MASS TRANSFER ECP 224

UNIT 2
DISTILLATION
 OUTLINE
 Introduction to distillation- basics and theory
 Vapor liquid equilibrium
 Phase Diagram
 X-Y Diagram
 Azetrope
 Batch distillation
 Flash distillation
 Continuous distillation
Tray distillation column
 Analysis of McCabe and thiele method for binary system
 Analysis of Ponchon-savariat method for binary system
 Tray efficiency
Packed distillation column
Approximate column sizing
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 INTRODUCTION
 Distillation is a method of separation of components
from a liquid mixture which depends on the
differences in boiling points of the individual
components.

 Distillation is based on the fact that the vapour of a

boiling mixture will be richer in the components that
have lower boiling points.

 Important aspects of distillation that seem to be

missed from the manufacturing point of view are that:
 distillation is the most common separation technique
 it consumes enormous amounts of energy, both in terms of
cooling and heating requirements
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 CONCEPT OF EQUILIBRIUM
 The separation processes are based on the
equilibrium stage concept which states that
streams leaving a stage are in equilibrium.
 Liquid molecules are continually vaporizing,
while vapor molecules are continually
condensing.
 If two chemical species are present, they
will, in general, condense and vaporize at
different rates.
 When not at equilibrium, the liquid and the
vapor can be at different pressures and
temperatures and be present in different
mole fractions.
 At equilibrium the temperatures, pressures,
and fractions of the two phases cease to
change.
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VLE: Raoult’s Law

Where xi is a liquid phase mole fraction, yi is a

vapor phase mole fraction, and Pisat is the vapor
pressure of pure species i at the temperature of
the system (a function of temperature only).
The product yiP is known as the partial pressure
of species i.

 Raoult’s Law for ideal phase behavior

relates the composition of liquid and
vapor phases at equilibrium through
the component vapor pressure, Pisat.

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VLE: RAOULT’S LAW

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VLE: RAOULT’S LAW

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VLE: RAOULT’S LAW

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 VAPOR PRESSURE
 The pressure exerted by the gas in equilibrium with a solid
or liquid in a closed container at a given temperature.
 The vapor pressure can be calculated from Clausius-
Clapeyron Equation or by using Antoine Equation,

CLAUSIUS-CLAPEYRON EQUATION:
Where pV and p1V are the vapour pressures
in Pascal at absolute temperature T and T1 in
K. λ is the molar latent heat of vaporization
which is independent of temperature.

ANTOINE EQUATION:

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Typical representative values of the constants A, B and C

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 VOLATILITY
 Volatility: is a measure of the tendency of a substance to
vaporize

 Water, at a temperature of 25 °C, has a vapour pressure of

0.03 atmospheres while Methanol, at the same temperature,
has a vapour pressure of 0.16 atmospheres

 Methanol is more volatile than water => more likely to be found

as vapour. Vapour pressure is a measure of volatility. Methanol
has a lower boiling point (65 °C) than water

 Volatile liquids have low boiling points

 Volatility = Pa/xa (Pa= partial pressure, xa = mole fraction)

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 RELATIVE VOLATILITY
 Relative volatility (α): is a measure of the differences in volatility
between two components, and hence their boiling points.
 The relative volatility of component ‘A’ with respect to component
‘B’ in a binary mixture is defined as:
𝑦𝐴 𝑦𝐴
𝛼𝐴𝐵 =
𝑦𝐵 𝑦𝐵
 where, yA = mole fraction of component ‘A’ in the vapor, xA = mole
fraction of component ‘A’ in the liquid. In general, relative volatility
of a mixture changes with the mixture composition. For binary
mixture, xB = 1-xA.
 So Equation can be rearranged, simplifying and expressed by
dropping subscript 'A' for more volatile component as:
𝜶𝒂𝒗𝒆 𝒙
 𝒚=
𝟏: 𝜶𝒂𝒗𝒆 ;𝟏 𝒙

 It indicates how easy or difficult a particular separation will be.

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Some Optimal Relative Volatility That Are Used
For Distillation Process Design

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 PHASE DIAGRAM
 The more volatile component (MVC) is labelled as x in the liquid
phase concentration and y in the vapour
 xA = mole fraction of a in liquid.
 xA = mole fraction of a in vapour
 Bubble point curve and Dew point curve are both shown,
 Bubble = Dew for pure components only
 Sub-cooled liquid beneath bubble point curve
 Super-heated vapour above dew point curve
 Both liquid and vapour phases exist in between

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PHASE DIAGRAM

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PHASE DIAGRAM

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BOILING A MIXTURE – (METHANOL-
WATER MIXTURE)

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BOILING A MIXTURE CONTD’

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CONDENSING A BINARY MIXTURE

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X-Y DIAGRAM
 An alternative method of
presenting Vapour
Liquid Equilibrium (VLE)
data
 XA is plotted against YA
– usually a curve
 The X=Y line is also
shown
 An easy way to estimate
how many distillations
are required to achieve
a certain purity

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EXAMPLE– ETH- H2O

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 AZEOTROPE
 Azeotrope (constant boiling mixtures): A boiling
liquid at this composition produces a vapor of exactly
the same composition
 No separation is possible by conventional distillation
at azeotropic point.
 Dewpoint and bubble point are the same at the
azeotrope
 Usually occurs at a particular mole fraction. Outside
this point separation is possible
 Can have a minimum or maximum boiling point
azeotrope
 Can limit the separation and purity of the product
 Changing the pressure can be the solution –
Extractive Distillation DEPARTMENT OF CHEMICAL AND
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DISTILLATION METHODS
Single stage distillation methods :
 Equilibrium/Flash distillation
 Batch or differential distillation
 Steam distillation

Multistage distillation methods: (fractional

distillation, distillation with reflux or rectification)

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FLASH DISTILLATION

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 FLASH DISTILLATION
 A liquid mixture is partially vaporized.
 The vapour is allowed to come to equilibrium with the liquid,
and the vapour and liquid phases are then separated.
 This can be done batch wise or continuously.

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 BINARY FLASH DISTILLATION
 Overall balance F = L +V
 Species balance zi F= xi L+ yiV
 Re-arranging

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DEPARTMENT OF CHEMICAL AND
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 GRAPHICAL SOLUTION FOR A
FLASH DISTILLATION
 The intersection of the equilibrium curve and the operating line is
the solution (answer) of the material balances (this plot is called
“McCabe-Thiele diagram”) for the flash distillation, as the
intersection of the equilibrium line (curve) and the operating line is
the point where the system (i.e. the flash tank) reaches the
equilibrium

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 PROBLEM
We are separating a mixture of methanol and water in a
flash drum at 1atm pressure. Equilibrium data are shown
in the figure.
a)Feed is 50 mol% methanol, and 40% of the feed is
vaporized. What are the vapour and liquid mole
fractions and flow rates? Feed rate is 100 kg
moles/hr.

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BATCH DISTILLATION

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 BATCH DISTILLATION
 (more volatile) and B (less volatile). The system
consists of a batch of liquid (fixed quantity) inside a
kettle (or still) fitted with heating element and a
condenser to condense the vapour produced as
shown in Figure below.
 Batch distillation is versatile
and commonly employed for
producing biochemical,
biomedical, and/or
pharmaceutical products, in
which the production
amounts are small but a very
high purity and/or an ultra-
clean product is needed.

