M.Sc.

Abdulrazzaq Saeed Distillation

Chapter Two Gas – Liquid Contacting Equipment

2.1Introduction

In previous Chapter we discussed the basic principles of diffusion and mass transfer in
a single phase or at a phase boundary. Equipment and devices for interphase mass
transfer can be broadly classified into the following categories:
1. Gas–liquid or vapour–liquid contacting (gas absorption and stripping,
distillation, humidification or dehumidification and water cooling)
2. Liquid–liquid contacting (solvent extraction)
3. Gas–solid contacting (drying and adsorption)
4. Liquid–solid contacting (leaching, crystallization and ion exchange).
A variety of gas–liquid contacting equipment is in use. In some of these, the gas is
dispersed in the liquid in the form of bubbles (for example, tray towers, bubble
columns, and agitated vessels); in some others the liquid is dispersed in the form of
droplets or discontinuous films in a continuous gas phase (for example, spray towers,
packed towers, and venturi scrubbers). Sometimes both gas and liquid phases are
continuous (for example, a ‘falling film contactor’ which is used for certain gas–
liquid reactions). Tray and packed columns are most widely used for gas–liquid
contacting — namely for gas absorption, stripping, distillation, and liquid–liquid
extraction.
2.2Tray or Plate Column

A tray column primarily consists of a vertical cylindrical shell and a set of ‘tower
internals’ that include (i) trays or plates on which the gas–liquid contact occurs, (ii)
arrangements for flow of the liquid from one tray to the lower one through the
downcomer, and (iii) inlet and outlet nozzles for the two phases. Figure 5.1
schematically shows a few essential parts of a ‘sieve tray’ column.

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M.Sc. Abdulrazzaq Saeed Distillation

24
M.Sc. Abdulrazzaq Saeed Distillation

2.2.1The Tray

A ‘tray’ has two major functions:

1. It allows the gas to flow through the holes or passages; the gas vigorously bubbles
through the liquid to form a ‘gas–liquid dispersion’. The tray holds the dispersion
on it.
2. The trays separate the column into a number of compartments each of which
constitutes a stage. Mass transfer between the phases occurs on a tray. Therefore, the
trays as a whole constitute the heart of a column. The performance of a column
depends upon the performance of the trays.
Trays are also called ‘plates’. There are quite a few types of trays in use. The
bubble-cap tray will be described first.
The bubble-cap tray
This is the oldest type of tray and is still in commercial use. A bubble cap consists of
two major components—a bell-shaped ‘cap’ and a ‘riser’ (also called a ‘
chimney’). Figure 5.2(a) and (b) shows a typical bubble-cap design. The riser is
inserted through a hole on the tray floor (or deck) and the bell shaped cap is bolted to
it. A ring gasket (not shown) is used below the nut. The riser or chimney is a
piece of tube with a flared or expanded bottom end (there are other designs too). In
fact, the riser acts as the vapour passage and also holds the cap.
The caps and the risers are made of low carbon steel, stainless steel or any other
suitable material that can withstand the environment within the tower. Caps are
arranged on a tray on equilateral triangular pitch with rows normal to the direction
of liquid flow. Bubble caps generally range from 1 inch to 6 inches in diameter.

25
 M.Sc. Abdulrazzaq Saeed Distillation

2.2.2Downcomers and Weirs

The ‘downcomer’ is a passage through which the liquid flows down from one
tray to the next below (Figures 5.1 and 5.3). The desired depth of the gas–liquid
dispersion is maintained on a tray by using a ‘weir’ in the form of a vertical plate
The lower edge of the downcomer plate should remain dipped into the liquid on
the lower tray maintaining a clearance, (called ‘downcomer clearance’) of ½ to 1
inch from the tray floor. This makes a ‘downcomer seal’ [also shown in Figure
5.5(b) as D.S.] prevent ‘short-circuiting’of some of the gas through the
downcomer. The weir length may vary from 60 to 80% of the tower diameter; the
downcomer area (on one side) correspondingly varies from 5 to 15% of the tray
area. A weir height of 1 to 2 inches is generally maintained.

2.2.3Nozzles

A tower for contacting a liquid and a vapour (or a gas) should be provided with a
few nozzles for feed entry (both gas and liquid), entry of reflux at the top and of the
reboiler vapour return at the bottom (in a distillation column), and for product
withdrawal from the tower.

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M.Sc. Abdulrazzaq Saeed Distillation

2.3The Packed Tower

A packed tower is a continuous contact

equipment widely used for gas absorption,
distillation and liquid– liquid extraction. It consists
of a cylindrical shell filled with a suitable packing
material to provide a large interfacial area of
contact between the phases. A set of ‘tower
internals’ such as packing support, liquid and gas
distributors and redistributors, demister, etc. are
fitted into the tower .The liquid is distributed at
the top of the packing and trickles down through
the bed. The gas (or the vapour) is fed at the
bottom. It flows up through the void spaces of the
bed and comes in intimate contact with the liquid
flowing down the packing surface as a film. The
packing material is held on a support plate having
provisions for gas distribution at and liquid
discharge from the bottom of the packed section.

