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DISTILLATION

separation of different components in a liquid solution


involved producing a vapour from a liquid
by heating the liquid in a vessel
eg. Ethanol-water:
vapour phase = higher conc. of ethanol
liquid phase = higher conc. of water
2 methods of distillation:
rectification/fractional/distillation with reflux
part of the vapour is condensed & returned as
liquid back to the vessel
all of the vapour is removed or is condensed as
product

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DISTILLATION

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DISTILLATION
Types of distillation:
simple
fractional
steam
immiscible solvent
azeotropic
extractive
vacuum
molecular
Distillation tower at an oil refinery.

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entrainer sublimation

VAPOUR-LIQUID EQUILIBRIUM RELATIONS


vapour & liquid in intimate contact for a long time,
equilibrium is attained
RAOULTS LAW
ideal solution (substances very similar to each other)
pA = PAxA

or

yA =(pA/P)=(PA/P)xA

where
pA = partial pressure of component A in the vapour
PA = vapour pressure of pure A
P= total pressure
xA = mole fraction of A in the liquid
yA = mole fraction of A in the gas
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BOILING-POINT DIAGRAMS & x-y PLOTS


(VLE diagrams)

Vapour-liquid equilibrium for A-B mixture eg. benzene(A)toluene (B)

heat a mixture of benzene-toluene at xA1 = 0.318( boil at 98oC), first


vapour in equilibrium is yA1 = 0.532
distance bet. equilibrium & 45o line = diff. bet. xA & yA ( diff., easier
separation)
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VLE diagrams

non-ideal systems which will present more difficult separation

An azeotrope is a liquid mixture which when vaporised, produces the same


composition as the liquid.
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RELATIVE VOLATILITY OF VAPOUR-LIQUID


SYSTEMS
Relative volatility, - numerical measure of ease of separation
AB - relative volatility of component A with respect to component B
yA
y A /x A
xA
AB = y =

B
1 y /1 x
A
A
xB
where
yA = mole
fraction of A in the gas phase

xA = mole fraction of A in the liquid which is in


equilibrium with yA phase
For an ideal system (obeys Raoults law):
x
yA = A
1+ 1x A
where

PA vapour pressure of pure A


=
P
vapour pressure of pure B
B

AB =

when 1 , separation is possible


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SINGLE-STAGE EQUILIBRIUM
CONTACTOR
Binary distillation - components A & B
yA1

yA2

xA1

xA0

Constant molal overflow:

V1 = V2
L0 = L1

Total material balance:


Balance on A:

L0 + V2 = L1 + V1
L0xA0 + V2yA2 = L1xA1 + V1yA1

Unknown : x1 & y1 solve simultaneously (graphically) between equilibrium


line & overall material balance
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Example 11.2-1

A vapor at the dew point and 101.32 kPa


containing a mole fraction of 0.4 benzene (A)
and 0.6 toluene (B) and 100 kg mol total is
brought into contact with 110 kg mol of a liquid
at the boiling point containing a mole fraction
of 0.30 benzene and 0.70 toluene. The two
streams are contacted in a single stage, and
the outlet streams leave in equilibrium with
each other. Assume constant molar overflow.
Calculate the amounts and compositions of the
exit streams.

SINGLE-STAGE EQUILIBRIUM
CONTACTOR
Example 11.2-1

=100 kmol
yA2 =0.4

yA1
=110 kmol
xA0 =0.3

Constant molal overflow:

xA1

V1 = V2= 100 kmol


L0 = L1 = 110 kmol

Balance on A:

L0xA0 + V2yA2 = L1xA1 + V1yA1


110(0.3) + 100(0.4) = 110xA1 + 100yA1
lets xA1 = 0.2, yA1 = 0.51
lets xA1 = 0.4, yA1 = 0.29
lets xA1 = 0.3, yA1 = 0.4
At intersection, xA1 = 0.25, yA1 = 0.455

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SIMPLE DISTILLATION METHODS


EQUILIBRIUM OR FLASH DISTILLATION
Single stage binary distillation
V,y
F,xF

Heater

Separator

L,x
liquid mixture partially vapourized
vapour allowed to come to equilibrium with liquid
vapour & liquid then separated
Balance on A:

FxF = Lx + Vy or FxF = (F-V)x + Vy

Unknown : x & y solve simultaneously (graphically) between equilibrium


line & overall material balance similar to eg. 11.2-1
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SIMPLE DISTILLATION METHODS


SIMPLE BATCH OR DIFFERENTIAL DISTILLATION
liquid mixture charged to a still (heated kettle)
V, y
slowly boiled & vapourized part of the liquid
vapour withdrawn rapidly to condenser
L, x
first portion of vapour = richest in component A
vapourized product gets learner in comp. A
L1 = original moles charge
x1 = original composition
L2 = moles left in the still
x2 = final composition of liquid

unknown: x2

L1 x dx
=
L 2 x y x
Graphical solution:
ln

L1
ln
area under the curve 1/(y-x) vs x plot = L
2

Average composition of total material distilled, yav:


L1x1 = L2x2 + (L1-L2)yav
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Example 11.3-2

A mixture of 100 mol containing 50 mol%


n-pentane and 50mol% n-heptane is
distilled under differential conditions at
101.3 kPa until 40 mol is distilled. What is
the average composition of the total
vapor distilled and the composition of the
liquid left? The equilibrium data are as
follows, where x and y are mole fractions
of n-pentane:

The equilibrium data are as follows, where x and y


are mole fractions of n-pentane:
x

1.000

1.000

0.398

0.836

0.059

0.271

0.867

0.984

0.254

0.701

0.594

0.925

0.145

0.521

Example 11.3-2
Equilibrium data:

L1 = 100 mol
x1 = 0.5 mol /mol

1.0 0.867 0.594 0.398 0.254 0.145 0.059 0

V = 40 mol

1.0 0.984 0.925 0.836 0.701 0.521 0.271 0

x2 = ? , yav = ?

Total balance :

L1 = V + L2
100 = 40 + L2

L2 = 60 mol
L
ln 1 = xx ydx
x
L2
ln 100 = x0.5 ydx
x = 0.51
60
1

L1x1 = L2x2 + (L1-L2)yav


100(0.5) = 60(0.277)+ (100-60)yav
By trial-&-error, x2 = 0.277
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yav = 0.835

McCABE-THIELE METHOD
binary mixture A-B
assume equimolar overflow/constant molal overflow between
feed inlet & top tray
feed inlet & bottom tray
graphical method for determining the number of theoretical stages,N

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q line
Effect of feed condition (q line)

q=heat needed to vaporize 1 mol of feed


at entering conditions per molar latent heat
of vaporization of feed.
q-line equation:

McCabe-Thiele Method

Graphical method requires:


i.Top Operating Line
ii.Feed Operating Line (q-line)
Iii.Bottom Operating Line

Feed Operating Line (q-line)

q-line equation:
Lm=Ln + qF
Vn=Vm + (1-q)F
Vny=Lnx+DxD (Top) ---(1)
Vmy=Lmx WxW (Bottom)-----(2)
(2)-(1):
(Vm-Vn)y=(Lm-Ln)x-(DxD-FxF)
(Vm-Vn)y=(Lm-Ln)x FxF
Lm-Ln=qF
Vm-Vn=(q-1)F

q-line cont
(q-1)Fy = qFx FxF
y = [(q)/(q-1)]x xF/(q-1)

q-line cont

q value depends on feed conditions:


If feed is liquid at boiling pt: q=1
If feed is saturated vapor:q=0
If feed is liquid below its boiling pt:q>1
If feed is a mix bet. Liq & vap: 0<q<1

Example 11.4-1
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, containing 45 mol% benzene and 55 mol%
toluene, and enters at 327.6 K(130oF). 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 (38 btu/lb mol.oF) and the average latent heat
32099 kJ/kg mol (13800 btu/lbmol). Equilibrium data for this
system are given in Table 11.1-1.Calculate the kg moles per
hour distillate, kg mole per hour bottoms, and the number of
theoretical trays needed.