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 BATCH DISTILLATION PROCESS
 There may be several reasons for running a batch
process such as this:
i. Small capacity doesn’t warrant continuous
operation
ii. Separation is to be done only occasionally
iii. Separation is preparative to produce a new product
iv. Upstream operations are batch-wise or feed-stocks
vary with time or from batch to batch
v. Feed materials are not appropriate for a continuous
flow system.

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 BATCH DISTILLATION
Overall balance:

more volatile component (MVC) balance:

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 Normally, Wo and xo are specified (or given in the
problem statement), and the value of either, xw,final or
xD, is also specified (or given).
 Thus, there are 3 unknowns for the binary mixture
batch distillation system: Wfinal , Dtotal either xw,final or
xD,
 However, by just performing material balances, we
have only 2 equations
 The additional equation for solving batch
distillation problems is commonly known as the
Rayleigh equation

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 RAYLEIGH EQUATION
The rate of distillate flowing out of the batch distillation system, dD,
is equal to the rate at which the liquid in the still pot is decreasing, -
dW

The rate of species i in the distillate flowing out of the batch distillation
system, xD dD, is equal to the decreasing rate of species i the liquid in the
still pot -(d Wxw)

The instantaneous rate of depletion of a component in the liquid is given by:

Rearranging to use separation of variables gives:

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 RAYLEIGH EQUATION
 Integrate both sides between xo (composition in the feed)
to xwfinal:
 Graphical integration of the LHS of Rayleigh Equation can be done by
 Plot an equilibrium curve
 At each value of x ,(xo, to xw,final) determine the value of y from
the equilibrium curve/equation

 Graphically determine the area under the curve from xo, to xw,final
or perform the integration numerically
 After the numerical value of the integration is obtained, the value of Wfinal
(i.e. the amount of liquid remained in the still pot) can be obtained

 Average distillate concentration, xD,avg , and the total amount of the

distillate, Dtotal, can be obtained from simultaneous solution of

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 EXAMPLE PROBLEM
A mixture of 40 mole % isopropanol in water is to be
batch-distilled at 1 atm until 70 mole % of the charge has
been vaporized. Calculate the composition of the liquid
residue remaining in the still pot, and the average
composition of the collected distillate. VLE data for this
system, in mole fraction of isopropanol, at 1 atm are
(Seader and Henley, 1998):

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 SOLUTION
Assume 100 moles of feed
Given Data:
xo = 0.4
Feed Wo= 100 moles
Distillate Dtotal = 70moles
Liquid residue remaining in still pot Wfinal= Wo - Dtotal=
100-70= 30 moles

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 SOLUTION

Find xw,final by trial error by

The value of xw,final = 0.067

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CONTINUOUS
DISTILLATION

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 DISTILLATION COLUMN
 Remember that boiling results in a change of composition, and
condensing also results in a change of composition
 Therefore, combine the two processes inside the column to improve the
distillation process
 A distillation column is designed to encourage vapour liquid contact
 Falling liquid meets rising vapour. Boiling and condensing do not just occur
in the reboiler and the condenser. They happen inside the column also.

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 BASIC OPERATION
 The liquid mixture that is to be separated is known as
the feed and is usually introduced somewhere near the
middle of the column to a tray known as the feed tray.
 The feed tray divides the column into a top part called
(enriching or rectification section and a bottom part
stripping section.
 In binary distillation, a feed mixture of two components
is separated into two products, an overhead product
distillate and a bottom product, whose compositions
differ from that of the feed.

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LIQUID MOVEMENT
 Feed flows down the column where it
is collected at the bottom in the
reboiler.
 Heat is supplied to the reboiler to
generate vapour. The source of heat
input can be any suitable fluid,
although in most chemical plants this
is normally steam. In refineries, the
heating source may be the output
streams of other columns.
 The vapour produced in the reboiler
is re-introduced into the unit at the
bottom of the column. The liquid
removed from the reboiler is known
as the bottoms product or simply,
bottoms.

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 Vapour movement
 The vapour moves up the
column, and as it exits the top
of the unit, it is cooled by a
condenser.

 The condensed liquid is stored

in a holding vessel known as
the reflux drum.

 Some of this liquid is recycled

back to the top of the column
and t is called the reflux.
 Inside the column, the liquids and
vapors are always at their bubble and
 The condensed liquid that is
dew points respectively, so that the
removed from the system is
highest temperature is at the bottom,
known as the distillate or top
the lowest at the top.
product.
 Note: In a distillation column the stages
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MAIN COMPONENTS OF DISTILLATION
COLUMNS
 A typical distillation contains several major components:
 Stripping Section – MVC is vapourised
 Rectifying Section – LVC is condensed
 Column internals such as trays/plates and/or packings encourage
vapour liquid contact
 Reboiler: where heat necessary for vaporization of the liquid is
supplied
 Condenser: to cool and condense the vapour leaving the top of the
column
 Reflux drum: to hold the condensed vapour from the top of the
column so that liquid (reflux) can be recycled back to the column
 Vertical shell: houses the column internals

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 COLUMN INTERNALS
 Trays and Plates: Most common tray designs
 Bubble cap trays
 Valve trays
 Sieve trays
 Packings

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HOW TO SEPARATE A BINARY MIXTURE – POT STILL

 Boil the mixture, condense the vapour and collect the distillate.
Repeat the procedure until the desired purity is obtained.
 EACH STILL IS A STEP ON THE X-Y CURVE+

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CLASS ACTIVITY – COUNT STAGES

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CALCULATION METHODS
Types of Binary Distillation Calculation

 Energy requirements and heat exchanger design for a given

adiabatic separation process (calculate the heat duties of the
condenser and reboiler, specify the heating steam consumption
and coolant requirements, thermal-hydraulic design of the
condenser and reboiler)

 Determination of main dimensions of the distillation column:

estimating the number of equilibrium stages required for a given
separation, the column height and the column diameter for a
desired pressure drop (H = f(N), D)
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 Historical Review of Calculation Methods
Until 1970s:
 Simplified, graphical design procedures for tray columns separating binary mixtures:
 Ponchon- Savarit (1921/22),

 McCabe-Thiele (1925)

 Approximate calculation methods for the solution of multicomponent, multistage

separation problems (Shortcut methods): Fenske (1932), Gilliland (1940),
Underwood (1946)

 Design of packed columns based on NTU/HTU concepts: Chilton, Colburn (1935)

in the present:
 complex mathematical matrix methods allow to find exact solutions of nonlinear
equation systems: Wang-Henke (1966),

 Naphtali-Sandholm (1971) commercial process simulation software allowing design

and rating calculations of tray and packed columns operating at steady or unsteady
state conditions (ASPEN, CHEMCAD)

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MCCABE THIELE METHOD

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 McCABE-THIELE METHOD
ASSUMPTIONS AND SIMPLIFICATIONS
 The two components have equal and constant molar enthalpies of
vaporization (latent heats).

 The component heat capacity changes and the heat of mixing are
negligible compared to the heat of vaporization (considering ideal
behaviour of binary mixtures).

 The distillation column, the condenser and the reboiler are well
insulated so that heat losses to environment are negligible.

