UNIT II

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UNIT II

DISTILLATION

Vapour-liquid equilibria, Raoult's law and deviations from ideality, methods of distillation;
fractionation of binary and multicomponent system; design calculations by McCabe-Thiele and
ponchon-Savarit, methods; continuous contact distillation tower (packed tower) design; extractive and
azeotropic; distillation low pressure distillation; steam distillation.
University Repeated Question

1. Derive Fenske's equation. State its limitation.

2. A mixture of benzene and toluene containing 40 mole percent of benzene' is separated to give a
product of 90 mole percent of benzene at top and a bottom product with not more than 10 mole
percent benzene. Using an average value of a 2.4 for the volatility of benzene relative to toluene,
calculate the number of theoretical plates required at total reflux. Also calculate the minimum
reflux ratio, if t feed is liquid and at its boiling point.

3. Explain the utility of McCabe-Thiele method in determining the number of ideal plates in a fractionating
column. List out the limitations of this method.

4. Describe the following with neat flow diagram;


a.Azeotropic distillation b.Simple distillation c. Low pressure distillation d.Steam
distillation e. Extractive Distillation f. Molecular distillation

5. Illustrate the method of calculation of ideal trays by Panchon - Savarit method


6. A Benzene -Toluene solution containing 55% Benzene is to be fractionated continuously in a
distillation column to get a top product of 85%, and a bottom product of 10%Benzene. The feed
is at its bubble point. The relative volatility is 2.5. Find
(a) The no. of plates required for a reflux ratio of 2.5.
(b) Minimum no. of plates.
7.
8. A fractionating column separates a liquid mixture containing 50 mole % A and 50 mole % B into an
overhead product of 95 mole % A and a bottom product of 96mole A. A reflux ratio of twice the
minimum will be used and the feed enters at its boiling point. Determine the number of theoretical stages
required and the location of feed point. Equilibrium data:
X 0.03 0.06 0.11 0.14 0.26 0.39 0.53 0.66 0.76 0.86
Y 0.08 0.16 0.27 0.33 0.50 0.63 0.71 0.83 0.88 0.93
X,Y mole fraction of A in liquid and vapor phase respectively

9. 1000 kmollhr of ethanol-propanol mixture containing 65 mole %ethanolis to be separated in a


continuous .plate column operating at 1 atm.pressure. The desired terminal compositions for ethanol
are : XD = 0.92and Xw = 0.07. The feed is a saturated vapor and a total condenser ispsed. When reflux
'ratio is four times the amount of top product, findthe number of theoretical plates required for the
separation. Data given: Relative volatility = 2.10. Also find Nmin.

10. A binary distillation column is operating under conditions as feed rate == 450 kmol/h, overhead product
rate = 200 kmol/h XD = 0.95, XW = 0.05, W=250kmol/h R= 35.
In the stripping section, it was found that the mol. fraction of more volatile component in the vapor
leaving a plate is 0.35 while the mole fraction in the liquid coming to the same plate is 0.25. Assuming
constant molal overflow, determine whether the feed is vapor, liquid or partially vapor.

Page:1 UNIT-II DISTILLATION


UNIT II
DISTILLATION
Distillation is a method of separating the components of a solution which depends upon the
distribution of the substances between a gas and a liquid phase, applied to cases where all
components are present in both phases. This unit operation is also termed as ‘Fractionation’ or ”
Fractional distillation “
Concept of Distillation
In distillation , the phase involved are liquid and vapour or gas and mass is transferred from both the
phase to one another
a. Vaporization from liquid phase
b. Condensation from vapour phase
Equilibrium
Separation of components by distillation is that composition of vapour be different from the
composition of the liquid which it is ‘Equilibrium’
Vapour – liquid Equilibria (VLE)
Successful application of distillation method depends greatly upon an understanding of equilibrium
existing between the vapour and liquid phase of the mixture encountered
Constant Pressure Equilibria
Consider the upper curve provides the temp – vapour composition (t-y*) relationship, the lower that of
the temperature – liquid (t-x) relationship composition

Page:2 UNIT-II DISTILLATION


Relative volatility :
Relative volatility is the ratio of the concentration ratio of A and concentration ratio B in one phase to
that in other and is a measure of separability
=
=

=
Ideal solution (Raoult’s law)
“ Equilibrium of partial pressure P* of the compound is directly proportional to its product of its
vapour pressure ‘pA’ and its mole fraction ‘x’ in the liquid is called as Raoult’s law
P* = pA x
Components B
P* = pB (1-x)