Example 11.4-1
Binary mixture A-B (benzene-toluene) at 101.3kPa. Reflux ratio (R) = 4.
Average heat capacity of feed = 159 kJ/kmol.K & average latent heat = 32099
kJ/kmol. Determine D kmol/h, W kmol/h & N theoretical trays needed.
Total material balance:
F =100 =D + W
D kmol/h
xD = 0.95

Balance on benzene (A):

F =100 kmol/h

FxF = DxD + WxW

xF = 0.45

100(0.45) = D(0.95) + W(0.1)

TF = 327.6K

Substituting D = 100-W
W kmol/h

45 = (100-W)(0.95) + W(0.1)

xW = 0.1

45 = 95 +(W)(0.95) + W(0.1)

W = 58.8 kmol/h
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D =100 - W

D = 100-58.8 = 41.2 kmol/h

Example 11.4-1
L
F =100 kmol/h

D kmol/h
xD = 0.95
1. Plot equilibrium & 45o lines on x-y graph

xF = 0.45
TF = 327.6K

W kmol/h
xW = 0.1

R = 4 = L/D
2. Draw enriching operating line
x
y = R x+ D
R +1 R +1
y = 4 x + 0.95 = 0.8x + 0.19
4 +1 4 +1

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Example 11.4-1
3. Calculate q (fraction of feed that is liquid)
H V H F H V H L + cP (TB TF )
q=
=
HV HL
HV HL

Average heat capacity of feed =159 kJ/kmol.K


Average latent heat 32099 kJ/kmol
32099 + (159)(TB 327.6)
q=
32099

From Fig. 11.1-1, at xF = 0.45, TB = 93.5oC (366.7K)


32099 + (159)(366.7 327.6)
q=
= 1.195
32099

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Example 11.4-1
q = 1 (liquid at its boiling point) , q = 0 (saturated vapour) , q 1 (cold liquid feed)
q 0 (superheated vapour) , 0 q 1 (mixture of liquid & vapour)

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Example 11.4-1
4. Draw q-line

q-line

q = 1.195

xF
q
y=
x
q1
q1

y= 1.195 x 0.45 = 6.12x 2.31


1.1951
1.1951

Slope = 6.12 = y/x = (0.45 y)/(0.45-x)


Lets x = 0.40
0.45 y
6.12 = 0.45 - y = 0.45 - y =
0.45 x 0.45 0.4
0.05
y = 0.144

5. Draw stripping operating line

Connect xW(on 45o line) with the point of intersection of the q-line & the
enriching operating line
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Example 11.4-1
6. Stepping off from xD
Starting from xD, make steps bet.
equilibrium line & enriching line to q-line

2
3

Feed tray

4
5

7. Shift to stripping line after passing qline

6
7

8. Feed location = tray on the shift


Feed tray = tray 5 from the top
9. Ntheo. stages = number of steps
Ntheo. stages = 8 stages
10. Ntheo. trays = theo. stages - reboiler
Ntheo. trays = 8 1= 7 trays plus a reboiler
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TOTAL REFLUX, R =
minimum number of stages, Nmin
operating lines coincide with 45o line
infinite sizes of condenser, reboiler & tower diameter
stepping off from xD to xW on the 45o line
or using Fenske equation (total condenser)

xD 1 x W
log
1 xD x W
Nmin =
log av

av = average value of relative volatility


= (1W)
1= relative volatility of the overhead vapour
W= relative volatility of the bottom liquid
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Example 11.4-2

For the rectification in Example 11.4-1,


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:
(a)Minimum reflux ratio Rmin
(b)Minimum number of theoretical plates at
total reflux.

Example 11.4-2

41.2 kmol/h

At R = , Nmin = ?
Steps are drawn from xD to xW.

xD = 0.95
F =100 kmol/
h
xF = 0.45
58.8 kmol/h
xW = 0.1

Nmin = 5.8 stages or 4.8 trays plus a reboiler


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MINIMUM REFLUX, Rmin


infinite number of stages/trays
minimum vapour flow
minimum condenser & reboiler
Rmin at pinch point (x,y)
or when equilibrium line has an inflection,
operating line tangent to the equilibrium line

Enriching op. line:


x
y = R x+ D
R +1 R +1
y-intercept:
xD
0.95
=
= y intercept
R min + 1 R + 1
min
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Minimum Reflux Ratio


The top operating line intercepts q-line at
equilibrium line.
The line passes through the points (x,y)
and (xD,xD):

OPERATING AND OPTIMUM REFLUX RATIO


Two limits of tower operation exist:
At total reflux
-minimum number of plates with infinite tower diameter
-cost of tower, steam & cooling tower increases.
At minimum reflux
-infinite number of tray
-infinite cost of tower.
So, actual operating reflux ratio lies between total reflux and
minimum reflux (Rmin).
Normally, Ractual=1.2 -1.5 of Rmin

EXAMPLE 11.4-2

For the rectification in Example 11.4-1, 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, deretmine the
following:
(a) Minimum reflux ratio Rmin.
(b) Minimum number of theoretical plates at
total reflux (Nmin).