 That means, that all liquid and vapor molar flow rates in the
rectifying section are constant and that all liquid and vapor molar
flow rates in the stripping section are constant but not the same
as those in the rectifying section.
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 DESIGN PROCEDURE McCabe-Thiele Method
 The steps to be followed to determine the number of theoretical stages by
McCabe-Thiele Method:
1. Start with VLE data and draw an x-y diagram
2. On the x-y diagram draw the line y=x or the 45oC line
3. Determine the Rectifying section operating line (ROL) and draw it on the
x-y diagram
4. Determine the feed condition and use it for the determination of the feed
section operating line (q-line) and draw it on the x-y diagram
5. Determinate the stripping section operating line (SOL) and draw it on
the x-y diagram
6. Using the ROL and the equilibrium curve draw steps from the distillate
composition to the feed point.
7. when you reach point of intersection of q-line, ROL and SOL start stepping
using equilibrium curve and SOL until you reach the required composition
of the bottoms.
8. Count the number of steps. Each one equals an equilibrium or theoretical
stage
9. Using the stripping operating line and the equilibrium curve draw steps
from the bottoms composition to the feed point
10. Convert this to a number of plates by dividing by the plate efficiency.

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DETERMINATION OF THE RECTIFYING SECTION
OPERATING LINE (ROL).
 Consider loop I in the rectifying section
 Material balance

 Overall balance: 𝑉𝑛:1 = 𝐿𝑛 + 𝐷 I

Component balance (MVC):
𝑦𝑛:1 𝑉𝑛:1 = 𝐿𝑛 𝑥𝑛 + 𝐷𝑥𝑑
𝐿𝑛 𝐷
𝑦𝑛:1 = 𝑥𝑛 + 𝑥𝑑
𝑉𝑛:1 𝑉𝑛:1
Applying constant molar overflow
𝑳 𝑫
𝒚 = 𝒙 + 𝒙𝒅
𝑽 𝑽
𝐿
But: 𝑉 =𝐿+𝐷 Reflux ratio(R) : 𝑅=
𝐷
This is expressed as:
𝑹 𝟏
𝒚= 𝒙+ 𝒙𝒅
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 𝑹 𝟏
𝒚= 𝒙+ 𝒙𝒅
𝑹+𝟏 𝑹+𝟏
 This Equation is the rectifying section operating line
(ROL) Equation having
slope = R/(R+1) and
Intercept = xD/(R+1)

 The line has the coordinates Point 1 (x= xD, y = xD),

the operating line passe through the point (xD, xD) on
the 45o diagonal line.

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 Construction of ROL on x-y diagram
 ROL is constructed as follows.
 Desired top product composition(xD) is located on the x-y diagram, by drawing
a vertical line until it intersects the diagonal line..
 A line with slope R/(R+1) is then drawn from this intersection point as shown in
the diagram below.

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DETERMINATION OF THE STRIPPING SECTION
OPERATING LINE (SOL).  Consider loop II
Material balance
𝐿′ 𝑚:1 = 𝑉 ′ 𝑚 + B

𝐿′ 𝑚:1 𝑥𝑚:1 = 𝑉 ′ 𝑚 𝑦𝑚 + B𝑥𝐵

II
𝐿′ 𝑚:1 𝐵
𝑦𝑚 = ′ 𝑥𝑚:1 − ′ 𝑥𝐵 SOL
𝑉𝑚 𝑉𝑚
𝐿′ 𝐵
𝑦 = ′ 𝑥 − ′ 𝑥𝐵
APPLYING CONSTANT MOLAL OVERFLOW: 𝑉 𝑉
 Boil-up ratio(𝑉𝐵 ): is as the ratio of vapour returning to the column
𝑉′
to the bottoms product flow: 𝑉𝐵 = 𝐵
𝑉𝐵 + 1 1
 SOL can, also be expressed as: 𝑦=
𝑉𝐵
𝑥 − 𝑥𝐵
𝑉𝐵

 The stripping operating line (SOL) which is a straight line with slope ( L' / V' ) and
intercept ( B𝑥𝐵 / V'). When 𝑥 = 𝑥𝐵 , y =𝑥𝐵 , the SOL passes through (𝑥𝐵 , 𝑥𝐵 ) on the
45 o diagonal line.
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STRIPPING LINE ON X-Y DIAGRAM
 SOL is constructed starting from desired bottom product ( xB )
composition. A vertical line is drawn from this point to the
diagonal line, and a line of slope L/V is drawn as illustrated in
the diagram below.

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PROBLEM – OPERATING LINES
 A mixture of Acetic Acid and Acetic Anydride
containing 40 mol % Acetic Acid is to be
separated by distillation. The top product is
to be 90 mol % Acetic Acid and the bottom
product 10 mol % Acetic Acid. The feed is
heated to its boiling point. The vapour is
condensed but not cooled and some is
returned at a reflux ratio of 3 kmol/kmol
product. Determine the operating lines for
the rectifying and stripping sections and
draw them on an equilibrium curve.

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SOLUTION

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POSSIBLE FEED CONDITIONS

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FEED CONDITION and THE q-VALUE

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 Derivation of q- line
 The point of intersection of the ROL and SOL on x y lot can
be derived as: 𝑉 , 𝑚 𝑦 = 𝐿, 𝑚 𝑥 + 𝐵𝑥𝐵
𝑉𝑛 𝑦 = 𝐿𝑛 𝑥 + 𝐷𝑥𝐷
Where the y and x values are the point of intersection of the two
operating lines
Subtracting: 𝑉 , 𝑚 − 𝑉𝑛 𝑦 = 𝐿, 𝑚 − 𝐿𝑛 𝑥 − 𝐷𝑥𝐷 + 𝐵𝑥𝐵
Substituting the previously marked equations and the total balance
equation: F𝑥𝐹 = 𝐷𝑥𝐷 + 𝐵𝑥𝐵
Into the above equation
The q line Equation
𝑞 𝑥𝐹
and rearranging results 𝑦 = 𝑞 𝑥 − 𝑞
𝑞−1 𝑞−1

 For a given feed condition, 𝑥𝐹 and q  At this condition the q-line

are fixed, therefore the q-line is a passes through the point (𝑥𝐹 ,
straight line with slope -q / (1-q) and 𝑥𝐹 ) on the 45o diagonal.
intercept 𝑥𝐹 /(1-q). Different values of q will result
in different slope of the q-line.
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q-lines for different feed conditions

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 CALCULATION OF q-VALUE
 For saturated liquid (q = 1) and saturated vapour (q = 0). In other
cases one must calculate
𝐻𝑒𝑎𝑡 𝑡𝑜 𝑣𝑎𝑝𝑜𝑟𝑖𝑠𝑒 1 𝑚𝑜𝑙 𝑜𝑓 𝑓𝑒𝑒𝑑
the value of q. 𝑞 =
𝑀𝑜𝑙𝑎𝑟 𝑙𝑎𝑡𝑒𝑛𝑡 𝑕𝑒𝑎𝑡 𝑜𝑓 𝑣𝑎𝑝𝑜𝑟𝑖𝑠𝑎𝑡𝑖𝑜𝑛
𝐻𝑣 − 𝐻𝐹 Where: Hv- is the enthalpy of the feed at the dew
𝑞= point, HL -the enthalpy of the feed at the boiling point
𝐻𝑉 − 𝐻𝐿
(bubble point), HF- the enthalpy of the feed at its entrance
conditions
 If the feed is a mixture of liquid and vapour then q is the fraction that
is liquid
For cold liquid feed (q>1): For superheated vapor
feed (q<1):
𝐶𝑝,𝐿 𝑇𝑏𝑝 − 𝑇𝐹 + 𝜆
𝑞= 𝐶𝑝,𝑉 𝑇𝑏𝑝 − 𝑇𝐹
𝜆 𝑞=
Where: 𝐶𝑝,𝐿 heat capacity of the liquid, 𝐶𝑝,𝑉 𝜆
heat capacity of the liquid, Tbp is the bubble
point, l is the latent heat of vaporization TF
feed temperature and Tdp is the dew point of
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 MCCABE THIELE METHOD:
SPECIFICATIONS REQUIRED