27
M.Sc. Abdulrazzaq Saeed Distillation

The sketch of a packed tower is shown in Figure 5.19. The details of its construction
and operation are given below.
2.3.1Packing

A variety of packings differing in shape, size and performance are available. These
may be classified into three categories: (i) random or dumped packings, (ii)
structured packings, and (iii) grid packings. Random packings are just dumped into
the shell to give the packing pieces a random orientation. Structured packings are
stacked in the shell to take the shape of a packed bed.
Characteristics of Tower Packings
Besides low cost, the desirable characteristics of packings are described below
(a) A large surface area.
(b) Uniform flow of the gas and the liquid.
(c) Void volume.
(d) Mechanical strength.
(e) Fouling resistance.
Types of tower packings
Tower packings are made of ceramics, metals or plastics. Several innovations in the
design of tower packings took place in the last quarter of the twentieth century and
the process is continuing

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 M.Sc. Abdulrazzaq Saeed Distillation

Distillation

3.1Introduction

is the technique of preferential separation of the more volatile component from less
volatile one in a feed solution by partial vaporization of the feed followed by
condensation.
Volatility: is the ratio of the partial pressure to the mole fraction in the liquid
Relative Volatility: is the defined as the concentration ratio of A to B in the vapor
divided by the same ratio in the liquid phase.

Binary Mixture : A mixture involving two components.

Miltucomponents Mixture: A mixture having more than two components.

Vapour–Liquid Equilibria (VLE) The relationship between a liquid and its

vapour at equilibrium. At a given temperature and pressure, the composition of the
vapour will be determined by the composition of the liquid.

Raoult’s law : A law that states that the partial pressure exerted by each component
in an ideal liquid mixture is the product of the vapour pressure of each component
and its mole fraction at the temperature of the liquid.

Equilibrium Curve–shows the relationship between composition of residual liquid

and vapor that are in dynamic phase equilibrium .This curve will be very useful in
calculations to predict the number of the ideal stages required for a specified
distillation process.
Azeotropic Mixture : A mixture of liquids that has a constant boiling point because
the vapour has the same composition as the liquid mixture( Example ethanol–water
mixture)

3.2Parts of Distillation Column

The most important parts of a distillation unit as illustrated in Figure 7.1 are:
(a) a column having trays or a packing and Suitable internals , (b) a reboiler, and (c) a
condenser.

29
 M.Sc. Abdulrazzaq Saeed Distillation

The feed enters at a suitable point of the tower. The reboiler, normally heated by
steam, partially vaporizes the liquid received from the bottom of the column.

The vapour flows up through the trays or through the packing in the column, leaves
at the top and enters into an overhead condenser. A part of the condensate is
withdrawn as the top product and the rest is fed back into the column as reflux
which flows down the trays or the packing. An intimate contact between the down
flowing liquid and the up flowing vapour occurs on the trays or on the packing
surface. Exchange of mass takes place between the liquid and the vapour phases. The
more volatile components move from the liquid to the vapour phase and the less
volatiles move in the reverse direction—from the vapour to the liquid phase
3.3Functions of Distillation

1. Separation of products from a mixture. For example: separation of aniline and

nitrobenzene in the process of manufacture of aniline.

2. Recovery of products. For example: recovery of ethanol from its solution in

water in the process of manufacture of alcohol.

3. Increasing the purity of a product. For example: drying of commercial

benzene for the removal of traces of water present in it.

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 M.Sc. Abdulrazzaq Saeed Distillation

3.4Partial Vaporisation and Partial Condensation

If a mixture of benzene and toluene is heated in a vessel, closed in such a way that the
pressure remains atmospheric and no material can escape and the mole fraction of the
more volatile component in the liquid, that is benzene, is plotted as abscissa, and the
temperature at which the mixture boils as ordinate, then the boiling curve is obtained
as shown by ABCJ in Figure 11.5.
If a mixture of composition x2 is
at a temperature T3 below its
boiling point, T2, as shown by
point G on the diagram, then on
heating at constant pressure the
following changes will occur:
(a) When the temperature
reaches T2, the liquid will boil,
as shown by point B, and some
vapour of composition y2,
shown by point E, is formed.
(b) On further heating the
composition of the liquid will change because of the loss
of the more volatile component to the vapour and the boiling point will therefore
rise to some temperature T’. At this temperature the liquid will have a composition
represented by point L, and the vapour a composition represented by point N.
Since no material is lost from the system, there will be a change in the proportion of
liquid to vapour, where the ratio is:

(c) On further heating to a temperature T1, all of the liquid is vaporised to give
vapour D of the same composition y1 as the original liquid.
It may be seen that partial vaporisation of the liquid gives a vapour richer in the more
volatile component than the liquid. If the vapour initially formed, as for instance at
point E, is at once removed by condensation, then a liquid of composition x 3 is
obtained, represented by point C. The step BEC may be regarded as representing an
ideal stage, since the liquid passes from composition x2 to a liquid of composition x3,
31
 M.Sc. Abdulrazzaq Saeed Distillation

which represents a greater enrichment in the more volatile component than can be
obtained by any other single stage of vaporisation.
Starting with superheated vapour represented by point H, on cooling to D
condensation commences, and the first drop of liquid has a composition K. Further
cooling to T’ gives liquid L and vapour N. Thus, partial condensation brings about
enrichment of the vapour in the more volatile component in the same manner as
partial vaporisation. The industrial distillation column is, in essence, a series of units
in which these two processes of partial vaporisation and partial condensation are
effected simultaneously.
3.5Raoult’s laws

If xA is the mole fraction of A in the binary solution, that of B is (1 – x A)

v
P =x P

A AA

v
P = (1 − x )P

B A B

v v
P=P+P=x P + (1 − x )P
A
A B AA B

v
P−P
B

xA = v
Pv −P

A B

Here PAand PB are the equilibrium partial pressures of A and B in the vapour; PAv and
v
P are the vapour pressures of A and B at the given temperature. The mole fraction of A in the vapour (y A) is given by
B

P x Pv

A A A

y = =

P P

Equation above can be used to calculate the vapour–liquid equilibrium data ( x–y)
for an ideal binary mixture.