Example 11.4-2
41.2 kmol/h
xD = 0.95
F =100 kmol/
h

Given R = 4, Rmin = ?
The enriching op. line from xD is drawn
through the intersection of the q-line & the
equilibrium line to intersect the y-axis

xF = 0.45
58.8 kmol/h
xW = 0.1
Enriching op. line:
x
y = R x+ D
R +1 R +1
y-intercept:
xD
0.95
=
= 0.43
R min + 1 R + 1
min
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Rmin = 1.21

SPECIAL CASE DISTILLATION

1.Stripping column distillation


2.Enriching column distillation
3.Rectification with direct steam injection
4.Rectification tower with side streams
5.Partial condensers

STRIPPING-COLUMN DISTILLATION
feed is saturated liquid at boiling point (q=1)
added to the top of the column
overhead product is not returned back to the tower
Wx W
Lm
y
=
x

operating line:
Vm + 1 m V
m +1

Ntheo. stages - starting from xW(on 45o line) draw


a straight line to the intersection of yD with the qline

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ENRICHING-COLUMN DISTILLATION
feed is saturated vapour (q=0)
D

added to the bottom of the column


overhead product is refluxed back to the tower
xD
R
y=
x+
operating line:
R +1 R +1
N theo. stages - starting from xD(on 45o line) draw a
straight line to the y-intercept, xD/(R+1)

xF
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xD

DIRECT STEAM INJECTION


heat provided by open steam injected directly at bottom of tower
steam injected as small bubbles into liquid
W
stripping operating line: y = W x x W
S
S
draw a straight line from (xW,0) through WxW/(W-S) on
the 45o line

use of open steam requires an extra fraction of a stage


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SIDE STREAM
stream removed from sections of tower
side stream above feed inlet:

Ox O + Dx D
LS
intermediate operating line: y = V x +
V
S +1

liquid side stream:

Ln = LS+O

S +1

VS+1 = Vn+1=V1=Ln+D
from the intersection of enriching op. line & xO, draw a
straight line to y-intercept of intermediate op. line

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PARTIAL CONDENSERS
overhead product = vapour
liquid condensate returned to tower as reflux
one extra theoretical stage for partial condenser (both
liquid & vapour in condenser is in equilibrium)

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TRAY EFFICIENCY
3 types of tray efficiency:
Overall tray efficiency, Eo
Murphree tray efficiency, EM
Point/local tray efficiency, EMP
EO = no. of ideal trays
no. of actual trays

EM =

yn - yn + 1
y *n -y n + 1

EMP =

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y'n -y'n + 1
y *n -y'n + 1

TRAY EFFICIENCY
Graphical determination of actual trays given EM:
1 ideal tray = triangle acd on ideal equil. line
1 actual tray = triangle abe on actual equil. line
Eg. EM = 0.6 (60% efficiency)
distance ac = 10 cm
distance ab = 0.6(10 cm) = 6 cm
Get 4-5 points & draw actual
equil. line thru each points
Step off actual trays between
operating & actual equil. lines
Reboiler = 1 stage (bet. ideal equil. &
operating lines
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Problem (Tray efficiency)


No 11.5-1 (pg 755):
For the distillation of heptane and ethyl
benzene in problem 11.4-2, the Murphree
tray efficiency is estimated as 0.55.
Determine the actual number of trays
needed by stepping off the trays using the
tray efficiency of 0.55. Also, calculate the
overall tray efficiency Eo.

Condenser Duty (qc)


Enthalpy Balance Around the Condenser:
V1(H1) =L(hD) + D(hD) + qc
qc=VHD (LhD+DhD)
For total condenser:
V1=VD, HD=H1
H1=the saturated vapor enthalpy (equation 11.6-2):

H1 can also be determined from the enthalpy-concentration diagram

Reboiler Duty (qR)


Overall Enthalpy Balance :
Enthalpy in = Enthalpy out
qR +Fhf = qc + DhD + WhW
qR =qc + DhD + WhW Fhf
hD and hf from equation (11.6-1) or from
the enthalpy-concentration diagram.