 The following information is needed

F : Total feed rate
xF : Mol fraction of MVC in the feed
P : Column operating pressure
xD : Mol fraction of MVC in the distillate
xB : Mol fraction of MVC in the bottoms
R/Rmin : Ratio of reflux to minimum reflux

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MCCABE THIELE METHOD :
RESULTS PROVIDED
 McCabe Thiele provides the following results
D: Overall distillate flowrate
B: Overall bottoms flowrate
Nmin : Minimum number of equilibrium stages
Rmin : Minimum reflux ratio (Lmin/D)
R: Reflux ratio (L/D)
VB : Boilup ratio (V/B)
N: Number of equilibrium stages
xn, yn : Vapour and liquid compositions at
each of the stages DEPARTMENT OF CHEMICAL AND
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 DESIGN ILLUSTRATED

 The feed stage/tray is the stage that

crosses from the rectifying or enriching
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DESIGN ILLUSTRATED

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 EXAMPLE PROBLEM11.4-1 (GEANKOPLIS)
A liquid mixture of benzene-toluene is to be distilled in a
fractionating tower at 101.3 kPa pressure. The feed of 100 kg
rnol/h is liquid and it contains 45 mol % benzene and 55 mol %
toluene and enters at 327.6 K (130°F). A distillate containing 95
mol % benzene and 5 mol % toluene and a bottoms containing 10
mol % benzene and 90 mol % toluene are to be obtained. The
reflux ratio is 4: 1.The average heat capacity of the feed is 159 .
kJ/kg mol· K (and the average latent heat 32099 kJ/kg mol.
(Equilibrium data for this system is given in Table below.
Determine
i. the kg moles per hour distillate, kg moles per hour
bottoms,
ii. The number of theoretical trays needed.
iii. The minimum no. of theoretical stages required at total
reflux
iv. Feed plate
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DEPARTMENT OF CHEMICAL AND
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 SOLUTION:
The given data are:
F = 100 kg mol/h, XF =0.45, XD = 0.95, Xw = 0.10, and R =
Ln/D = 4.
CpL = 159 . kJ/kg mol· K; λ=32099 kJ/kg mol

Overall material balance: F = D + W

100 = D + W

Component material balance: FxF = DxD + Wxw

100(0.45) = D(0.95) + (100 - D) (0.10)
D = 41.2 kg mol/h ; W = 58.8 kg rnol/h
Plot the equilibrium data on an x-y
Determination of the enriching section operating line
𝑅 𝑥𝐷 4 0.95
𝑦𝑛:1 = 𝑥 + = 𝑥 + = 0.800𝑥𝑛 + 0.190
𝑅+1 𝑛 𝑅+1 4+1 𝑛 4+1
Plot the enriching operating line on the x-y diagram starting from
y = xD = 0.95 with slope of 0.800
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 SOLUTION CONT’:
 Next, determination of the value of q

The boiling point of the feed which is at xF = 0.45, is

found by graphical method or interpolation.

 Graphical method A graph of temperature against

composition is drawn as shown below and the boiling
point temperature read from the graph

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SOLUTION CONT’:

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 SOLUTION CONT’:
Interpolation.

368.2 − 363.2
𝑇𝑏.𝑝 𝑚𝑖𝑥𝑡𝑢𝑟𝑒 𝑎𝑡 𝑥𝐹 = 368.2𝐾 − 0.411 − 0.45 = 367𝐾
0.411 − 0.581
Thus feed enters at a temperature below boiling point of mixture that’s
our feed condition is sub-cooled liquid.

𝐶𝑝,𝐿 𝑇𝑏𝑝 − 𝑇𝐹 + 𝜆
For cold feed 𝑞=
𝜆
Where Tb= 367K and Tf= 327.6K inlet feed temperature
159(367 − 327.6)
𝑞 =1+ = 1.195
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 SOLUTION CONT’:
Slope of q line is:
𝑞 1.195
= = −6.12
𝑞;1 1.195;1

 Plotted q line on the X-Y diagram starting at the point y =xF =

0.45 with a slope of 6.12.
 The stripping operating line is drawn connecting the point y = x
=xw = 0.10 with the intersection of the q line and the enriching
operating line.
 Starting at the point y = x = xD, the theoretical steps are drawn on
the x-y diagram as shown below.
 The number of theoretical steps is 8 (7.6) or 8(7.6) steps minus a
reboiler, which gives 7(6.6) theoretical trays. From graph (Red
colour)
 The feed is introduced on tray 5 from the top.

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SOLUTION CONT’:

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 REFLUX CONSIDERATIONS
R = Flow returned as Reflux/Flow of top product taken off

 The rectifying operating line slope depends on R.

 Therefore, the number of stages required for a given

separation depends on R.

 Effective reflux ratio can be greater than R if the

column is poorly insulated and may be subject to
change due to weather conditions. A well lagged
column is more consistent.

 The amount of reflux lies somewhere between the

two extremes of total reflux and minimum reflux

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 REFLUX CONSIDERATIONS
 The number of theoretical trays needed depends- upon
the operating lines. To fix the operating lines, the reflux
ratio (R= L/D) at the top of the column must be set.
 The two extremes are Total Reflux and Minimum Reflux
 Total Reflux - all condensate is returned, no product is
taken off and no feed added. This gives the minimum
number of stages to achieve the separation.
 Minimum Reflux - reducing R requires more stages to
achieve the separation. Further reduction creates a
pinch point where an infinite number of stages is
required.
 Minimum reflux happens when the intersection of the
operating lines lies on the equilibrium curve

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 TOTAL REFLUX
 One of the limiting values of total reflux ratio is that of total reflux
 All vapour is condensed and returned as liquid

 Hence, the operating lines of both sections of the column coincide

with the 45° diagonal line,

 This gives the minimum number of trays that can possibly be

used to obtain the given separation.

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 TOTAL REFLUX

Fenske eqn to calculate Nmin

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 MINIMUM REFLUX
 The minimum reflux ratio can be defined as the reflux ratio
Rm that will require an infinite number of trays for the given
separation to get desired xD and xB.
 This corresponds to the minimum vapor flow in the tower,
and hence the minimum reboiler and condenser sizes.
 If xD is remains constant, as R decreases, the slope
(R/R+1) of ROL Equation decreases, while its intercept
(xD/R+1) increases. The ROL moves closer to the
equilibrium curve as R decreases until point Q is
reached. Point Q is the point of intersection between
the q-line and the equilibrium curve.
 As a result, the number of steps required to give a fixed xD
and xB increases
 Min Reflux happens when the two operating lines intersect
on equilibrium curve (intersection point is called a pinch
point ). Thus point Q in diagram below
 Don’t forget the q line. Min reflux occurs at intersection with
equilibrium curve because all three lines should intersect.
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MINIMUM REFLUX

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 MINIMUM REFLUX
 using definition of slope of line = R/(R+1)
 Where x’, y’ is the intersection
of line with curve

 Rmin can also be

calculated (if feed is liquid
at b.p.)