Methods of Distillation
Basically distillation is carried out in two ways:
1. The liquid mixture is heated to create vapour. The vapour formed are condensed in condenser
and withdraw as a product - NO Reflux
2. The liquid mixture is heated to create vapour. The vapour formed are condensed in condenser
part of the condensed liquid is returned to distillate system - Reflux
Common methods used in distillation
1. Differential or Simple distillation
2. Flash or Equilibrium distillation
3. Rectification or Fractionation
Differential or Simple distillation
This method is commonly known quantity of liquid mixture is charged into jacked kettle or
still.The jacked kettle is provided for heating the mass in still with help of a heating media
Let ‘F’ be the Kmol of the liquid mixture A+B containing
Let Xf – mole fraction of component ‘A’
Let ‘D’ be Kmol of the Distillate Let ‘W’ be Kmol of the residual liquid
Let yDavg and xw are mole fraction of ‘A’ in distillate and bottom residual liquid
Page:3 UNIT-II DISTILLATION
Let ‘L’ be Kmol of the liquid in still Let ‘x’ be the mole fraction of ‘A’ in liquid

Overall material balance at any time


L = (L -dL) + dD------------1
L = L- dL+dD
dL = dD---------------2
Individual material balance any time
Lx = (L -dL) (x-dX) + (y. dD)---------------3
Lx = Lx-LdL - x dL + dL dX + y. dD
Ldx + xdD = dDdx + y. dD {dL = dD ---2
dDdx are being very small can be neglate
Ldx + xdD = y. dD ----------4
Ldx = (y-x) dD
Ldx = (y-x) dL
dx /(y-x) = dL / L --------5
Intergrating above equation between two extreme condition
L =F x =xF
L=W x = xw
Page:4 UNIT-II DISTILLATION
=

[ln L ]FW =

ln (F/W) = ----------------------6
This equation is known as Rayleigh equation

Page:5 UNIT-II DISTILLATION


Page:6 UNIT-II DISTILLATION
Flash or Equilibrium distillation
Consider 1mole of liquid mixture having xF mole fraction of more volatile component is fed to flash
distillation unit

• Let ‘F’ can be fraction of feed or vapourized and composition ‘y’


• Let ‘x’ will be mole fraction of more volatile component
• Let (1-f) will be mole of residual liquid obtained

Material balance for more volatile component


(1. Xf ) = fy + (1-f) x -----------1
- (1-f) x + Xf = fy
y = - (1-f) x / f + Xf / f
x = - (1-f) x + Xf / f { x=y
x = Xf
y = Xf
For f=1 feed totally vaporised
slope =0 = - (1-f) / f = - (1-1) / 1 =0
and hence the operating line is parallel to ‘x’ axis through the point( Xf ,Xf ) on diagonal

For f=0 no feed is vaporised

Slope is infinity and the operating line will be parallel to y axis

Page:7 UNIT-II DISTILLATION


Continuous Rectification –Binary System (Fractionating column)
1. Rectification or Fractionating column is commonly encountered in industrial practice
2. The enrichment of the vapour stream as it passes through the column in contact with reflux
3. In this separation method part of the condensed liquid is returned back as a reflux and
maximum enrichment of more volatile compound in vapour is obtained
4. Vaporization and condensation by multistage contact of vapour and liquid is called as (single
unit) Fractionating column

Fractionating column consists of: Cylinder shell divided into section by a series of perforated trays
1. Reboiler
2. Condenser

Page:8 UNIT-II DISTILLATION


The liquid mixture to be separated in introduced in the cylindrical column . The column itself is dived
into 2 section
a) Rectification section
b) Stripping section
Rectification section
1. The section above the feed plate is called as Rectifying section
2. The vapour is washed to remove the less volatile compound with the liquid return to column
from top.(Reflux)
Stripping section
1. The position below the feed plate including feed plate is called as stripping section

2. Liquid is stripped off more volatile compound by rising vapour

Overall Material balance:


1. Consider that column is feed with ‘F’ (moles/time)of liquid mixture (feed)
with xf mole fraction of more volatile component
2. Let ‘D’ (mole /time) of composition xD are withdrawn as a distillate
3. Let W (mole /time) of composition xw are withdrawn as a bottom product
Overall Material Balance
Feed = Distillate + Bottom Product
F = D + W ---------- 1
Material Balance of more volatile compound (A) over fractionator
A in Feed = A in Distillate + A in Bottom Product