3.6Relative Volatility

Relative volatility of a component A in a mixture indicates the ease of its separation

from another component B.
y ⁄(1 − y ) AB
α = A A xA⁄( 1 − xA)

α xA

yA =

1 + (α − 1)xA

32
M.Sc. Abdulrazzaq Saeed Distillation
yA

xA =

α − (α − 1)yA

Whilst α does vary somewhat with temperature, it remains remarkably steady for
many systems, and a few values to illustrate this point are given in table below.

It may be seen that α increases as the temperature falls? Why?

Q) Prove that
∗
P
α A
=

PB∗

Example3.1: Vapor pressures of Benzene – Toluene mixture are given in the table
below. Assuming that this mixture follow Rault's law, calculate and plot the boiling
point diagram and the equilibrium composition curve. Note the total pressure is 1
atm.

Solution

To plot the T-y-x diagram find y, x at each

T ºC Pv (mmHg) Pv (mmHg)
temperature for component (Benzene), because it is the A B
more volatile component since its boiling point at 1 80.1 760 0
atm (80.1º C) is lower that of Toluene at the same 85 877 345
pressure (110.6 ºC). At T=85 ºC
xA = v
P−P
v
B
v
90 1016 405
B
100 1344 557
PA −P

760 − 345

xA = = 0.78
877 − 345 110 1748 743
110.6 1800 760
x Pv

AA

y =

A
P

877 × 0.78
y = = 0.9

760

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M.Sc. Abdulrazzaq Saeed Distillation

Repeat for all the given temperatures establish the following table:

T ºC 80.1 85 90 100 110 110.6

1 0.78 0.581 0.258 0.017 0
yA
1 0.9 0.777 0.456 0.039 0

The following diagram is plotted according to the above data:

Example3.2: for the binary mixture (A&B), the relative volatility is αAB =2.81.
Plot the equilibrium data for this system.
Solution

1 + ( − 1)

2.81 x A
y= A 1 + 1.81 xA

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M.Sc. Abdulrazzaq Saeed Distillation

xA yA

0 0
0.1 0.237
0.2 0.412
0.3 0.546
0.4 0.651
0.5 0.737
0.6 0.808
0.7 0.867
0.8 0.913
0.9 0.96
1 1

3.7Flash Vaporization:

3.7.1Introduction

If a sufficiently hot liquid mixture is throttled into a vessel, a part of it will

vaporize. The vapour produce will be richer in the more volatile component and
thus partial separation of the desired component will be achieved. This is called
flash vaporization or equilibrium vaporization. A schematic sketch of a flash
vaporization unit is shown in figure below.

In this process, a pressurised feed stream, which is in

liquid phase, is passed through a heater in order to pre-
heat the feed then passed through the throttling
valve/nozzle, connected to a tank or drum, which is
called a “flash” tank or drum After being passed through
the valve/nozzle, the feed enters the tank/drum, whose
pressure is low; thus, there is a substantial pressure drop
in the feed stream, causing the feed to partially vaporize

35
M.Sc. Abdulrazzaq Saeed Distillation

It is noteworthy that, although the illustration of the

flash tank is in vertical direction , flash tanks/drums in
horizontal direction are also common.

Both the vapor and the residual liquid are cooled to the
saturation temperature of the liquid at the reduced
pressure. This is often referred to as "auto-refrigeration"
and is the basis of most conventional vapor-compression
refrigeration systems.

3.7.2Features

a. Continuous , steady state process. Operating conditions (T & P) are constant.

b. Compositions and flow rates of feed , products of overhead and bottom

are constant.

c. There is equilibrium always between phases of vapor and liquid.

3.7.3Uses

1. Refrigeration

2. Desalination

3. Production of biofuels

Overall Material Balance

F=V+L

A material balance
F. xf = V. y + Lx
F. xf = V. y + (F − V)x
y = VF xf − LV x
‫( عطقالو‬ − L
V ) ‫ ليم اله ميقتسم طخ ةلداعم ةالعا ةلداعلما برتعت‬
. ( VF xf)

. ‫هالعا ةلداعلما للح نزاوتال نيحنم جاتنح‬ 

36
M.Sc. Abdulrazzaq Saeed noitallitsiD

Example 3.3 : A liquid mixture containing 50 mole% n-heptane (A) 50 mole% n-

octane (B), at 30°C, is to be continuously flash–vaporized at std atm pressure to
vaporize 60 mol% of the feed. What will be the composition of the vapor and liquid
?in the separator
0.487 0.312 0.157 0 0.655 1 X
0.674 0.492 0.279 0 0.810 1 y

Solution
F = 100 mol / h Basis

V = 60 mol / h , L = 40 mol /h

1.0

0.9

0.8

0.7

0.6

0.5

0.4

0.3

0.2

0.1

0.3 0.2 0.1 0.0

0.8 0.7 0.6 0.5 0.4

1.0 0.9

:‫ترسم معادلة برج التقطري الوميضي كااليت‬

° 45. ‫( واليت تقع على خط‬0.5 , 0.5) ‫ وهي‬xf , xf) ) ‫النقطه‬ 1.

60
40
= −0.667− = )VL− ( ‫ امليل وهو‬2.
. ‫ اللتان يف حالة توازن من نقطة تقاطع اخلط املستقيم مع منحني النوازن‬x ‫ و‬y ‫ حتسب قيمة‬3.

x= 0.387,y=0.575

37
M.Sc. Abdulrazzaq Saeed Distillation

Example3.4: A mixture of 40 mol% benzene and 60 mol% toluene is being Flash–

distilled at a rate of 10 kmol/h at 1 atm total pressure. The liquid product should not
contain more than 30 mol% benzene. Calculate the amounts and the composition of
the top and bottom product. The relative volatility of benzene in the mixture is 2.5.
Solve analytically as well as graphically.