Example
Binary mixture A-B (benzene-toluene) is to be distilled in a
fractionation column 101.3kPa. The feed of 100 kgmol/h is
liquid, containing 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. A
Reflux ratio (R) = 1.5Rm. Given that Rm=1.17. Determine
the condenser duty and the reboiler duty required by the
distillation column by assuming constant molar overflow.
Physical property for benzene and toluene and enthalpyconcentration diagram are given in Table 11.6-1(pg 733)
and Table 11.6-2 (pg 734), respectively.

ENTHALPY-CONCENTRATION METHOD
Ponchon-Savarit method
takes into account latent heats, heats of solution & sensible heats
no assumption of molal overflow rates
graphical procedure combining enthalpy & material balances
provides information on condenser & reboiler duties

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Enthalpy-concentration for benzene-toluene


data Table 11.6-2 pg. 734 (Geankoplis 4th Ed.)
calculation shown in eg. 11.6-1

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ENTHALPY-CONCENTRATION METHOD
Drawing isotherms (tie lines) on the enthalpy-concentration diagram from

(a) temperature-concentration diagram (b) x-y diagram


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Example 11.6-2
Given : R = 1.5 Rm = 1.5(1.17) = 1.755

41.2 kmol/
h

F =100 kmol/
h

xD = 0.95

xF = 0.45

58.8 kmol/h

TF = 327.6K

xW = 0.1

1. Plot enthalpy-concentration diagram and x-y diagram on the same sheet of


paper. Locate points D, W and F at xD, xW and xF, respectively.
hF = xFcpA(TF-T0) + (1-xF)cpB(TF-T0)
where cpA = cp of liquid benzene = 138.2 kJ/kmol.K
cpB = cp of liquid toluene = 167.5 kJ/kmol.K
T0 = Tref. = Tb.p. of liquid benzene = 80.1oC
hF= 0.45(138.2)(327.6-353.1) + (1-0.45)167.5(327.6-353.1) = -3938.1 kJ
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Example 11.6-2
1

0.8

0.6

0.4

0.2

140.0
0
0

0.2

0.4

0.2

0.4

0.6

0.8

0.6

0.8

120.0

100.0

80.0

60.0

40.0

20.0

0.0

0.0
- 20.0

- 40.0

- 60.0

- 80.0

- 100.0

- 120.0

- 140.0

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1.0

Locating R
2. Locate rectifying-section difference point,R
QC
hD + H1
D
H
R=
= R 1
H1 hD
Hh

1 D

Sat. vapour

Sat. liquid

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hD+QC/D
R H 1

V1

H1
h DH1

hD

Example 11.6-2
1

QC
hD +
H1
D
H
R=
= R 1
H1 h D
Hh

0.8

0.6

1 D

QC
hD + H1
R H 1
D
R H1
R=
=
= 1.755 =
H1 hD
Hh
1cm

0.4

1 D

R H1 = 1.7551cm = 1.755cm

0.2

140.0
0
0

0.2

0.4

0.6

0.8

120.0

100.0

R =85x

103kJ/kmol

80.0

60.0

H1=31x 103kJ/kmol

V1

40.0

20.0

hW=5x 103kJ/kmol

0.0

- 20.0

- 40.0

- 60.0

- 80.0

- 100.0

- 120.0

- 140.0

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0.0

0.2

0.4

0.6

0.8

1.0

Example 11.6-2
3. Locate stripping-section difference point, S
4. Step off trays for rectifying section using R.
5. Step off trays for stripping section using S
6. Theoretical stages = numbers of tie lines
7. Theoretical trays = theoretical stages - reboiler
Theoretical trays = 11.9 1 = 10.9 trays
8. Feed tray = tie line that crosses the line R FS
Feed trays = tray no. 7 from the top
9. Condenser duty, QC = (R hD)D or

QC

hD +
H1
3-0)41.2 = 3 460 800 kJ/h
Q
=
(85x10
D

R=
H1 h D
10. Reboiler duty, QR = (hW-S)W
QR = (hW-S)W = (5 x 103 [-64x103])58.8 = 4 057 200 kJ.h
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Locating S
Draw a straight line from R through F to intersect the
vertical line at xW