Page:9 UNIT-II DISTILLATION


F xf = D xD + W xw ---------- 2
From equation 2
W = F - D ---------------- 3
Sub : W = F - D in equation 2
F xf = D xD + (F- D) xw
= D xD + F xw - D xw
F xf = D (xD - xw ) + F xw
F (xf – xw ) = D (xD - xw )
D/ F = (xf – xw ) / (xD - xw ) -------------4
Eliminating “D” gives (from equation) 1
D =F - W
F xf = (F- W) xD + W xw
= F xD - W x D + W xw
F (xf – xD ) = W (xW - xD )
W/ F = (xf – xD ) / (xW - xD ) -------------5
a. Let ‘L’ be (mole/ time) of liquid returned to the top of column then
Reflux ratio = R = L/D This reflux ratio is also known as external reflux ratio
b. Let ‘V’ is the (mole/ time) molal flow rate of vapour leaving the top of column then
Reflux ratio = R = L/V This reflux ratio is also known as Internal reflux ratio

Rectification section

Page:10 UNIT-II DISTILLATION


Material Balance over Condenser:
V = L + D ---------- 6
L = V - D
D = V - L
Overall Material Balance Over fig (above)
Vapour flow to plate (n) = Liqiud flow from plate (n) + Distillate withdrawn
Vn+1 = Ln + D -----------7
Material Balance of more volatile component (A)
Vn+1 yn+1 = Ln xn + D xD -----------8
yn+1 = ( Ln / Vn+1 ) xn + D xD / Vn+1 --9
From equation 7 sub in eq 9
yn+1 = ( Ln / Ln+D ) xn + D xD / Ln+D ------10
Eq 10 is known as material balance line (or) Operating line for ‘Rectifying section’

Stripping section (Including Reboiler)

Material Balance including Reboiler:


Liquid flow to plate (m+1) withdrawn = Vapour flow from plate (n) + Bottom product

Lm = Vm+1 + W -----------11
Similarly Vm+1 = Lm - W ------------11a

Page:11 UNIT-II DISTILLATION


Material Balance of more volatile component (A)
Lm xm = Vm+1 ym+1 + W xw -----------12
Rearrange the equation 12
ym+1 = ( Lm / Vm+1 ) xm - W xw / Vm+1 -- 13
Equation 13 becomes
Vm+1 = Lm - W
ym+1 = ( Lm / Lm- W ) xm – (W/Lm- W)xw -- 13
Equation 14 is operating equation for ‘stripping section’

Analysis of fractionating column:


The theoretical/ ideal stage/ plates required for given degree of separation can be obtained by
1. Mccabe - Thiele method
2. Lewis – sorel method
3. Ponchon – savarit method

Mccabe - Thiele method


Assumption :
1. Constant molal heat of vaporization
2. No heat loss
3. No heat of mixing
Consider any plate ‘n’ in the rectifying section
Heat Balance across plate ‘n’ is
Ln-1 HLn-1 + Vn+1 HVn+1 =Ln HLn + Vn HVn + Heat loss+ Heat of mixture
Heat losses are negligible for good insulation. Heat of mixing is zero for ideal system. Then equation 1
becomes
Ln-1 HLn-1 + Vn+1 HVn+1 =Ln HLn + Vn HVn-----------2
Where
• HL and HV are Enthalpy of liquid and vapour per mole
If the molal heat of vapouraization is constant than one mole of vapour Vn+1 on condensing,release
sufficient heat to liberate 1 mole of vapour Vn