Solution

Overall Material Balance

F=L+V

10 = L + V …………. (1)

Benzene Material Balance

(10) (0.4) = L (0.3) + y V

4 = 0.3 L + y V ……(2)
αx
y=
1 + (α − 1)x

y = (2.5(0.3))/(1+(2.5-1) 0.3 )=0.517

Sub in (2)

4 = 0.3L + 0.517 V …..(3)

Sub in (1) in (3) yield

L = 5.39 mol/h

V = 4.61 mol/h

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M.Sc. Abdulrazzaq Saeed Distillation

Continuous Multistage Fractionation Of Binary Mixtures

Introduction
Separation of a volatile liquid mixture to relatively pure products is very often done
in a continuous fractionating column. A packed or a tray tower can be used, the
choice depending upon several factors.
The feed (it may be a liquid, a vapour or a two-phase mixture containing
components A and B; A is the more volatile com ponent) enters the column at a
suitable location. The liquid stream flows down the column from one tray to the
next lower tray; the vapour stream flows up bubbling through the liquid on the trays.
The vapour from the top tray is condensed and the condensate is collected in a reflux
drum. A part of this liquid is drawn as the top product and the other part is fed back
to the top tray (the top tray is marked tray no. 1) as reflux. The top
product contains the more volatile component A
and a little of the less volatile B. The liquid from
the bottom tray goes to a reboiler where it is
partly vaporized, the vapour is fed back to the
tower and the liquid part is continuously
withdrawn as the bottom product. The bottom
product is rich in the less volatile component B
and has only a small amount of A in it. An
intimate contact between the liquid and the
vapour phases occurs on a tray, facilitating rapid
exchange of mass between them. Transport of the
more volatile component A occurs from the
liquid to the vapour phase, while transport of the
less volatile B occurs from the vapour to the liquid phase
-The section of the column above the feed point is called the rectifying or enriching
section while the section of the column below the feed tray, is called the stripping
section
-The more important variables, parameters and factors involved in the design of a
trayed distillation tower:

39
M.Sc. Abdulrazzaq Saeed Distillation

a. The flow rate, composition and state of the feed. The state of the feed may be
described by its temperature, pressure, phase, etc. The feed may be a liquid, a
vapour, or a mixture of liquid and vapour
b. The required degree of separation. The degree of separation is mainly
determined by the requirement of quality or purity of the products drawn
from the column.
c. The reflux ratio and the condition of the reflux The reflux ratio is an
important design parameter. A specified degree of separation can be achieved
with a lesser number of trays if the reflux ratio is increased. The condition of
reflux means whether the reflux is a saturated liquid or a subcooled liquid.
d. The operating pressure and the allowable pressure drop across the column.
The operating pressure also determines the temperature of the column. The
pressure drop for the vapour flow depends upon the type, the number and the
hydraulic design of the trays. Pressure drop becomes a more important factor
if a column is run at a low pressure.
e. Tray type and column internals. The efficiency of separation (given by the
tray efficiency) is largely determined by these factors.

McCabe-Thiele Method of Calculation for Number of Theoretical

Stages

A mathematical-graphical method for determining the number of theoretical trays or

stages needed for a given separation of a binary mixture of A and B has been
developed by McCabe and Thiele. The method uses material balances around
certain parts of the tower, which give operating lines, and the xy equilibrium curve
for the system. The most important assumptions made to apply this method are:
1- The two components have equal and constant molar enthalpies of vaporization
(latent heat).
2- Component sensible enthalpy changes (Cp T) and heat of mixing are negligible
compared to latent heat changes.
3- The column is well insulated so that heat loss is negligible.
4- The pressure is uniform throughout the column (no pressure drop).

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M.Sc. Abdulrazzaq Saeed Distillation

Equations For Enriching Section

Overall material Balance

F=D+W

A total material balance

F xf = D xd + W xw

O. M. B. around the selected section:

Vn+1 = Ln + D
[A] M. B. for the selected section:
Vn+1 yn+1 = Ln xn + D xd
Solving for yn+1 Ln D xd
yn+1 = xn +
Vn Vn

L n
Since R= reflux ratio = D = constant Vn = Ln + D
constant molar over
= D*(R+1) flow
Then R xd
Vn+1 = Vn
y = x +
n+1 R+1 n R+1

Ln+1=Ln

Enriching Operating
Line

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M.Sc. Abdulrazzaq Saeed Distillation

Equations For Stripping Section

Total material balance on over dashed–line section

Lm = Vm+1 + W
Vm+1 = Lm – W

A total material balance:

Vm+1 ym+1 = Lm xm – W xw
Stripping–section Operating

Lm wx
y = x − W

m+1 m
Line
Vm Vm

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M.Sc. Abdulrazzaq Saeed Distillation

The Intersection of the Operating Lines

If the two operating lines intersect at a point with coordinates (xq, yq ), then
from equations of operating lines:

If Hf is the enthalpy per mole of feed, and Hf s is the enthalpy of one mole of feed at
its boiling point, then the heat to be supplied to bring feed to the boiling point is
F(Hf s − Hf ), and the number of moles of vapour to be condensed to provide this
heat is F(Hf s − Hf )/λ, where λ is the molar latent heat of the vapour.The reflux
liquor is then:

43
‫‪M.Sc. Abdulrazzaq Saeed‬‬ ‫‪noitallitsiD‬‬

‫‪q‬‬ ‫‪x‬‬
‫‪q – line‬‬ ‫‪yq = q−1 xq − fq−1‬‬
‫‪+‬‬ ‫‪cp (T‬‬ ‫‪λ‬‬
‫=‪q‬‬ ‫)‪f Bp − Tf‬‬
‫‪λ‬‬