FKKKSA

Example 11.6-2
1

0.8

0.6

0.4

0.2

140.0
0
0

0.2

0.4

0.6

0.8

120.0

100.0

80.0

60.0

40.0

20.0

0.0

0.0

0.2

- 20.0

- 40.0

-64 x103kJ/kmol

- 60.0

- 80.0

- 100.0

- 120.0

- 140.0

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0.4

0.6

0.8

1.0

Stepping off trays for the rectifying section


1

From V1 vertically to 45o


line, horizontally across
to equilibrium line and
vertically
back
to
saturated liquid line, to
give L1. Connect L1 to V1
using a tie line. From L1
to R intersecting the
saturated vapour line to
give V2.Repeat until a tie
line crosses over the line
RFS.

0.8

0.6

0.4

0.2

140.0
0
0

0.2

0.6

0.8

100.0

80.0

60.0

V7 V6 V5 V V V V
1
4
3
2

40.0

20.0

0.0

0.0

0.2

- 20.0

- 40.0

- 60.0

- 80.0

- 100.0

- 120.0

- 140.0

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0.4

120.0

0.4

L7 L6 L5
F

L4
0.6

L3

L2

0.8

L1
D

1.0

Stepping off trays for the stripping section


1

Draw a line from S


through L7 up to the
saturated vapour line to
give V8. From V8
vertically to 45o line,
horizontally
to
equilibrium line and
vertically
back
to
saturated liquid line to
give L8. Connect L8 and
V8
using
a
tie
line..Repeat until a tie
line touches W or exceed
W.

0.8

0.6

0.4

0.2

140.0
0
0

0.2

0.4

0.8

100.0

80.0

60.0

V12

40.0

WL L
12
11 L10

20.0

0.0

0.0

0.2

- 20.0

V11
L9

V10

- 40.0

- 60.0

- 80.0

- 100.0

- 120.0

- 140.0

V9

L8 L7 L6 L5
F

0.4

No. of theoretical stages = no. of tie lines = 11.9 stages


FKKKSA

0.6

120.0

V8 V7 V6 V5 V V V V
1
4
3
2
L4
0.6

L3

L2

0.8

L1
D

1.0

MINIMUM REFLUX RATIO, Rmin


1

Rmin occur when the line RFS


coincides with the tie line that
passes through F

0.8

0.6

0.4

Get a tie line that passes through


F and extend that line to
intersect the vertical line xD to
get Rmin

0.2

140.0
0
0

0.2

0.4

0.6

0.8

120.0

100.0

QC
hD + H1
D min
H
Rmin =
= Rmin 1
H1 hD
Hh

1 D

60.0

40.0

20.0

0.0

0.0
- 20.0

- 40.0

- 60.0

- 80.0

- 100.0

- 120.0

- 140.0

FKKKSA

Rmin

80.0

0.2

0.4

0.6

0.8

1.0

MINIMUM STAGES, Nmin


1

0.8

Nmin is obtained when the


operating lines are vertical since
R and S are at infinity.

0.6

0.4

Nmin = 5.9 stages

0.2

140.0
0
0

0.2

0.4

0.2

0.4

0.6

0.8

0.6

0.8

120.0

100.0

80.0

60.0

40.0

20.0

0.0

0.0
- 20.0

- 40.0

- 60.0

- 80.0

- 100.0

- 120.0

- 140.0

FKKKSA

1.0

PARTIAL CONDENSER
yD

Distillate product, VD vapour with the composition yD


Condensed liquid/reflux, L0, have the composition xo
which is in equilibrium with yD
0.8

0.6

Partial condenser = 1 stage

0.4

0.2

140.0
0
0

0.2

0.4

0.6

0.8

x0

120.0

100.0

80.0

60.0

V6 V5 V4 V V V V
D
3
2
1

40.0

20.0

0.0

0.0

0.2

- 20.0

- 40.0

- 60.0

- 80.0

- 100.0

- 120.0

- 140.0

FKKKSA

0.4

L6 L5 L4
F

L3
0.6

L2

L1

0.8

L0
1.0

PARTIALLY VAPOURISED FEED,zF


1

0.8

F with the composition zF lies on


the tie line LF (composition = xF)
and VF (composition = yF)
0.6

0.4

By trial-and-error, locate the point


F so as to satisfy the inverse lever
rule:
0.2

140.0
0

VF FL F
=
LF FVF

0.2

zF

0.4

120.0

0.6

0.8

1.0

100.0

80.0

60.0

40.0

20.0

0.0

0.0
- 20.0

- 40.0

- 60.0

- 80.0

- 100.0

- 120.0

- 140.0

FKKKSA

0.8

0.2

LF LF

0.4

F
F

VF VF
0.6

MULTICOMPONENT DISTILLATION
more than 2 components
shortcut calculation methods an approximation
only allow separation between two components, heavy key and light key

