high-boiling acetic acid, which leaves as a residue
product.
viii. Azeotrope is then distilled overhead. Working Procedure:
ix. Their composition is unchanged by distillation; azeotropes are also called constant boiling mixtures. i. This is multi components – rectification method similar in purpose to azeotropic distillation.
x. If two solvents can form a positive azeotrope, then distillation of any mixture of those constituents ii. To binary mixture which is difficult or impossible to separate by ordinary means a third common
will result in the distillate being closer in composition to the azeotrope than the starting mixture. termed a ‗solvent‘ (low relative volatility).
 P a g e | 41 P a g e | 42

iii. Isooctane in this mixture is the more volatile but the separation is difficult.
iv. In the presence of phenol, isooctane relative volatility increases, phenol in the liquid.
v. The separation from toluene is relatively easy.
vi. Solvent –Recovery section of the tower which may be relatively short, to separate the phenol from
Isooctane.
Residue – Toluene and phenol
Overhead Product – Isooctane
vii. The residue from the tower must be rectified in the tower to separate toluene from the phenol which
is recycled but this is a relatively easy separation.
viii. The method is used for mixtures having a low value of relative volatility, nearing unity.
ix. Such mixtures cannot be separated by simple distillation, because the volatility of the two
The composition of the distillate will now be different from that given by normal vaporization and the
components in the mixture is nearly the same, causing them to evaporate at nearly the same
ratio of the constituents is given by
temperature at a similar rate, making normal distillation impractical.
General Requirements of Extractive distillation solvent:   PA  
  0.5  
1. High selectivity and ability to alter VLE of the original mixture. N A Moles of A   M A  
 