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MINIMUM REFLUX

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EXAMPLE 7.1 DISTILLATION OF A MIXTURE OF BENZENE
AND TOLUENE. (SEPARATION PROCESS PRINCIPLES BY SEADER)

Four hundred and fifty lbmol/h (204 kmol/h) of a mixture

of 60 mol% benzene (LK) and 40 mol% toluene (HK) is
to be separated into a liquid distillate and a liquid
bottoms product of 95 mol% and 5 mol% benzene,
respectively. The feed enters the column with a molar
percent vaporization equal to the distillate-to-feed ratio.
Use the McCabe–Thiele method to compute, at 1 atm
(101.3 kPa):
a) N min,
b) R min, and
c) number of equilibrium stages N, for R/Rmin = 1.3,
d) the optimal feed-stage location.

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Equilibrium data:
Equilibrium Data for Benzene- Toluene System

Mole fraction of Benzene at 101.325kPa

xA yA

1.000 1.000

0.780 0.900

0.581 0.777

0.411 0.632

0.258 0.456

0.130 0.261

0 0

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 SOLUTION
Given Data:
F = 204 kmol/h; xF = 0.6; xD = 0.95; xw = 0.05

Material balance
overall mass balance: F = D +W
204 = D + W……………1

Component material balance: FxF = DxD + Wxw

204(0.6) = D(0.95) + (W) (0.05)…………..2

Combining equations 1and 2 gives

204(0.6) = D(0.95) + (204 - D) (0.05) ………….3

Solving equation 3 and substituting the value of D in equation 1

gives
D = 124.66 Kmol/h; W= 79.34Kmol/h
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 𝐷 124.66
Molar vaporization of the feed = = = 0.611
𝐹 204

𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑙𝑖𝑞𝑢𝑖𝑑 𝑖𝑛 𝑓𝑒𝑒𝑑 𝐿𝐹 𝐹 − 𝑉𝐹 𝑉𝐹

𝑞= = = =1−
𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑓𝑒𝑒𝑑 𝐹 𝐹 𝐹

= 1 − 0.611 = 0.389

𝑞 0.389
The slope of the q-line is: = = −0.637
𝑞;1 0.389;1

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Draw x-y diagram using Equilibrium data given

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(a) Determination of minimum number of stages Figure below
shows the plot for total reflux that gives Nmin ,where y and x refer to
benzene, xD = 0.95 and xB =0.05, the minimum stages are stepped
off between the equilibrium curve and the 450 line, giving Nmin = 7.

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(b) In Figure below a q-line is drawn that has a slope of - 0.637 and
passes through the feed composition (xF=0.60) on the 45oline.
For Rmin, an operating line for the rectifying section passes through
the point x = xD =0.95 on the 45o line and through the point of
intersection of the q-line and the equilibrium curve (y =0.684, x =
0.465).

The slope of this operating line is 0.55, which equals to

R𝑚𝑖𝑛 . DEPARTMENT OF CHEMICAL AND
R 𝑚𝑖𝑛 = R
Therefore, R 𝑚𝑖𝑛 = 1.22 PROCESS SYSTEM ENGINEERING/
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( c ) The operating reflux ratio is 1.3Rmin = 1.3(1.22) = 1.59. the
Rectifying section operating-line slope is
𝑅 1.59
𝑠𝑙𝑜𝑝𝑒(𝑅𝑂𝐿 ) = = = 0.614
𝑅+1 1.59 + 1

Rectifying section operating-line and the q-line are drawn in

figure below. Stripping section operating line is obtained by
joining point x=xW =0.05 on the 45o line and through the
intersection of the q-line with the rectifying-section operating
line.

The equilibrium stages are stepped off, first, between the

rectifying-section operating line and the equilibrium
Curve, and then between the stripping-section operating line
and the equilibrium curve, starting from point A (distillate
composition) and finishing at point B (bottoms composition).

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 No of equilibrium stages N = 13.2, The
bottom stage is the partial reboiler,
leaving 12.2 equilibrium stages in the DEPARTMENT OF CHEMICAL AND
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 For the optimal feed stage, is found at the transfer from the
rectifying-section operating line to the stripping-section operating
line and this takes place at point P. The feed going into stage 7
from the top.
 If the plate efficiency were 0.8, 16 trays would be needed

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 OPTIMUM REFLUX RATIO
 Increase R
 Diameter (D) gets bigger  No. of Plates gets
 Since D = fn(V, L) smaller

 Heat exchangers get bigger

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 REFLUX AND COST
 A trade off between operating cost and capital
cost is needed.

 Increase R --- Less stages, less capital cost

BUT also ---More boiling and condensing

 Decrease R --- More stages, More capital cost

BUT also -- Less boiling and condensing

 Capital and operating costs combine to give a

total cost. This is minimised with the following

 Rule of thumb: R = 1.2 to 1.5 times Rmin

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RECTIFICATION TOWER WITH SIDE STREAM.
 In certain situations, intermediate product or side streams
are removed from sections of the tower between the
distillate and the bottoms.

 The side stream may be vapor or liquid and may be

removed at a point above the feed entrance or below
depending on the Composition desired.

 The top enriching operating line above the liquid side

stream and the stripping operating line below the feed are
found in the usual way.

 The equation of the q line is also unaffected by the side

stream and is found as before.
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 RECTIFICATION TOWER WITH SIDE STREAM
Mass Balance
 Total balance on the tower
𝐹 =𝐷+𝐵+𝑂
Component balance
𝐹𝑥𝐹 = 𝐵𝑥𝐵 + 𝑂𝑥𝑜 + 𝐷𝑥𝐷

 The liquid side stream alters the liquid

rate below it, and hence the material balance
or operating line in the middle portion
between the feed and liquid side stream plates.
Rectification Tower With Side Stream Total
material balance on the top portion of the
tower: 𝑉𝑠:1 = 𝐿𝑠 + 𝑂 + 𝐷
 Solving for ys+1 , the operating
where O is mol/h saturated liquid removed as a
line for the region between the
side stream
side stream and the feed is
 Since the liquid side stream is saturated, 𝐿𝑠 𝑂𝑥𝑜 + 𝐷𝑥𝐷
𝑉𝑠:1 = 𝑉𝑛:1 and 𝐿𝑛 = 𝐿𝑠 + 𝑂 𝑦𝑠:1 = 𝑥 +
𝑉𝑆:1 𝑠 𝑉𝑠:1

 Balance on the MVC (A) DEPARTMENT OF CHEMICAL AND

𝑉𝑠:1 𝑦𝑠:1 = 𝐿𝑠 𝑥𝑠 + 𝑂𝑥𝑜 + 𝐷𝑥𝐷 PROCESS SYSTEM ENGINEERING/
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 The line can be located
by the q line, which
determines the
intersection of the
stripping line and
operating line of the side
stream, or it may be fixed
by the intersection of the
side stream line and the
enriching section
operating line at xo.

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 PARTIAL CONDENSERS
 In some cases it may be required to remove the overhead
distillate product as a vapour instead of a liquid.
 In the normal distillation, the condenser used in the operation is
a total condenser, at which all vapour from the top of the column
is condensed to liquid.
 A Partial condenser condenses only a fraction of vapour from
the top of the column.
 The liquid condensate in a partial condenser is returned to the
tower as reflux and the vapour removed as product.
 There is an equilibrium between vapour (distillate: D, with the
concentration of xD ) and liquid (reflux: LR , with the
concentration of xR) at the condenser. Thus
o The concentration of the distillate (yD ) is no longer equal to the
concentration of the reflux (xR) ,
o But xR can be read from the equilibrium curve when yD is known
o The partial condenser is considered an additional equilibrium stage

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PARTIAL CONDENSERS

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PONCHON AND SAVARIT
METHOD

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 INTRODUCTION
 PONCHON AND SAVARIT METHOD is a graphical
method for binary non-ideal system, which is used when
the molar latent heat is no longer constant and there
is a substantial heat of mixing.