Equilibrium data
Raoults law for ideal mixture
p P
p P
y B = B = B xB
y A = A = A xA
P P
P P

yC =

pC PC
= x
P P C

yD =

pD PD
= x
P P D

hydrocarbon system:
yC = K CxC

y B = K B xB

y A = K AxA

y D = K Dx D

where KA = vapour-liquid equilibrium constant or distribution coefficient


relative volatility, i :

A =

KA
K ref.

B =

KB
K ref.

C =

KC
K ref.

D =

FKKKSA

KD
K ref.

Example 11.7-2
F = 100 mol/h at boiling point at 405.3 kPa. xFA = 0.4, xFB = 0.25, xFC = 0.20 and
xFD = 0.15 where components A = n-butane, B = n-pentane, C = n-hexane and
D = n-heptane. 90% of B is recovered in the distillate and 90% of C in the
bottoms. Calculate: (a) D and W moles/h (b) dew point of distillate and
boiling point of bottoms (c) minimum stages for total reflux and distribution
of other components in the distillate and bottoms.
Solution:
1st trial: Assume all of component A will be in the distillate and all of component
D will be in the bottom product
Components

xF

xFF

yD

yDD

A
B(L)
C(H)
D

0.40
0.25
0.20
0.15

40.0
25.0
20.0
15.0
F=100

0.62
0.349
0.031
0
yD=1.00

40.0
22.5
2.0
0
D=64.5

FKKKSA

xW

xWW

0
0
0.070
2.5
0.507
18.0
0.423
15.0
xW=1.00 W=35.5

Assume all A go to distillate and all D go to the bottoms.


yAD(D)=xAF(F)=0.4(100)=40 mol/h
xDW(W)=xDF(F)=0.15(100)=15 mol/h
N-pentane(B): Light Key
Overall Balance: F =D+W
Comp Balance:
xBF(F)=0.25(100)=25 mol/h=yBD(D) + xBW(W)
Since 90% of B is in distillate:
yBD(D) = (0.90)(25) = 22.5, xBW(W)=2.5
N-hexane (C): Heavy Key
xCF(F)=0.20(100) =20 mol/h
Since 90% of C is in the bottoms:
xCW(W)=0.90(20)=18 mol/h, yCDD=2.0 mol/h

DEW POINT
For a vapour mixture of A, B, C and D:

yi yi yi

xi = =
=1

K
K
i ref. i
Liquid composition which is in equilibrium with the vapour mixture:
yi

xi =

i

i

1. By trial-&-error, assume Td.p.


2. Get corresponding
values of Ki and i

3. Calculate yi/i
4. From Kref. = (yi/i) , get the corresponding T
5. Compare latest T with assumed T. If differ, use latest T for next iteration
by repeating steps 2-4
6. Once Td.p. is obtained, calculate liquid composition
FKKKSA

Example 11.7-2
Components

xF

xFF

yD

yDD

A
B(L)
C(H)
D

0.40
0.25
0.20
0.15

40.0
25.0
20.0
15.0
F=100

0.62
0.349
0.031
0
yD=1.00

40.0
22.5
2.0
0
D=64.5

xW

xWW

0
0
0.070
2.5
0.507
18.0
0.423
15.0
xW=1.00 W=35.5

Dew point: Assume Td.p. = 67oC (Kref. = KC = (yi/i) = 0.26)


Components

yiD

Ki

A
B(L)
C(H)
D

0.62
0.349
0.031
0
yiD=1.00

1.75
0.65
0.26
0.10

6.73
2.50
1.00
0.385

FKKKSA

yi /i

xi

0.0921
0.351
0.1396
0.531
0.0310
0.118
0
0
yi /i=0.2627 xi=1.00

Example 11.7-2

1.75

0.65

0.26

0.10

FKKKSA

BOILING POINT
For a liquid mixture of A, B, C and D:
yi = Kixi = K ref. ixi = 1
Vapour composition which is in equilibrium with the liquid mixture:
x
yi = i i
x
i i
1. By trial-&-error, assume Tb.p.