2. High capacity or ability to dissolve the components in mixture. N B Moles of B   PB  
3. Low volatility in order to prevent vaporization of solvent.   0.5  
  M B  
4. Easy separability, for easier removal of the solvent.
In molecular distillation this ratio is maintained by allowing the liquid to flow in a thin film over a solid
5. Cheap and easily available.
surface thus renewing the surface continually and at the same time maintaining low hold-up of liquid.
6. Non-toxic.
A schematic arrangement of a device used for this type of distillation is shown in above figure. The
7. Non –corrosive.
degassed liquid to be distilled is introduced at the bottom of the inner surface of the rotor, rotating at 400 to 500
8. Chemically stable.
rpm. A thin layer of liquid 0.05 to 0.1 mm spreads over the inner surface and travels rapidly to the upper
9. Low freezing point.
periphery under centrifugal force.
10. Low viscosity.
Heat is supplied to the liquid through the rotor from radiant electrical heaters. Vapours generated are
Comparison of Azeotropic and Extractive distillation:
condensed and collected in the collection troughs. The residue liquid is collected in the collection gutter and
In both the processes an additional external agent is added, which is undesirable. Solvent to feed ratio in
removed.
extractive distillation greater than 3 or 4 is found to be effective. Proper choice of material of construction and
The entire unit is maintained at low pressure, good enough for molecular distillation to occur. Normal
recovery technique are to be examined.
residence time is of the order of 1 second and hence decomposition of mixture does not take place. Multiple
However, of the two, extractive distillation is said to be more favoured than azeotropic distillation since,
units can be used to have multistage separation effects.
i. There is a greater choice of solvent.
iv. Low Pressure Distillation
ii. The smaller quantity of solvent to be volatilized.
Whenever the heat sensitive materials are to be separated, as in the case of many organic mixtures, low
In spite of the above advantages, the azeotropic distillation is said to be more effective in the
pressure distillation will be effective.
dehydration of ethanol from an 85.6 mole % Ethanol—water solution. In this case water is azeotroped with n—
pentane and then separated rather than using extractive distillation with ethylene glycol as solvent.
iii. Molecular distillation or vacuum distillation
Molecular distillation or vacuum distillation is a method of distillation whereby the pressure above
the liquid mixture to be distilled is reduced to less than its vapor pressure (usually less than atmospheric
pressure) causing evaporation of the most volatile liquids (those with the lowest boiling points).
This distillation method works on the principle that boiling occurs when the vapor pressure of a liquid
exceeds the ambient pressure.
Vacuum distillation is used with or without heating the mixture.
This is a very low pressure distillation where the absolute pressure is in the range of 0.003 mm Hg to
0.03 mm Hg. On reducing the absolute pressure, the mean free path of the molecules becomes large.
If the condensing surface is placed at a distance from the vaporizing liquid, surface not exceeding few
cms, only a few molecules will return to the liquid.
 P a g e | 43 P a g e | 44
In this case the time of exposure of the substances to high temperature is kept minimum. In plate columns, the minimum plate spacing is 300 mm. For columns diameter 2.5m or more spacing of
i. Packed towers can be used for distillation under pressures of 50 to 250 mm Hg. 450 or 600 mm is used for easier tray access.
ii. Bubble cap and sieve trays can be used for pressure drops around 2.6 mm Hg. In plate columns, plates are provided with downcomers and weirs. The function of the downcomer is to
iii. Shower trays for pressure drops around 0.75 mm Hg. provide a passage for the downward flow of the liquid from a plate above to the plate below.
This is used in the separation of vitamins from animal and fish oils as well as the separation of The downcomer area for the each plate is limited to 10% of the total area of the plate. Pipe downcomer,
plasticizers. segmental downcomer and chord type downcomer are various types of downcomers that can be used.
DISTILLATION TOWERS/COLUMNS A depth of liquid on the plate required fur gas contacting is maintained by an overflow (outlet) weir. An
Distillation (fractionation) is the most widely used mass transfer operation in the chemical industry. In inlet weir helps to distribute liquid as it enters the plate from the downcomer and prevents impingement of
case of this operation, the gas-liquid contacting devices for mass transfer are: plate columns and packed liquid on a contacting device.
columns. i. Bubble cap plate (tray)
A column is also known as a tower. It is essentially a tall vertical cylindrical shell, with number of In case of bubble cap tray, gas/vapour flows through a riser, reverses flow under cap, moves downward
nozzles. The column consists of a series of plates or trays or variety of packings (usually random packings). through the annular space between the riser and the cap, and finally it bubbles into a pool of liquid through a
Based upon the contacting devices used for mass transfer to take place, the towers/columns are divided series of slots (openings) provided along the periphery of the cap at the bottom. The slots may be circular.
into two types namely, plate or tray columns and packed columns. rectangular or trapezoidal in shape.
1. PLATE COLUMNS
The process of distillation with rectification makes use of either a plate (tray) column or packed column,
for intimate phase contacting, the former being more common. In the plate columns, the process of mass
transfer is stage wise and in packed towers/columns, the process of mass transfer is continuous.
Each plate in a vertical column represents a stage as on each plate, phases (gas and liquid) are brought
into intimate contact, mass is transferred from one phase to another (to and from both the phases) and finally
phases are separated and leave the plate/tray in equilibrium (ideal case).
A plate column is a vertical column divided into sections by a number of horizontal plates. In this
column the liquid enters the plate from the top, flows over the plate and then from plate to plate via
downcomers.
A certain height of a liquid pool is maintained on each plate with the help of an outlet weir. Gas/vapour Bubble cap disperses the gas phase into the liquid as the fine bubbles; it prevents the liquid drainage
enters in the column from bottom inlet and flows upward through the opening in the plate; it bubbles through through the gas passage at low gas rates. It directs the gas flow first horizontally and then vertically upward
the pool of liquid on the plate, disengages from liquid and passes to the plate. through the pool of liquid in the form of bubbles.
The bubble cap columns can be operated with high and constant stage efficiencies over a wide range of
the vapour and liquid flow rates. Bubble cap plates are now rarely used for new installations because of
a) Their relatively high cost
b) High pressure drop
ii. Sieve plate
Vary common plates in use in recent years are the perforated plates because of their
a) Simplicity
b) Low cost
A sieve plate is the perforated plate employing the perforations for dispersing gas into liquid on the
plate. It is a metal sheet having hundreds of round perforations in it of the size ranging between 3 to 12 mm (5
mm is a common size).