‫‪where‬‬

‫‪.λ‬‬ ‫‪: latent heat of vaporization of feed‬‬

‫‪.Cpf‬‬ ‫‪: average heat capacity of the feed‬‬
‫‪.of‬‬ ‫‪the feed‬‬ ‫‪TBp : average boiling point‬‬
‫‪.Tf‬‬ ‫‪: feed temperature‬‬

‫‪ ‬اذا املغذي يدخل الربج عند درجة الغليان فأن ‪q=1 .‬‬
‫‪ ‬اذا املغذي يدخل الربج كبخار عند نقطة الندى فأن ‪q= 0 .‬‬
‫‪ ‬اذا املغذي يدخل الربج كسائل بارد فأن ‪q > 1 .‬‬

‫‪ ‬اذا املغذي يدخل الربج كبخار محمص فأن ‪q < 1 .‬‬

‫‪ ‬اذا املغذي يدخل الربج جزء سائل وجزء خبار فأن ‪ q‬هي كسر السائل يف املغذي ‪.‬‬

‫‪44‬‬
M.Sc. Abdulrazzaq Saeed Distillation
/ ‫ةظحالم‬
. 1- ‫يرارحلا طلخا ةلداعبم ىمست هالعا ةلداعلما‬
xf xf

‫ عطقال وا‬. q

‫( ليلماو‬xf , xf) 2- ‫ةطقنال من مسرت‬

xq =
q
‫ وا‬y q =−
q−1 q−1

Enrichment in Still and Condenser

Point 16 in Figure 11.15 represents the concentration of the liquor in the still. The
concentration of the vapour is represented by point 15, so that the enrichment
represented by the increment 16–15 is achieved in the boiler or still body. Again, the
concentration on the top plate is given by point 2, but the vapour from this plate has
a concentration given by point 1, and the condenser by completely condensing the
vapour gives a product of equal concentration, represented by point A. The still and
condenser together, therefore, provide enrichment (16 − 15) + (1 − A), which is
equivalent to one ideal stage. Thus, the actual number of theoretical plates required
is one less than the number of stages shown on the diagram. From a liquid in the
still, point 16 to the product, point A, there are eight steps, although the column
need only contain seven theoretical plates.

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M.Sc. Abdulrazzaq Saeed Distillation

Example A liquid mixture of benzene-toluene is to be distilled in a fractionating tower

at 101.3 kPa pressure. The feed of 100 kg mol/h is liquid and it contains 45 mol
% benzene and 55 mol % toluene and enters at 327.6 K. 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 , the boiling point of the feed is 93°C and the
average latent heat 32099 kJ/kg mol . Equilibrium data for this system are given in
Table below. Calculate the kg moles per hour distillate, kg moles per hour bottoms,
and the number of theoretical trays needed.

Solution

For the overall material balance

F=D+W

100=D+W ……………….. (1)

A material balance
F xf=D xd+W xw

100(0.45)=D (0.95) + W (0.1) …………(2)

46
M.Sc. Abdulrazzaq Saeed Distillation
Substitute equation (1) in (2)
D=41.2 kgmol/h , W=58.8 kgmol/h

For enriching operating line

yn+1 = R+1R xn + R+1xd= 0.8 xn + 0.19

 (xd,xd)=(0.95,0.95)
 xd/R+1=0.19

For q-Line
= 32099 + 159(366.7 − 327.6) = 1.195 32099

 (xf,xf)=(0.45,0.45)
 q/(q-1)=6.12=0.61/0.1

For stripping operating line

 (xw,xw)=(0.1,0.1)

No. of stages=7.6

No. of plates=6.6

Feed is introduced on tray 5 from top

47
M.Sc. Abdulrazzaq Saeed Distillation

Example: A continues fractionation column, operation at atmospheric pressure , is to be

designed to separate a mixture containing 15.67 CS2 and 84.33% CCl4 into an overhead
product containing 91% CS2 and a waste of 97.3 % ccl4 (all weight percent).
If the reflux ratio is taken as 3.16, using the data below. Determine the number of
plates required in the following cases: -

a- Feed inlet at T = 290 k

b- Feed inlet at T = 336 k
c- Feed inlet partially vaporized 70% liquid and 30% vapor.
d- Feed is saturated vapor and xf = 0.5 mol fraction.
e- Feed inlet at T = 380 k (xf = 0.5).

Given the following data:- cpf = 1.7 kJ/kg.k, TB.p = 336k, λ = 25900 kJ/kmol ,

Mwt cs2 = 76 kg/kmol , Mwt ccl4 = 154 kg/kmol

y% 8.23 15.55 26.6 33.2 49.5 63.4 74.7 82.9 87.8 93.1

x% 2.96 6.15 11.06 14.35 25.85 39 53.18 66.3 75.75 86.2

Solution
Basis 100kg /h feed Basis 100kg /h over head product

Comp. Mass Mole xf Comp. Mass Mole xd

CS2 91 1.197 0.95
CS2 15.67 0.206 0.27

CCl4 84.33 0.547 0.73 CCl4 9 0.058 0.05

Total 100 0.7535 1 Total 100 1.255 1

48
M.Sc. Abdulrazzaq Saeed Distillation

Basis 100 kg /h waste

Comp. mass Mole xf

CS2 2.7 0.0355 0.05

CCl4 97.3 0.631 0.95

Total 100 0.6673 1

Mwtav = (0.27 * 76) + (0.73 * 154) = 132.6

∴ cpf = 1.7 * 132.6 = 225.42 kJ / kmol

cpf(TBp− T f)+ λ 225.42 (336−290)+ 25900

q= = = 1.4
λ
25900

Slop =
1. 4

=3.5 ⇒
−1 0. 4
= tan−1(3.5)

= 74

For enriching operating line

1) (xd , xd ) = (0.95 , 0.95)

xd
2) R+1 = 3.0.16+195 = 0.229

For q-Line

1) (xf , xf) = (0.27 , 0.27)