Page:12 UNIT-II DISTILLATION


Vn = Vn+1 HLn = HLn-1 -----sub eq 2
HVn = HVn+1
Sub eq2 becomes
Ln-1 HLn-1 + Vn+1 HVn+1 =Ln HLn-1 + Vn+1 HVn+1
Ln-1 HLn-1 = Ln HLn-1
Ln-1 = Ln
So the moles of liquid reflux in this section are also constant
• Ln and Vn+1 are constant is rectifying section
• Lm and Vm+1 are constant in the stripping section
ie., The molal flow rate of vapour and liquid are constant is each section of column
Ln = Ln-1 = L
Vn = Vn+1 = V
Ln-1 HLn-1 = Ln HLn-1
Ln-1 = Ln
So the moles of liquid reflux in this section are also constant
• Ln and Vn+1 are constant is rectifying section
• Lm and Vm+1 are constant in the stripping section
ie., The molal flow rate of vapour and liquid are constant is each section of column
Ln =Ln-1 = L
Vn = Vn+1 = V
Lm =Lm-1 = L’
Vm = Vm+1 = V’
Operating line equation for rectifying section
yn+1 = ( L / L+D ) xn + (D / L+D) xD --------3
In general,
y = ( L / L+D ) x + (D / L+D) xD ----------3a
Divide (÷D) in equation 3a
y = { ( L/D / (L/D)+(D/D )} x + {(D/D)/(L/D)+(D/D) } xd
Page:13 UNIT-II DISTILLATION
y = { ( L/D / (L/D)+(1)} x + {(1)/(L/D)+(1) } xd
W.K.T R= L/D
y = ( R / R+1 ) x + (xD / R+1)-----------4
Here, point of intersection of operating line for rectifying section and diagonal (x= y) obtained as
x = (R / R+1 ) x + (xD / R+1)-----------5
{ 1 – (R / R+1 )} x = (xD / R+1)
{R+1 – R / R+1 )} x = (xD / R+1)
x /R+1 = xD / R+1
x = xD ------------a y = xD -----------b
Thus the operating line of rectifying section to be drawn on equilibrium diagram through the point with
the co-ordinates (xD , xD )on diagonal and with a slope of R/R+1 and Intercept on y axis = xD / R+1. The
operating line of stripping section becomes ,equation 3a
y = ( L ‘ / L’-W ) x - (W / L’-W) xW -------5
Here, point of intersection of operating line for stripping section and diagonal (x= y) obtained as
x = ( L ‘ / L’-W ) x - (W / L’-W) xW
x( L’-W ) = L ‘x - W xW
L’ x -W x = L ‘x - W xW
W x = W xW
x = xw------------c y = xw -----------d
Thus the operating line of Stripping section is to be drawn through the point having co-
oridinates (xw , xw )on diagonal and with a slope of L’/L’-W and Intercept on W xW / L’-W
Limitation of Mc cabe -Thiele method ;
1. It is not used when relative volatility is less than 1.3 or greater than 5 (1.3<∞>5)
2. It is not used when more than 25 theoretical plates are required
3. It is not used when the operating reflux ratio is less than 1.1 times the minimum reflux ratio

Feed plate and Feed line


The plate on which feed is introduced is called feed plate
The feed to the column may be introduced as

Page:14 UNIT-II DISTILLATION


a) Cold Liquid

b) Liquid at its Bubble point (Saturated liquid)

c) Partially Vaporized (Partially vapour/Partially liquid)

d) Saturated vapour at its Dew point

e) Super heated vapour

To calculate the change in phase flow rate by introduction of feed, factor ’q’ is introduced
‘q’ – It is a measure of thermal condition of feed
for feed F
L’ = L + qF ---------------1
V = V’ +(1-q)F ----------2

The values of “q” for various thermal condition of feed are:


a) Cold Liquid : q>1
b) Liquid at its Bubble point : q =1
(Saturated liquid)

c) Partially Vaporized: (0<q<1)


(Partially vapour/Partilly liquid)

d) vapour at its Dew point : q=0


(Saturated vapour)

e) Super heated vapour :q<0

‘q’ value for any particular feed condition can be calculated from :
q = Energy to convert 1 mole of feed to sat.vapour
Molal latent heat of vaporization
Liquid flow in stripping section is from 1 eq
L’ = L + qF ---------------1

Page:15 UNIT-II DISTILLATION


L’- L = qF ---------------3
Similarly vapour flow in rectifying section from 2 eq
V = V’ +(1-q)F ----------2
V- V’ = (1-q)F ----------4
Overall material balance for upper section;
V = L+ D--------------5
material balance of mole fraction comp A;
Vy = Lx+ DxD--------------6
Overall material balance for Lower section
w+ v’ = L’ ---------------7
V’ = L’ - W ---------------8
for material balnce of mole fraction of comp A Eq8
V’y = L’x - Wxw ---------------8.1
Substract equation 8.1 from eq 6
Vy - V’y = Lx- L’x +DxD +Wxw
(V- V’)y = (L- L’)x +DxD +Wxw ---------9
W.K.T
F xf = D xD + W xw ---------- 10
From eq 10 eq 9 becomes
(V- V’)y = (L- L’)x +DxD +FxF ---------11
sub eq 3 and 4 in eq11
y (1-q) F= -xqF +FxF
y (1-q) F= F(-xq +xF ) --------------------12
y = {-q/(1-q)} x + [xF /(1-q)] --------13
Eq 13 is known as feed line or q-line point of intersection of feed line and diagonal (y=x)is
x = {-q/(1-q)} x + [xF /(1-q)]
x(1-q) = -xq +xF
x-xq= -xq +xF
Page:16 UNIT-II DISTILLATION
x = xF
y = xF
The feed line thus passes the point (xF, xF) on diagonal and slope -q/(1-q) and intercept XF /1-q