 This method is much more tedious, and based on the use

of an enthalpy-composition chart.

 An enthalpy-concentration diagram for a binary vapour-

liquid mixture of A and B takes into account latent heats,
heats of solution or mixing, and sensible heats of the
components of the mixture
 It is necessary to construct an enthalpy-composition
diagram for particular binary system over a temperature
range covering the two-phase vapour-liquid region at the
pressure of the distillation

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 ENTHALPY-COMPOSITION DIAGRAM
 The saturated liquid
enthalpy is:

 The saturated vapour

enthalpy is

 where ΔHVAb and ΔHVBb are the

latent heat values of pure A and
pure B at the normal boiling
point TbA and TbB , respectively.

 That is, the liquid is first changed from temperature

T0 to Tb and then evaporated at Tb , the vapor
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ENTHALPY-COMPOSITION DIAGRAM
 If an amount Q of heat is added to a mass mA 𝑄
𝐻𝐴 + = 𝐻𝑐
of a phase, the increase in enthalpy from HA to 𝑚𝐴
HC will be given by:

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 Example
Devise an enthalpy-concentration diagram for the Benzene-Toluene
system at 760 mm Hg, assuming zero heat of mixing.

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SOLUTION

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Solution Cont’

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Solution Cont’

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 CONTINUOUS DISTILLATION COLUMN
Figure below represents a continuous
distillation unit operating with a feed F of
composition xf , and giving a top product
D of composition xD and a bottom product
B of composition xB.

Let’s consider loop I enriching section,

material balance s for the section are
Total material balance:

𝑉𝑛 − 𝐿𝑛:1 = 𝐷 ……………..2.4.1

Component balance:
𝑉𝑛 𝑦𝑛 − 𝐿𝑛:1 𝑥𝑛:1 = 𝐷𝑥𝐷 ……….….2.4.2

The left hand side net flow upwards of the more volatile component. Since for a
given distillation the right-hand side is constant it follows that the difference or net
rate of flow upward is constant, independent of tray number in
this section of tower and equal to that
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 Enthalpy balance:
𝑉𝑛 𝐻𝑉𝑛 + 𝐿𝑛:1 𝐻𝐿𝑛:1 = 𝑄𝐶 + 𝐷𝐻𝐷 ……….2.4.3
𝑄𝐶
𝑉𝑛 𝐻𝑉𝑛 − 𝐿𝑛:1 𝐻𝐿𝑛:1 = 𝐷 + 𝐻𝐷 ……..2.4.4
𝐷
𝑄𝐶
Let , 𝑄′ = + 𝐻𝐷 ……………….2.4.5
𝐷
𝑉𝑛 𝐻𝑉𝑛 − 𝐿𝑛:1 𝐻𝐿𝑛:1 = 𝐷𝑄′ ……….2.4.6
Left-hand side is the net flow of heat upward. Since for a given distillation the right-
hand side is constant it follows that the difference or net rate of flow of heat upward is
constant, independent of tray number in this section of tower and equal to that
permanently taken out at the top with distillate and at condenser.

Elimination of D between Eqs. 2.41 and 2.4.2 and between 2.4.1 and
2.4.6 yields
𝐿𝑛+1 𝑥𝐷 ;𝑦𝑛 𝑄′ ;𝐻𝑉𝑛
= = …………………………..2.4.7
𝐷 𝑦𝑛 ;𝑥𝑛+1 𝐻𝑉𝑛 ;𝐻𝐿𝑛+1
A stream ∆𝐷 may be defined with mass equal to the difference between
the vapour and liquid streams between two plates and it has composition
𝑥𝐷 and enthalpy 𝑄′ . Then the three quantities
𝑉𝑛 ,𝐿𝑛:1 , and 𝑄′ on a straight line passing through
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 Loop II
 Below the feed plate a similar series of equations for material
and heat balance can be written
Total material balance:
𝐿𝑚:1 − 𝑉𝑚 = 𝐵 ……………………..2.4.8
𝐿𝑚:1 𝑥𝑚:1 − 𝑉𝑚 𝑦𝑚 = 𝐵𝑥𝐵 ………….2.4.9
𝐿𝑚:1 𝐻𝐿𝑚:1 − 𝑉𝑚 𝐻𝑉𝑚 = 𝐵𝐻𝐵 − 𝑄𝐵 ……..2.4.10
𝑄𝐵
𝐿𝑚:1 𝐻𝐿𝑚:1 − 𝑉𝑚 𝐻𝑉𝑚 = 𝐵 𝐻𝐵 − …….2.4.11
𝐵
′ 𝑄𝐵
Let , 𝑄 ′ = 𝐻𝐵 − ……….….2.4.12
𝐵
𝐿𝑚:1 𝐻𝐿𝑚:1 − 𝑉𝑚 𝐻𝑉𝑚 = 𝐵𝑄 ′′ ………2.4.13
𝐿𝑚+1 ;𝑥𝐵 : 𝑦𝑚 ;𝑄 ′′ : 𝐻𝑉𝑚
= = ……..2.4.14
𝐵 𝑦𝑚 ; 𝑥𝑚+1 𝐻𝑉𝑚 ;𝐻𝐿𝑚+1
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Eqn. 2.4.14 represents any operating line below the
feed plate, and shows that all such lines pass through
a common pole ΔB of coordinates xB and 𝑄′′ . As with
the rectifying section a stream
ΔB may be defined by mass 𝐿𝑚:1 − 𝑉𝑚 and its
composition xB and enthalpy𝑄′′ .
Then
𝐹 = ∆𝐷 + ∆𝐵 …………………………..2.4.15
𝐹𝑥𝐹 = ∆𝐷 𝑥𝐷 + ∆𝐵 𝑥𝐵 …………………2.4.16

Thus it follows that 𝐹, ∆𝐷 , 𝑎𝑛𝑑 ∆𝐵 will be on a straight

line on the H-xy chart as shown below.