Various plates used for contacting of phases are:

i. Bubble cap plate/tray
ii. Sieve plate
iii. Valve plate
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The total area of holes ranges from 5 to 15 % of the plate area. In the sieve plate column, liquid flows i. Cross flow: It is most frequently used. Provides a good length of the liquid path. Here the liquid
across the plate and gas passes vertically upward through the holes, in the form of bubbles through the liquid on flows across a plate and then falls to the plate below through a passage at the other side of the plate.
the plate. Gas flow through the perforations prevents the down-flow of liquid through perforation in the plate ii. Reverse flow: Provides a very long liquid path especially suitable for low liquid to gas ratios.
but at low flow rates weeping (draining of the liquid through perforations in plate) is severe which in turn iii. Split flow: Especially suitable for handling high liquid to gas ratios. Here the liquid flowing across
reduces stage efficiencies, and this is a limitation of the sieve plate. the plate is splitted into at least two paths.
Gas-liquid contact is poor with the sieve plate as compared to that with bubble cap plate because in Downcomers and Weirs:
sieve plate gas is directed vertically and in the bubble cap plate gas is first directed horizontally and then moves A downcomer is the passage for liquid flow from a plate above to the plate below which may be in the
vertically upward. form of circular pipes or segments of the tower/column set aside (for liquid flow) by vertical plates (partitions).
The pressure drop with sieve plate is low as compared to it with bubble cap columns. This is the most The discharge end of the downcomer is generally projected far enough into the liquid on the plate so as
common type of plate (or tray) contacting device. It is usually operated over a wide range of flow rates between to avoid vapour (gas) from rising up the downcomer to short-circuit the plate above.
weeping and flooding points. For this purpose, inlet weir may be used. An exit weir or outlet weir is used for maintaining a certain
iii. Valve plate: depth of liquid (liquid pool) on each plate needed for the gas contacting. Straight rectangular weirs with length
It is the recent development in the perforated plates. A valve plate is nothing but a perforated metal equal to 60 to 80% of the tower diastole are frequently used.
sheet wherein the perforations are covered with liftable caps (valves).

The valves are metal discs and are held in the plate by means of legs which restrict the upward motion
of caps. The valve provides variable orifices for vapour flow i.e. opening in the plate will be small at the low
vapour rate and large at high vapour/gas rate. Entrainment:
Thus weeping will be greatly reduced with this plate at low gas rates. Valve plates can be operated over As gas/vapour bubbles through the pool of liquid on a plate, a large amount of turbulence is set up and
a wide range of phase flow rates. Gas-liquid contact with the valve plate is much better than it with sieve plate the liquid particles can be entrained by the rising gas. Carry-over of liquid particles by the rising gas from a
as liftable caps direct the gas horizontally into the liquid on the plate while in sieve plate gas passes vertically plate below to the plate above is known as entrainment and is much more pronounced at high gas flow rates.
upward through the liquid. The cost of the valve plate is in between that of bubble cap and sieve prate, Entrainment reduces the concentration change per plate and hence, decreases the plate efficiency. Tray
approximately twenty percent higher than that of the sieve plate. spacing, vapour flow rate, depth of liquid on the plate is the factors on which the amount of entrainment
Liquid flow patterns over plate/tray: depends.
The type of liquid flow pattern over a plate depends upon liquid to gas flow ratio. Various flow patterns
are:

2. PACKED COLUMNS FOR DISTILLATION

For distillation operation, packed columns are especially useful whenever we have to carry out operation
at low pressure (vacuum distillation) and whenever we are dealing with heat sensitive materials.
Packed columns are cheaper than plates for column diameter less than 600 mm. A packed column
consists of a cylindrical shell filled with some sort of packings (rings or saddles) which offer a large interfacial
area for mass transfer.
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A common arrangement of the packed column for distillation operation is shown in following figure, UNIVERSITY IMPORTANT QUESTIONS
wherein the vapour flows upward and the refluxed liquid flows downward giving a continuous contact. Part-A
The ability of a given packing to affect the desired mass transfer between gas and liquid phases (i.e. to 1. State Raoult's law
affect the desired degree of separation) is usually expressed as the height equivalent to one theoretical plate 2. Define Relative volatility in distillation column
(HETP). 3. What is meant by Reflux ratio?
In plate columns wherein a process of enrichment is stage wise, the vapour leaving the plate is richer 4. What does Fenske's equation determine?
with respect to more volatile component than the vapour entering the plate by one equilibrium stage. 5. What is plate efficiency?
In packed columns, the same enrichment of the vapour will occur in a certain height of packing which is 6. What is Murphree tray efficiency?
termed as the height equivalent to one theoretical plate or height equivalent to a theoretical plate. 7. Distinguish between equilibrium distillation and differential Distillation.
Thus, in packed columns, one equilibrium step is represented by a certain height of a packed bed and the 8. Write Rayleigh‘s Equation
required height of packing for the desired degree of separation is given by: HETP x number of ideal plates 9. What is steam Distillation?
required. 10. What is the use of entrainer in azeotropic distillation?
HETP is defined as the height of packing (packed bed) giving the enrichment of vapour same as that can 11. Define Molecular distillation.
be obtained by one theoretical plate (in stage-wise operation). 12. Write P-X-Y diagram for constant temperature?
13. Define Dalton's law? How do you relate the law with the composition?
14. How does reflux ratio depend on separation efficiency?
15. Enlist the assumptions made in McCabe Thiele Method?
16. State Henry‘s law and its significance.
17. Sketch the T-x-y and P-x-y diagrams of minimum boiling azeotropes.
18. The vapor pressures of A and B are 250 mm Hg and 500 mm Hg .The total pressure is 800 mm Hg.
Estimate the relative volatility.
19. Explain the significance of q line.
20. What are ideal and non-ideal solutions? Give an example.
Part-B
1. Derive Fenske's equation and state its limitation.
2. A mixture of benzene and toluene containing 40 mole percent of benzene' is separated to give a product
of 90 mole percent of benzene at top and a bottom product with not more than 10 mole percent benzene.
Using an average value of a 2.4 for the volatility of benzene relative to toluene, calculate the number of
theoretical plates required at total reflux. Also calculate the minimum reflux ratio, if t feed is liquid and at
its boiling point.
3. Explain the utility of McCabe-Thiele method in determining the number of ideal plates in a fractionating column
and list out the limitations of this method.
4. Describe the following with neat flow diagram.
i. Azeotropic distillation
HETP can be estimated with the help of the following empirical equation such as
ii. Simple distillation
1 
HETP  k1.G k 2 .Dtk3 .Z 3 . . L  iii. Low pressure distillation
 L  iv. Steam distillation
v. Extractive Distillation
Where, vi. Molecular distillation
k1, k2 & k3 - Empirical constants for packing and are function of type and size of packing. 5. Illustrate the method of calculation of ideal trays by Panchon - Savarit method.
G - Superficial gas mass velocity 6. A Benzene -Toluene solution containing 55% Benzene is to be fractionated continuously in a distillation
Dt - Tower diameter column to get a top product of 85%, and a bottom product of 10%Benzene. The feed is at its bubble
Z - Height of packing point. The relative volatility is 2.5. Find
(a) The no. of plates required for a reflux ratio of 2.5.
α - Relative volatility
(b) Minimum no. of plates.
µL & ρL- Viscosity and Density of liquid respectively.
7. A fractionating column separates a liquid mixture containing 50 mole % A and 50 mole % B into an overhead
HETP is an experimental quantity, a characteristic of each packing and depends on the type and size of product of 95 mole % A and a bottom product of 96mole A. A reflux ratio of twice the minimum will be used and
the packing, flow rates of each fluid and concentration. the feed .enters at its boiling point. Determine the number of theoretical stages required and the location of feed
************************************************** point. Equilibrium data:
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X 0.03 0.06 0.11 0.14 0.26 0.39 0.53 0.66 0.76 0.86
Y 0.08 0.16 0.27 0.33 0.50 0.63 0.71 0.83 0.88 0.93
Where, X, Y mole fraction of A in liquid and vapor phase respectively.
8. 1000 kmol/hr of ethanol-propanol mixture containing 65 mole % ethanol is to be separated in a continuous
.plate column operating at 1 atm. pressure. The desired terminal compositions for ethanol are : X D = 0.92 and
Xw = 0.07. The feed is a saturated vapor and a total condenser is passed. When reflux ratio is four times the
amount of top product, find the number of theoretical plates required for the separation. Data given: Relative
volatility = 2.10. Also find Nmin.
9. A binary distillation column is operating under conditions as feed rate = 450 kmol/h, overhead product rate =
200 kmol/h, XD = 0.95, XW = 0.05, W=250kmol/h R= 35. In the stripping section, it was found that the mol.
fraction of more volatile component in the vapor leaving a plate is 0.35 while the mole fraction in the liquid
coming to the same plate is 0.25. Assuming constant molal overflow, determine whether the feed is vapor,
liquid or partially vapor.
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