Design of distillation column (Procedure for solving the distillation problem :)


1. Let xD , xF, and xw are the mole fraction of distillate ,feed and bottom product of the distillation
column
2. To draw the distillation tower diagram and locate the mole fraction xD , xF, and xw
3. Draw the equilibrium diagram with help of x – y data given in the problem (or) Generate the
data using the following relation
Assume the value of x from 0 to 1
4. Draw the diagonal joining the points (0,0) and (1,1)
5. Locate xD , xF, and xw in the x-axis
6. Draw a straight line from xD , xF, and xw to intercept the diagonal at this points a,b,c respectively
7. Draw the feed line from the point ‘b’ with the help of slope -q/(1-q) Where q- fraction of
liquid in feed
8. Let the point of intersection of feed line and equilibrium curve
9. Draw a straight line joining the point ‘a’ and ‘d’
10. The above line gives the intercept in the y-axis ;Let it be ‘emin ‘
11. Find RD min from the following relation
Intercept =

12. Find RD act RD act = RD min x Multiplying factor


Where –Multiplying factor will be given in the problem
13. Find the value of ‘eactual‘ from RD actual using the following
Intercept =

14. Locate the intercept value ‘eactual‘ in the y-axis


15. Join the points ‘eactual‘ and “a” with a straight line

Page:17 UNIT-II DISTILLATION


16. The above line is operating line of the rectifying section. This RoL Intercept the feed line at
point F
17. Joint the points “F” and “C” . The FC is he operating line of the stripping section
18. The line “af” and FC serves as the operating line of the entire column of distillation
19. Draw stepwise construction between the operating line of the column and equilibrium line
starting from point “a” and ending at point “c”

20. The number of theoretical plates in the column:


a. When Reboiler is used
no% of plates= plates from graph -1
b. When Partial condenser is used
no% of plates= plates from graph -2

21. Actual plate= Theoretical plates/ % OF efficiency

1. A mixture containing ethanol and water contains32% (mole %) of alcohol is to be separated in a


fractionating column using indirect stream as the source of heat.The fractionation is carried out at
1atm pressure to obtained to give product containing 97% alcohol is overhead product and bottom
product containing 1.5% . Clculate the minimum reflux ratio.Find out the number of theoretical stages
required if reflux ratio of 1.78 times the minimum is used.. Feed is a saturated liquid.VLE for the
system

x 0 0.02 0.04 0.06 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0

Y 0 0.13 0.23 0.30 0.41 0.57 0.66 0.72 0.77 0.82 0.87 0.91 0.95 1

xD = 0.32
xF, = 0.97
xw =0.015
RD act = RD min x 1.78
Page:18 UNIT-II DISTILLATION
q =1 (saturated liquid)
Feed line = -q/(1-q)
Slope = -1/(1-1) =∞
From graph: emin = 0.55
Intercept:
=

R D min +1 = xD / 0.55
= 0.97/0.55
R D min +1 = 1.7636
R D min = 0.7636

RD act = RD min x 1.78


RD act = 0.7636 x 1.78
RD act = 1.3592

Intercept = = 0.97/ (1.35927+1)

Intercept act = 0.411

From graph
No% of plates = 9
Feed plates =6
total reboiler is used
No% of plates ={plates from graph} – 1 =8

2. A Continuous fractionating column is to designed to separate 30000kg/hr of a mixture of 40%


benzene and 60% of toluene into an overhead product containing 97% benzene and bottom product
contains 98%toluene are by weight. A reflux ratio (RD) of 3.5 moles to 1 mole of products to be
used. Benzene and toluene from ideal system with a relatively volatility of about 2.5 , the feed has
a boiling point of 95oc at a pressure of 1atm.If the feed is a mixer of 2/3 vapor and 1/3 liquid
a) Calculate the moles of overhead product and bottom product per hour
Page:19 UNIT-II DISTILLATION
b) Determine the no/. of ideal plates and the postion of the feed plates
i. If the feed is liquid and its boiling point
ii. If the feed is liquid mixture of 2/3 vopur and 1/3 liquid
Given Data

Mol. Wt% of Benzene = 78 (C6H6)

Mol.Wt% of Toluene = 92 (C6H5 CH3)