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DEPARTMENT OF CHEMICAL AND
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PLATE TO PLATE GRAPHICAL PROCEDURE FOR
DETERMINING THE NUMBER OF EQUILIBRIUM STAGES
1. Draw the equilibrium curve and the enthalpy concentration
diagram for the mixture to be separated
2. Determine the composition of the feed, distillate and bottom
products. Locate these compositions on the enthalpy-
concentration diagram.
3. Locate the point F with coordinates (HF, xF) and
4. Locate the pole ∆𝐷 at point (xD, Q’) or use (R, xD)
𝑄
5. where, 𝑄 ′ = 𝐶 + 𝐻𝐷
𝐷
6. Pole ∆𝐵 is located as an extension of F∆𝐷 line cutting the ordinate
at xB in ∆𝐵 .
7. The condition of the vapour leaving the top plate is shown at V1
on the dew-point curve with abscissa xD. The condition of the
liquid on the top plate is then found by drawing the tie line T1 from
V1 to L1on the boiling curve.
8. The condition V2 of the vapour on the second plate is found, by
drawing L∆𝐷 to cut the dew-point curve on V2. L2 is then found on
the tie line T2.
9. The conditions of vapour and liquid V3, V4, V5, V6 and L3, L4, L5
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PLATE TO PLATE GRAPHICAL PROCEDURE FOR
DETERMINING THE NUMBER OF EQUILIBRIUM STAGES
 Tie line T6 gives L6, which has the composition below that of
the feed.
 When an equilibrium tie line crosses the line connecting the
difference points through the feed condition the other
difference point is used to complete the construction.
 After the feed point, points V on the vapour curve are
located by drawing lines between the ∆𝐵 point and point
L6 on the boiling curve
 V7 is then found using the line∆𝐵 𝐿6 𝑉7 , as this represents the
vapour on the top plate of the stripping section. L7, L8, L9,
L10 and V8, V9, V10, V11 are then found by a similar
construction. L10 has the required composition of the
bottoms, xw.
 Alternatively, calculations may start with the feed condition
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TOTAL REFLUX

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MINIMUM REFLUX

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EXAMPLE

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SOLUTION

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SOLUTION CONT’

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SOLUTION CONT’

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SOLUTION CONT’

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SOLUTION CONT’

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SOLUTION CONT’

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 PROBLEM 2
A feed containing 40 mole percent n-hexane and 60 percent n-octane is fed
to a distillation column. A reflux ratio of 1.2 is maintained. The overhead
product is 95 percent hexane and the bottoms 10 percent hexane. Find the
number of theoretical stages and the optimum feed stage. Assume that a
total condenser is used. The column is to operate at 1 atm.
Equilibrium data is collected.
VLE Data, Mole Fraction Hexane, 1 atm
x (liquid) 0.0 0.1 0.3 0.5 0.55 0.7 1.0
y (vapor) 0.0 0.36 0.70 0.85 0.90 0.95 1.0
Enthalpy-Concentration Data
Mole Fraction Hexane Enthalpy cal/gmol
Sat. Liquid Sat. Vapor
0.0 7000 15,700
0.1 6300 15,400
0.3 5000 14,700
0.5 4100 13,900
0.7 3400 12,900
0.9 3100 11,600
1.0 3000 10,000
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 PROBLEM 2
1000 kg/hr of a mixture containing 42 mole percent heptane and 58 mole
percent ethyl benzene is to be fractionated to a distillate containing 97
mole percent heptane and a residue containing 99 mole percent ethyl
benzene using a total condenser and feed at its saturated liquid
condition. The enthalpy-concentration data for the heptane-ethyl
benzene at 1 atm pressure are as follows:
xheptane 0 0.08 0.18 0.25 0.49 0.65 0.79 0.91 1.0

yheptane 0 0.28 0.43 0.51 0.73 0.83 0.90 0.96 1.0

Hl (kJ/kmol) x 10-3 24.3 24.1 23.2 22.8 22.05 21.75 21.7 21.6 21.4

Hv (kJ/kmol) x 10-3 61.2 59.6 58.5 58.1 56.5 55.2 54.4 53.8 53.3

Calculate the following:

a. Minimum reflux ratio
b. Minimum number of stages at total reflux
c. Number of stages at reflux ratio of 2.5
d. Condenser duty
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e. Reboiler duty HIT/ HARARE 131
TYPES OF TRAY EFFICIENCIES

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 PLATE EFFICIENCY
 For an equilibrium tray, the vapor and liquid leaving the tray
are in thermodynamic equilibrium.

 In a actual tray, equilibrium will rarely be attained.

 The no. of equilibrium stages must be converted to a

number of actual real plates.

 Tray efficiencies can be defined in several ways, the overall

tray efficiency, Eo is defined as:
𝑁𝑜. 𝑜𝑓 𝑡𝑕𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑡𝑟𝑎𝑦𝑠
𝐸0 =
𝑁𝑜 𝑜𝑓 𝑎𝑐𝑡𝑢𝑎𝑙 𝑡𝑟𝑎𝑦𝑠
 For example, if eight theoretical steps are needed and the overall
efficiency is 60%, the number of theoretical trays is eight minus a
reboiler, or seven trays. The actual number of trays is 7/0.60 or
11.7 trays
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 OVERALL EFFICIENCY
 It is applied for the whole column.
 Every tray is assumed to have the same efficiency.
 The overall efficiency depends on the
 Geometry and design of the contacting trays,
 Flow rates and flow paths of vapor and liquid streams,
 Compositions and properties of vapor and liquid streams.

 Typical values for tray efficiency are 0.5 to 0.75, i.e. they are
0.5 to 0.75 times as effective as an ideal stage.
 Divide the number of ideal stages by the efficiency, add 10%
extra trays.
 The overall efficiency is extremely easy to measure and use;
thus, it is the most commonly used efficiency value in the
plant.
 However, the overall efficiency is not representative of
column operation because the different compositions on the
various trays result in different tray efficiencies.

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 OVERALL EFFICIENCY
 The overall efficiency can be also calculated from the following
correlations:

i. The Drickamer-Bradford empirical correlation:

𝐸0 = 13.3 − 66.8log(𝜇)
The correlation is valid for hydrocarbon mixtures in the range of 342
K< T < 488.5K, 1 atm< P < 25 atm and 0.066<µ<0.355 cP .

ii. The O’Connell correction: Add 10% extra trays

𝐸0 = 50.3 ∝ 𝜇 ;0.226

iii. Another equation can be also used:

𝐸0 = 0.52782 − 0.27511 log10 ∝ 𝜇 + 0.044923 log10 𝛼𝜇 2
Where 𝛼- relative volatility of key components and 𝜇 – viscosity of
feed in cP
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MURPHREE EFFICIENCY

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MURPHREE EFFICIENCY

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MURPHREE EFFICIENCY

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PACKED DISTILLATION
COLUMN

References

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 PACKED COLUMNS: Introduction
 Packed columns are used for smaller diameter columns
since it is expensive to build a staged column that will
operate properly in small diameters.

 Packed columns are definitely more economical for

columns less than 2.5 feet(0.762m) in diameter.

 In larger packed columns the liquid may tend to

channel, and without careful design randomly packed
towers may not operate very well; in many cases large-
diameter staged columns are cheaper.

 Packed towers have the advantage of a smaller

pressure drop and are therefore useful in vacuum
fractionation.
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 PACKED COLUMNS: Introduction
In designing a packed tower, the choice of packing
material is based on economic considerations.

A wide variety of packings including random and

structured are available. Once the packing has been
chosen it is necessary to know the column diameter
and the height of packing needed.

The column diameter is sized on the basis of either the

approach to flooding or the acceptable pressure drop.

Packing height can be found either from an equilibrium

stage analysis or from mass transfer considerations.

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TYPES OF COLUMN PACKING:

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Determination of the column height
1. The theoretical stage method
2. The transfer unit method

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 THE THEORETICAL STAGE METHOD (HETP)
 If at a point of the distillation column the concentration of the liquid flow
is x, and the concentration of the counter-current vapor flow at the same
point is y, then there is a height above this point where the concentration
of the vapor flow (y*) is in equilibrium with x.
 This section is the Height Equivalent a Theoretical Plate (HETP).

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THE THEORETICAL STAGE METHOD (HETP)

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HTU METHOD FOR DISTILLATION
 In the HTU method, stages are not stepped off on a
McCabe–Thiele diagram. Instead, the diagram
provides data to perform an integration over the
packed height using mass-transfer coefficients or
transfer units.