2) Slop q−q1 = 3.5 = 00.35.1

For stripping operating line

1) (xw , xw) = ( 0.05 , 0.05)

2) Intersection of overhead operating line and q–line

49
M.Sc. Abdulrazzaq Saeed Distillation

1.0
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Number of stage = 9
Number of plates = 8

a) The feed is at boiling point

cp (T
q= f B.p − Tf) + λ
λ = λ=1

‫يرارحلا طلخا مسرن‬ 

1) (xf , xf) = (0.27 , 0.27)
2) Slop = 10 = ∞ ()

1.0
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2

50
M.Sc. Abdulrazzaq Saeed Distillation

0.1
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0

From fig (b)

Number of stages = 10

Number of plates = 9

b) The feed is partially vaporized (70% liq , 30% vap )

q=
( . − )+ 0.7
= = 0.7

‫من يرارحلا طلخا مسرن‬

1) (xf , xf ) = (0.27 , 0.27)

2) Slop −1 = − 00,3.7 = −2.33 ⇒ = −66.8

1.0
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
51
M.Sc. Abdulrazzaq Saeed Distillation

From fig (c)

Number of stage = 11

Number of plates =10

c) The feed is Saturated vapor
q=
( . − )+
= 0 (ℎ )

‫ يرارحلا طلخا مسرن‬

1) (xf , xf) = (0.5 , 0.5)

2) Slop −1 = −01 = 0

1.0
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0

From Fig (d)

Number of stage = 9

Number of plates = 8

52
M.Sc. Abdulrazzaq Saeed Distillation

e) The feed is superheated

q= ( − )+ .

= . ( − ) =− .

‫ يرارحال طخال مسرن‬

1) ( , )=(0.5,0.5)

2) Slop − =−. − .
= 0.27

1.0
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
From Fig (e)

Number of stage = 10

Number of plates = 9

53
M.Sc. Abdulrazzaq Saeed Distillation

Total and Minimum Reflux Ratio for McCabe-Thiele

Method 1. Total Reflux
One of the limiting values of reflux ratio is that of total reflux, or R = ∞, then Ln is very large, as is the vapor flow vn. This
means that the slope R/(R + 1) of the enriching operating line becomes 1.0 and the operating lines of both sections of the

column coincide with the 45° diagonal

line In actual practice, this condition
can be realized by returning all the
overhead condensed vapor VI
from the top of the tower back to
the tower as reflux, i.e., total
reflux. Also, all the liquid in the
bottoms is reboiled. Hence, all the
products distillate and bottoms are
reduced to zero flow, as is the
fresh feed to the tower.
This condition of total reflux can
also be interpreted as requiring
infinite sizes of condenser,
reboiler, and tower diameter for
a given feed rate.
Note: For operation at total reflux, sufficient amount of feed is charged into the
reboiler and flow of steam (to the reboiler) and of cooling water (to the condenser)
are started. The entire condensate is fed back as reflux. The rate, the concentration
and the thermal state of the feed are not relevant for a column operated at total reflux
since there is no feed input at all.
For conditions in which the relative volatility is constant, FENSKE derived an
equation for calculating the required number of plates for a desired separation. Since
no product is withdrawn from the still, the equations of the two operating lines
become:
Vn=Ln , Lm=Vm, F=D=W=0

yn+1=xn

ym+1=xm

54
M.Sc. Abdulrazzaq Saeed Distillation
yA xA
=α

y x

For the reboiler

yA xA
( ) =α ( )
y W x

B
B
W
W

From operating line equation

yAw=xAn

yBw=xBn

For plate n

yA xA
( ) =( )
y x

W B
n
B

xA yA xA
( ) =( )=α( )

W
x B y x
n
B B
W W

For plate n-1

xA yA
( ) =( )
x y

B
n−1 n
B

yA xA
( ) =α ( )

y n x

B
n n
B

xA yA xA xA
( ) =( )=α( )=αα( )

x y n x n W x

B
n−1

Bn
Bn B W

For top plate

x y
( A
) =( A
)
x y
B
d 1
B

yA xA
( ) =α ( )

y 1 x

B
1 1
B

xA xA
( )=αα….α αα ( )

1 2 n−1 n W

x x
B d B W

n+1

… . αn−1 αn αW
α = √α1 α2
avr.

55
M.Sc. Abdulrazzaq Saeed Distillation
n+1
α =α α ….α α α

avr. 1 2 n−1 n W

xA xA
( ) =α n+1 ( )

avr.
d
x
xB BW

x x
ln [( A) ( B) ]
xB xA
n+1= d W

ln α
avr.

n : number of theoretical plates

2. Minimum Reflux Ratio

The minimum reflux ratio can be defined as the reflux ratio Rm that will require an
infinite number of trays for the given separation desired of x D and xw.
This corresponds to the minimum vapor flow in the tower, and hence the minimum
reboiler and condenser sizes.
If R is decreased, the slope of the enriching operating line R/(R + 1) is decreased,
and the intersection of this line and the stripping line with the q line moves farther
from the 45° line and closer to the
equilibrium line. As a result, the number of steps required to give a fixed xd and xw
increases. When the two operating lines touch the equilibrium line, a "pinch point"
at y' and x' occurs where the number of

steps required becomes infinite. The slope of the

enriching operating line is as follows from Fig.

below, since the line passes through the points x',

y', and xd

Rm xd − ý

=
Rm + 1 xd − x́

The above strategy fails for some

other shapes of the equilibrium curve.
Examples are shown in Figure 7.21
and Figure 7.22. Because of the
typical curvature, the pinch point does not occur at the intersection of the feed line
and the equilibrium curve. As the reflux ratio is reduced, at a certain value of it the
pinch point K occurs at the point of tangency of the rectifying section operating line
(Figure 7.21) or the stripping section operating line (Figure 7.22) and the
56
M.Sc. Abdulrazzaq Saeed Distillation

equilibrium line. The location of the point of tangency depends upon the shape
of the equilibrium line. This type of pinch point and the minimum reflux ratio
can be determined only graphically
The optimum operating reflux ratio is (1.2-1.5)Rm.