∞ = 2.5

Tb = 950c

= 7360 cal/gmol

= 7960 cal/ gmol

Solution
Avg molecular weight of feed = (0.4 x 78) + (0.6 x 92) = 86.4 Kg/Kmol
Avg molecular weight of feed = (0.98x 92) + (0.02 x 78) = 91.72 Kg/Kmol
Avg molecular weight of feed = (0.97 x 78) + (0.03 x 92) = 78.42 Kg/Kmol

xF =

xF = 0.4398

xB =

xB = 0.0234

xD = =
xD = 0.974

Page:20 UNIT-II DISTILLATION


a)
F =30,000Kg/hr
F = 30,000/86.4

F = 347.222 Kmol/hr

D = 152.156 Kmol/hr
Material balance
F=D+W
W=F–D
W = 347.222 – 152.156
W = 195.064 Kmol/hr
b. i) Feed is a saturated liquid: q = 1
Slope of feed line = -q/1-q
= -1/1-1
=
= 2.5
=

x 0 0.2 0.4 0.6 0.8 1

y 0 0.384 0.625 0.789 0.909 1

Plot graph b/w x&y

From graph Intercept = 0.41


Page:21 UNIT-II DISTILLATION
Intercept =

0.41 =

RDmin +1 = 0.974/0.41

RDmin = 1.435

RD act = RD min x 3.5

RD act = 1.435 x 3.5

RD act = 5.0225

Intercept = 0.974/ (5.0225+1) = 0.16172

From graph, (total condenser is used)

No% of theoritical plates = 10

No% of theoritical plates = 10 – 1 = 9 plates

Feed plates = 5th plate

ii)Feed is mixture of two- third vapour and one – third liquid

q = 1 /3 = 0.333

slope = = -0.4995

From graph: emin = 0.31

Intercept =

R D min +1 = xD / 0.31

= 0.974/0.31

R D min = 2.1419

RD act = RD min x 3.5

RD act = 2.1419 x 3.5

RD act = 7.4966

Page:22 UNIT-II DISTILLATION


Intercept = = 0.974/ (7.4966+1)

Intercept = 0.114

From graph, (total Reboiler is used)

No% of theoritical plates = 10

No% of theoritical plates = 10 – 1 = 9 plates

Feed plates = 5th plate

University Question

3. 1000Kmol /hr of ethanol – Propanol mixture containing 65mole % ethanol is to be separated in a


continuous plate column operating at 1atm pressure. The desired terminal composition for ethanol are
XD = 0.92 and Xw = 0.07 .The feed is a saturated vapour and a total condenser is used. When the
reflux ratio is four times the amount of top product , find the number of theoretical plates required for
the separation .Data given relative volatility = 2.10

Given data
xD = 0.65
xF, = 0.92
xw =0.07
RD act = RD min x 4
Y = αx / 1 + x(α-1

q =0 (saturated Vapour)

Feed line = -q/(1-q)


Slope = -0/(1-0)
= 0
From graph: = 0.35
Intercept:
=

R D min +1 = xD / 0.35
= 0.92/0.35 = R D min = 1.62
RD act = RD min x Multiplying factor

RD act = 0.7636 x 4
RD act = 6.51

Intercept =

Page:23 UNIT-II DISTILLATION


= 0.92 / (6.51+1) = Intercept = 0.122
From graph
No% of plates = 8
Feed plates =4

total Reboiler is used


No% of plates ={plates from graph} – 1
=7

4. A benezene – toluene solution containing 55 % benzene is to be fractionated continuously in a


distillation column to get atop product of 85% and bottom product of 10% bezene . The feed is at
its bubbles point . the relative volatility is 2.5 . Find
i. The no/ of plates required for a reflux ratio is 2.5
ii. Minimum no of plates

Given data
xD = 0.85 xF, = 0.55 xw =0.10
RD act = RD min x 2.5

Y = αx / 1 + x(α-1)

q =1 (saturated Liquid)

Feed line = -q/(1-q)


Slope = -1/(1-1) =∞
From graph: = 0.57
Intercept:
Intercept =

R D min +1 = xD / 0.57
= 0.85/0.57 = R D min = 0.49
RD act = RD min x Multiplying factor
RD act = 0.7636 x 2.5
RD act = 1.23

Intercept =

Page:24 UNIT-II DISTILLATION


= 0.85 / (1.23+1) = Intercept = 0.38

From graph
No% of plates = 7
Feed plates =4
total Reboiler is used
No% of plates ={plates from graph} – 1
No% of plates = 6