 Consider the packed distillation column and its

McCabe–Thiele diagram in Figure below.

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DEPARTMENT OF CHEMICAL AND
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 Assume that V; L;𝑉𝑎𝑛𝐿𝑑, and L are constant. For
equimolar countercurrent diffusion (EMD), the rate of
mass transfer of the more volatile component from the
liquid to the vapor phase is
𝑛 = 𝑘𝑥 𝑎 𝑥 − 𝑥1 = 𝑘𝑦 𝑎 𝑦1 − 𝑦

𝑘𝑥 𝑎 𝑦1 ;𝑦
 Rearranging − =
𝑘𝑦 𝑎 𝑥1 ;𝑥

 In Figure packed distillation column (b), for any point (x,

y) on the operating line, the interfacial point (x1, y1) on
the equilibrium curve is obtained by drawing a line of
slope (kxa=kya) from point (x, y) to the point where it
intersects the equilibrium curve.

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Material balance over an incremental column
height, h with constant molar overflow:
𝑉𝑑𝑦 = 𝑘𝑦 𝑎 𝑦1 − 𝑦 𝑠𝑑𝑕 Where s is the cross- sectional area
over an incremental column height, h
L𝑑𝑥 = 𝑘𝑥 𝑎 𝑥 − 𝑥1 𝑠𝑑𝑕 with constant molar overflow
Integrating over the rectifying section
𝑦2 𝑥𝐷
𝑉𝑑𝑦 𝑉𝑑𝑦
𝑕𝑅 = 𝑑𝑕 = =
𝑦𝐹 𝑘𝑦 𝑎𝑆 𝑦1 − 𝑦 𝑥𝐹 𝑘𝑥 𝑎𝑆 𝑥 − 𝑥1
𝑦2 𝑥𝐷
𝐻𝐺 𝑑𝑦 𝐻𝐿 𝑑𝑦
𝑕𝑅 = 𝑑𝑕 = =
𝑦𝐹 𝑦1 − 𝑦 𝑥𝐹 𝑥 − 𝑥1
Integrating over the stripping section
𝑦𝐹 𝑥𝐹
𝑉𝑑𝑦 𝑉𝑑𝑦
𝑕𝑆 = 𝑑𝑕 = =
𝑦1 𝑘𝑦 𝑎𝑆 𝑦1 − 𝑦 𝑥1 𝑘𝑥 𝑎𝑆 𝑥 − 𝑥1
𝑦𝐹 𝑥𝐹
𝐻𝐺 𝑑𝑦 𝐻𝐿 𝑑𝑦
𝑕𝑅 = 𝑑𝑕 = =
𝑦1 𝑦1 − 𝑦 𝑥1 𝑥 − 𝑥1
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 Values of ky and kx vary over the packed height,
causing the slope (kxa/kya) to vary.

 If kxa > kya, resistance to mass transfer resides mainly

in the vapor and, in using
yF HG dy xF HL dy
hR = dh = y = x
1 y1 ;y 1 x;x1
it is most accurate to evaluate the integrals in y.

 For kya > kxa, the integrals in x are used. Usually, it is

sufficient to evaluate ky and kx at three points in each
section to determine their variation with x.

 These integrals can be evaluated

either graphically or numerically.

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 APPROXIMATE COLUMN SIZING
An approximate estimate of the overall column size can be made
once the number of real stages required for the separation is
known. This is often needed to make a rough estimate of the
capital cost for project evaluation.

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 Column Height
The height of a trayed column is calculated by multiplying the
number of (actual) stages by the tray separation.

Height of a trayed column

= Number of actual stages required by separation
∗ tray spacing

The most common tray spacing is 24 inches -- it allows enough

space to work on the trays whenever the column is big enough
around (>5 ft diameter) that workers must crawl inside. Smaller
diameter columns may be able to get by with 18 inch tray spacings.

In addition to the space occupied by the trays, height is needed at

the top and bottom of the column. Space at the top -- typically an
additional 5 to 10 ft -- is needed to allow for disengaging space.

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 Column Height
The bottom of the tower must be tall enough to serve as a liquid
reservoir. Depending on your boss's feelings about keeping
inventory in the column, you will probably design the base for about
5 minutes of holdup, so that the total material entering the base can
be contained for at least 5 minutes before reaching the bottom tray.

The total of height added to the top and bottom will usually amount
to about 15% or so added to that required by the trays.

You rarely will see a real tower that is more than about 175 ft. tall.
Tall, skinny towers are not a good idea, so watch the
height/diameter ratio.

You generally want to keep it less than 20 or 30. If your tower ends
up exceeding these values, you probably want to look at a redesign,
maybe by reducing the tray spacing, or splitting the tower into two
parts.
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 Diameter of tray towers
The flooding condition fixes the upper limit of vapour
velocity. A high vapour velocity is needed for high plate
efficiencies, and the velocity will normally be between 70
to 90 per cent of that which would cause flooding.
For design, a value of 80 to 85 per cent of the flooding
velocity should be used. The flooding velocity can be
estimated from the correlation given by Fair (1961):

𝜍 0.2 𝜌𝐿 − 𝜌𝑉
𝑢𝑓𝑙𝑜𝑜𝑑𝑖𝑛𝑔 = 𝐾𝑉
20 𝜌𝑉

The equation holds for non-foaming system..

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 4𝑉𝑚𝑎𝑠𝑠
𝐷𝑇 =
𝐴𝑑
𝑢𝑓𝑙𝑜𝑜𝑑𝑖𝑛𝑔 𝑓𝑑𝑒𝑠𝑖𝑔𝑛 𝜋𝜌𝑣 1 − 𝐴

𝑓𝑑𝑒𝑠𝑖𝑔𝑛 - fraction of flooding velocity; 𝑉𝑚𝑎𝑠𝑠 - vapour mass flow rate

Trays probably aren't a good idea for columns less than about 1.5 ft in
diameter (you can't work on them) -- these are normally packed.
Packing is less desirable for large diameter columns (over about 5 ft in
diameter).

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 STUDY QUESTIONS
1. What equipment is included in a typical distillation operation?
2. What determines the operating pressure of a distillation column?
3. Under what conditions does a distillation column have to operate under vacuum?
4. Why are distillation columns arranged for counter-current flow of liquid and vapour?
5. Why is the McCabe–Thiele graphical method useful in this era of more rigorous,
computer-aided algebraic methods used in process simulators?
6. Under what conditions does the McCabe–Thiele assumption of constant molar overflow
hold?
7. In the McCabe–Thiele method, between which two lines is the staircase constructed?
8. What is meant by the reflux ratio? What is meant by the boil-up ratio?
9. What is the q-line and how is it related to the feed condition?
10. What are the five possible feed conditions?
11. In the McCabe–Thiele method, are the stages stepped off from the top down or the
bottom up? In either case, when is it best, during the stepping, to switch from one
operating line to the other? Why?
12. Can a column be operated at total reflux? How?
13. How many stages are necessary for operation at minimum reflux ratio?
14. What is meant by a pinch point? Is it always located at the feed stage?
15. What is meant by sub-cooled reflux? How does it affect the amount of reflux inside the
column?
16. Is it worthwhile to preheat the feed to a distillation column?
17. Why is the stage efficiency in distillation higher than that in absorption?
18. What kind of a small laboratory column is useful for obtaining plate efficiency data?

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