Under conditions of minimum reflux, a column has to have an infinite number of

plates, or alternatively the composition on plate n is equal to that on plate n + 1.,
yn+1= yn then:

Vn+1=Ln+D
Vn+1(yn+1)=Ln(xn)+D(xd)
Vn+1(yn+1)A=Ln(xn)A+D(xd)A…….(1)

Vn+1(yn+1)B=Ln(xn)B+D(xd)B…….(2)

At Rm , (yn+1)A= (yn)A and (yn+1)B= (yn)B

Divide equation 1 on 2

y
nA = xnA Ln + D xdA

y x L +Dx
nB dB
nB n
y ⁄y
α = nA nB
x ⁄x
nA nB

57
M.Sc. Abdulrazzaq Saeed Distillation
x
nA
x
nA
L +D x
ndA
dividing by D
α( )=
xn x L +D x

B nB n dB

x x
nA nA Rm + xdA
α( )=
xn x R +Dx
nB m dB
B

1 x x
dA dB

Rm = [ −α ]

α−1
x x
nA nB

For feed plate

1 x
dA
x
dB

Rm = [ −α ]

α−1
x x
fA fB

For binary system

1 xd (1 − xd)

[ −α ]
Rm = α−1

xf (1 − xf)

Example: For the rectification in previous example, where a benzene-toluene

feed is being distilled to give a distillate composition of xd =0.95 and a bottoms
composition of xw = 0.10, calculate the following graphically and analytically.
(a) Minimum reflux ratio Rm ,
(b) Minimum number of theoretical plates at total reflux.

Solution

a) Reading off the values of. x'= 0.49 and y' =0.702

Rm=1.17 Analytically
Rm=1.35
b) The minimum number of theoretical
steps is 5.8, which gives 4.8 theoretical
trays plus a reboiler.
Analytically n+1=5.8 , n=4.8

58
M.Sc. Abdulrazzaq Saeed Distillation

xA yA yB xB α alpha αtotal αav

1 1 0 0 #DIV/0! 2.538462 34.44997 2.422687
0.78 0.9 0.1 0.22 2.538462 2.440126
581 0.777 0.223 -580 -3.47831 2.353066
0.411 0.63 0.37 0.589 2.440126 2.363589
0.258 0.45 0.55 0.742 2.353066
0.13 0.261 0.739 0.87 2.363589
0 0 1 1 #DIV/0!
‫ ةظحالم‬: ‫نزاوتال ميق من ةيرياطتال بستح الثلما اذه يف‬

Example:A rectification column is fed 100 kg mol/h of a mixture of 50 mol %

benzene and 50 mol % toluene at 101.32 kPa abs pressure. The feed is saturated
vapor at the dew point.. The distillate is to contain 90 mol % benzene and the
bottoms 10 mol % benzene.
Calculate the following.
(a) Minimum reflux ratio Rm,.
(b) Minimum number of theoretical plates at total reflux.
(c) Theoretical number of trays at an operating reflux ratio of 1.5(Rm)
Solution

59
M.Sc. Abdulrazzaq Saeed Distillation

Calculation of Number of Plates Using the Lewis–Sorel Method

Assumptions were made for this method that there is equilibrium over-flow
(approximately the same assumption in MaCabe-Thiele method), that is: V n = Vn+1 =
V1 = V2 = …
Ln = Ln+1 = L1 = L2 = …
Both the upper operating line equation and the lower operating line equation
(derived in previous section) can be applied for this method also.
y ……1
n+1 = R+1R xn + R+1xd
Lm w xW
ym+1 = xm − ……2
Vm Vm

To calculate the number of theoretical stages required using this method follow
these steps:
1- Find all streams F, D, W and their compositions.
2- Find R, either graphically or analytically.
3- Draw the equilibrium data.
4- Start from the first plate at the top of the column, where y 1 = xd. Then from the
equilibrium curve find x1 (which will in equilibrium with y 1). Substitute x1 in the
T.O.L. equation so to find y 2, and then find x2 from the equilibrium curve. Keep on
as in the above procedure until you reach the feed plate xn≤ xf .

60
M.Sc. Abdulrazzaq Saeed Distillation

5- Substitut last x in the bottom operating line equation to find y m+1 and then from
the equilibrium curve find xm+1. Keep on until you reach x m ≤ xw, which will be the
last plate.
6- The theoretical number of plates = N-1

Example: A mixture of benzene and toluene containing 40 mole percent benzene is

to be separated to give a product containing 90 mole per cent benzene at the top,
and a bottom product containing not more than 10 mole per cent benzene. The feed
enters the column at its boiling point, and the vapour leaving the column, which is
condensed but not cooled, provides reflux and product. It is proposed to operate the
unit with a reflux ratio of 3 kmol/kmol product and the relative volatility is 2.4. Use
Lewis method to find the number of theoretical plates needed and the position of
entry for the feed.
Solution
Basis F=100 kmol/hr of the feed
Overall mass balance gives:
F=D+W
100=D+W
A balance on benzene, gives:
(100 )(0.4) = 0.9 D + 0.1 W
Thus: 40 = 0.9(100 − W) + 0.1 W
W = 62.5 and D = 37.5 kmol
Ln
R=D