5. A continuous fractionating column is to be designed to separate 13,620 Kg/hr of mixture of 40%


benzene, 60% toluene in to an over head product contains 97% benzene and bottom products
containing 98% toluene are by weight. Reflux ratio of 3.5: 1 of product is to be used. The molar
latent heat of benzene, tolune are 7360 and 7960 cal/ mole. Calculate moles of over head product and
bottom product. Determine the number of ideal theoretical plates and position of the Feed plate if
Feed is liquid at its boiling point Feed at 1.36 atm gauge is used for heating, how much steam is
required / hr for each of the above cases. λ = 522 Kcal / Kg. Cooling water enters the condenser at
26.7degC and leaves at 65.5 deg C. How Much cooling water is required.
Mole fraction of benzene in liquid 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Mole fraction of benzene in vapour 0.0 0.2 0.38 0.51 0.63 0.71 0.78 0.85 0.91 0.96 1.0
F = 13, 620 Kg /hr
Xf = 0.4 X D = 0.97 XB = 0.02
F= 158.6 Kg moles / hr
Fxf = BxB + DxD
D = 69.47 Kg moles / hr
B = 89.19 Kg moles / hr
Feed is a saturated liquid q =1 Slope = 90 Intercept = 0.216
No of ideal plates = 11 including reboiler Feed location = 5 th plate
6. It is desired to distill a plate column for separating a equimolal feed mixture of A and B to get a
product of 95% A and 5%A in the distillate and residue respectively. The reflux enters the column at
it’s bubble point and a reflux ratio of 1.5 times the minimum is to be used. Estimate the number of
plates needed if the plate efficiency is 80%
XA 0 0.16 0.31 0.49 0.66 1.0
YA 0 0.28 0.49 0.67 0.81 1.0

Page:25 UNIT-II DISTILLATION


Xf = 0.5 XD = 0.95 XB = 0.05
R = 1.5 Rmin
q =1
XD / Rm + 1 = 0.38
Rm = 1.5
R = 2.25
n = 13 plat

Fenske Equation
This equation can be used to theoretically calculate the minimum no/. of trays ,if the relative
volatility remains constant

-----------------------------1

----------------------------2

Operating line equation for rectifying section interms of n+1

------------------------3

At total reflux ratio


D=0, RD = 1 RD = L/D=1 =L/V
3=> From equation ,we get

---------------------------------------4

2=> for n+1 tray

---------------------------5

Sub equation 4 in 5

--------------------6

Page:26 UNIT-II DISTILLATION


At n=1 in eq 6

---------------------------7

At n=2 in eq 6

---------------------------8

Let : n=n-1 in eq 6

------------------------------9

At n=0 in eq 5

---------------------------10

Let y1 =xD (Total condenser ,Total reflux)

-----------------------------------11

Multiplying the eaquation 7,8,9,11

xn = xD

Let n=Nmin+1

= ----------------------12

Taking log on both side we get ,above eq 12

Page:27 UNIT-II DISTILLATION


Nmin +1 ln ( )-----------------------------------12

Nmin +1 = -----------------------------------------13

Equation 13 is known as FENSKY EQUATION

Heating and Cooling Reqiuremnts:


When the saturated steam is used as the heating medium ,Steam requirements given by this formula,

ms – Steam consumption
v – Vapour rate from the reboiler
-latent heat of steam
-Molal latent heat of mixture
If the water is used as the cooling medium in the condenser and the condensate is not sub cooled, the
cooling water requirement

mw =water consumption
T2-T1 –temp rise of the cooling water
Note : The feed is a mixer of vapour and liquid .Then q =1-F, where f – fraction of original steam
vapour
If the feed is cold

-latent heat of vaporization


CpL -specific heat of liquid
Tf -temp of feed
Tb -bubble point of feed
For superheated vapor ,q is given by
Page:28 UNIT-II DISTILLATION
Cpv -specific heat of vapor
Tf –dew point of feed

Azeotropic distillation
1. This is a special case of multicomponent distillation used for separation of binary mixture
2. Azeotropic distillation are either difficult or impossible to separate by ordinary fractionation
3. Under this circumstances third component, sometimes called an Entertainer may be added to
binary mixture to form a new boiling azeotropic with one of the original constituents
4. By this process volatility is easily occur and it can easily be separated from the other original
constituent
5. Acetic acid can be separated from water by azeotropic method
6. To add butyl acetate is added to top of column
7. Azeotrope can readily be distillated from the high-boiling acetic acid, which leaves as a residue
product
8. Azeotrope is then distilled overhead
9. Their composition is unchanged by distillation, azeotropes are also called constant boiling mixtures.

10. If two solvents can form a positive azeotrope, then distillation of any mixture of those constituents will
result in the distillate being closer in composition to the azeotrope than the starting mixture

Choice of Entrainer:
1. Entrainer should from a low boiling azeotrope with only one of the constituents of the
binary mixture
2. Cheap and readily available 3.Chemically stable 4.Non-corrosive 5.Non-toxic
6. Low latent heat of vaporization 7.Low freezing point to outdoor handling
8. Low viscosity to provide high tray efficiency.

Page:29 UNIT-II DISTILLATION


Extractive distillation
1. This is multicomponents – rectification method similar in purpose to azeotropic distillation

2. To binary mixture which is difficult or impossible to separate by ordinary means a third


comond termed a ‘solvent’(low relative volatility)

3. Iso octane in this mixture is the more volatile but the sepeartion is difficult

4. In the presence of phenol , Iso octane relative volatility increases ,Phenol in the liquid

5. The separation from touene is relatively easy

6. Solvent –Recovery section of the tower which may be relatively short , to separate the phenol
from Isooctane.

Residue – Tolune and phenol.

Overhead Product – Iso Octane

7. The residue from the tower must be rectified in the tower (2) to separate toluene from the
phenol which is recycled but this is a relatively easy sepaeration
Page:30 UNIT-II DISTILLATION
8. Extractive distillation: is defined as distillation in the presence of a miscible, high boiling, relatively
non-volatile component, the solvent, that forms no azeotrope with the other components in the
mixture.

9. The method is used for mixtures having a low value of relative volatility, nearing unity.

10. Such mixtures cannot be separated by simple distillation, because the volatility of the two components
in the mixture is nearly the same, causing them to evaporate at nearly the same temperature at a similar
rate, making normal distillation impractical.

General Requirements of Extractive distillation solvent

1. High seletiviyt or ability to alter be VLE of the orginal mixture

2. High capcity or ability to dissolve the components in mixture to be separated

3. Low volatility in order to prevent vaporization

4. Of the solvent with overhead product.

5. Seperation –Solvent must be reaily separated from the mixture to which it is added

6. Low cost

7. Non-toxic

8. Non –corrosive

9. Chemically stable

10. Low freezing point

Molecular distillation or Vacuum distillation

1. Molecular distillation or Vacuum distillation is a method of distillation whereby the pressure


above the liquid mixture to be distilled is reduced to less than its vapor pressure (usually less
than atmospheric pressure) causing evaporation of the most volatile liquid(s) (those with the
lowest boiling points).
2. This distillation method works on the principle that boiling occurs when the vapor pressure of a
liquid exceeds the ambient pressure.
3. Vacuum distillation is used with or without heating the mixture.

Steam distillation

Steam distillation is a special type of distillation (a separation process) for temperature


sensitive materials like natural aromatic compounds.
Page:31 UNIT-II DISTILLATION
Separation by normal distillation, steam is introduced into the distillation apparatus. The Liquid
mixture (substances) to be distilled are very sensitive to heat, steam distillation can also be combined
with vacuum distillation. After distillation the vapors are condensed as usual.
Principle
When a mixture of two practically immiscible liquids are heated while being agitated to expose
the surfaces of both the liquids to the vapor phase, each constituent independently exerts its own vapor
pressure as a function of temperature .Consequently, the vapor pressure of the whole system increases.
Boiling begins when the sum of the partial pressures of the two immiscible liquids just exceeds
the atmospheric pressure
Applications
1. Steam distillation is employed in the manufacture of essential oils,
for use in perfumes.
2. Eucalyptus oil and orange oil are obtained by this method
on the industrial scale.
3. Steam distillation is also sometimes used to separate intermediate or
final products during the synthesis of complex organic compounds.
4. Steam distillation is widely used in petroleum refineries and
5. Steam distillation is also used in petrochemical plants

Simple Distillation
1. Simple Distillation is a chemical process where two or more liquids with different boiling
points can be separated from each other.
2. The liquids are heated until one of them boils and evaporates (turns to a gas).
3. The vapor is then fed into a condenser, which cools the vapour and condenses it back to a
liquid.
4. What remains in the original container is called the residue.
5. A fractionating column can be used to improve the separation.
6. Distillation can be used for making dirty water cleaner.
7. Fractional distillation can be used to purify crude oil so that it can become useful and can be
used for various things

Page:32 UNIT-II DISTILLATION


8. The vaporized and condensed component is called distillate and the other component as the
residue.
9. This has been used for a long time, to distill alcohol, pond water, and certain brands of coffee,
and produce distilled beverages.
10. Distillation is a commonly used operation in oil industry, where it is used to separate various
fuels and raw materials from crude oil.
Application
Simple distillation can roughly be divided in four groups:
1. laboratory scale, and industrial distillation,
2. Distillation of herbs for perfumery and medicinal (herbal distillate), and food processing.

Page:33 UNIT-II DISTILLATION

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