Ln = 3D = 112.5 kmol/hr
Vn+1 = Ln + D = 150 kmol/hr
The top operating line (T.O.L) is:
D xd
Ln
y = x n +
n+1 V

n n

y = 112.5 x + (37.5) (0.9)

n+1 n
150 150

yn+1 = 0.75 xn + 0.225 T.O.L ………….(1)

Lm = Ln + q F
Lm = 112.5 + 100 = 212.5 kmol/hr
Vn = Vm + (1-q ) F
Vn+1 = Vm+1 + 0
61
M.Sc. Abdulrazzaq Saeed Distillation

Vn+1 = Vm+1
Or, Lm = Vm+1+ W
Vm+1=Lm – W
Vm+1=212.5 – 62.5=150 kmol/hr
The bottom operating line (B.O.L) is:
Lm w xW
y = x −
m+1 m
Vm Vm

y = 212.5 x − (62.5 ) (0.1)

m+1 m
150 150

ym+1 = 1.415 xm − 0.042 B.O.L ….(2)

The value of yn+1 is obtained from equation (1) as:

-y1=0.9= xd from vapor-liquid equilibrium data x1=0.79

-y2 = 0.75 ( 0.79) + 0.225 = (0.593 + 0.225) = 0.818

x2 is obtained from the equilibrium curve as 0.644

-y3 = 0.75 ( 0.644) + 0.225 = (0.483 + 0.225) = 0.708

x3 is obtained from equilibrium curve = 0.492

-y4= 0.75 (0.492) + 0.225 = (0.369 + 0.225) = 0.594

x4 is obtained from the equilibrium curve = 0.382

This last value of composition is sufficiently near to that of the feed. Therefor, the
feed is introduced on the plate (4). For the lower part of the column, the operating
line equation (2) will be used.
y5 = 1.415 ( 0.382) − 0.042 = (0.540 − 0.042) = 0.498
x5 is obtained from the equilibrium curve = 0.298

y6= 1.415 (0.298) − 0.042 = (0.421 − 0.042) = 0.379

x6 is obtained from the equilibrium curve = 0.208

y7= 1.415 (0.208) − 0.042 = (0.294 − 0.042) = 0.252

x7 is obtained from the equilibrium curve = 0.120

62
M.Sc. Abdulrazzaq Saeed noitallitsiD

y8=
1.415
(0.12
0) −
0.042
=
(0.16
9−
0.042
)
0.127
x8 is
obtai
ned
from
the
equili
briu
m
curve
0.048

This liquid x8 is slightly weaker than the

minimum required and it may be withdrawn as
the bottom product. Thus, x8 will correspond
.to
the reboiler
Number of stages= 8
Number of plates= 7
.Feed is in traduced on tray 4 from top

Example: Repeat previous example but use a feed that is partially vaporized so that
mol % is liquid and 30 mol % vapor. Use Lewis method to find minimum reflux 70
ratio and the number of theoretical plates needed and the position of entry for the
.feed
Solution
‫ وكاليت‬TOL ‫ مع خط التشغيل العلوي‬q-line ‫جيب اجياد نقطة تقاطع‬
q x
f

=y q −x q

q−1 q−1

y=-2.34 x + 1.34 ……….1

‫‪Ln=112.5 kmol/h‬‬
‫‪Vn+1=150 kmol/h‬‬
‫‪Lm = Ln + q F‬‬
‫‪Lm = 112.5 + 100(0.7) = 182.8 kmol/hr‬‬
‫‪V n = Vm + (1-q ) F‬‬
‫‪Vm =120 kmol/h‬‬
‫‪Ln‬‬ ‫‪D xd‬‬
‫‪y‬‬
‫‪n+1‬‬
‫=‬ ‫‪x‬‬
‫‪n‬‬
‫‪+‬‬
‫‪V‬‬ ‫‪V‬‬

‫‪n‬‬ ‫‪n‬‬

‫‪yn+1 = 0.75 xn + 0.225……….2‬‬

‫‪Equate equation 1 with 2‬‬

‫‪x + 0.225=-2.34 x + 1.34‬‬ ‫‪0.75‬‬
‫‪x=0.36‬‬ ‫‪y=0.5 ,‬‬
‫‪ x=0.36 ,‬عندها تعرتب هي صينية املغذي« و نعوض بعد‬ ‫حتسب الصواين من االعلى اىل ان نصل اىل الرتكيز ‪ xi‬اقل او يساوي‬
‫ذلك يف خط التشغيل السفلي‬

‫‪63‬‬
M.Sc. Abdulrazzaq Saeed Distillation

‫ تيالاكو نزاوتال نيحنم عم‬q-line ‫ عطاقت ةطقن ةفرعم من عجارلل ةبسن لقا داجيا نكيم‬α x
y=
1 + (α − 1)x

y = 1+1.4x2.4x……3

Equate equation 1 with 3

2
x +0.87x – 0.4=0
x=0.33 , y= 0.56
Rm xd − ý

=
Rm + 1 xd − x́

Rm=1.5
Overall tray efficiency
Graphical and algebraic methods for determining stage requirements for distillation
assume equilibrium with respect to both heat and mass transfer at each stage. Thus,
the number of equilibrium stages (theoretical stages, ideal stages, or ideal plates) is
determined or specified when using those methods. The McCabe-Thiele method
assumes that the two phases leaving each stage are in thermodynamic equilibrium. In
industrial countercurrent, multistage equipment, it is not always practical to provide
the combination of residence time and intimacy of contact required to approach
equilibrium closely. Hence, concentration changes for a given stage are usually less
than predicted by equilibrium.
The simplest approach for staged columns is to apply an overall stage (or column)
efficiency, defined by lewis as: number of ideal trays
E=

For example, if eight theoretical stages are needed and the overall efficiency is 60%,
the number of theoretical trays is seven trays. The actual number of trays is 7/0.6, or
11.7 trays.

64