2. Get corresponding values of Ki and i


3. Calculate ixi
4. From Kref. = 1/(ixi) , get the corresponding T
5. Compare latest T with assumed T. If differ, use latest T for next
iteration by repeating steps 2-4
6. Once Tb.p. is obtained, calculate vapour composition

FKKKSA

Example 11.7-2
Components

xF

xFF

yD

yDD

A
B(L)
C(H)
D

0.40
0.25
0.20
0.15

40.0
25.0
20.0
15.0
F=100

0.62
0.349
0.031
0
yD=1.00

40.0
22.5
2.0
0
D=64.5

xW

xWW

0
0
0.070
2.5
0.507
18.0
0.423
15.0
xW=1.00 W=35.5

Boiling point: Assume Tb.p. = 132oC (Kref. = KC = 1/ixi = 1.144)


Components

xiw

Ki

xi i

yi

A
B(L)
C(H)
D

0
0.070
0.507
0.423
xW=1.00

4.95
2.34
1.10
0.61

5.00
2.043
1.000
0.530

0
0.1430
0.5070
0.2242
xi i=0.8742
1/ixi = 1.144

0
0.164
0.580
0.256
xi=1.00

FKKKSA

Example 11.7-2

5.00

2.35
1.15
0.61

FKKKSA

MINIMUM STAGES,NMIN AT R =
Minimum stages, Nmin, using Fenske equation:
log
Nmin =

where:

x LD D x HW W

x HD D x LW W

log L ,av

xLD = mole fraction of LK in distillate


xLW = mole fraction of LK in bottom product
xHD = mole fraction of HK in distillate
xHW = mole fraction of HK in bottom product
L,av =

LDLW

LD = relative volatility of LK at dew point.

LW = relative volatility of LK at boiling point.


xiDD
x D
Distribution of other components:
= (i,av )Nm HD
xiWW
xHWW
FKKKSA

Example 11.7-2
Components

yiD=xiD

yDD

xiw

xWW

A
B(L)
C(H)
D

0.62
0.349
0.031
0
yD=1.00

40.0
22.5
2.0
0
D=64.5

6.73
2.50
1.00
0.385

0
0.070
0.507
0.423
xW=1.00

0
2.5
18.0
15.0
W=35.5

4.348
2.043
1.000
0.530

LDLW = (2.50)(2.043) = 2.258

L,av =

LD

HD

x D x HW W

(0.349) 0.507
log

x D x LW W

0.031
0.070
Nmin =
=
= 5.404 theoretical stages

log L ,av
log 2.258
xiDD
x D
Distribution of other components:
= (i,av )Nm HD
xiWW
xHWW
Distribution of component A & D:
x ADD
x D
= (A,av )Nm HD = (A,av )5.404 (0.031)64.5 = (A,av )5.404 0.1111
x AWW
xHWW
(0.507)35.5
log

xDDD
x D
= (D,av )Nm HD = (D,av )5.404 (0.031)64.5 = (D,av )5.404 0.1111
xDWW
xHWW
(0.507)35.5
FKKKSA

Example 11.7-2
Components

yiD=xiD

yDD

xiw

xWW

A
B(L)
C(H)
D

0.62
0.349
0.031
0
yD=1.00

40.0
22.5
2.0
0
D=64.5

6.73
2.50
1.00
0.385

0
0.070
0.507
0.423
xW=1.00

0
2.5
18.0
15.0
W=35.5

4.348
2.043
1.000
0.530

A,av =

ADAW = (6.73)(4.348) = 5.409

D,av =

DDDW = 0.385(0.530) = 0.452

x ADD
x D
= (A,av )Nm HD = (A,av )5.404 (0.031)64.5 = (5.409)5.404 0.1111=1017
x AWW
xHWW
(0.507)35.5

xDDD
x D
= (D,av )Nm HD = (D,av )5.404 (0.031)64.5 = (0.452)5.404 0.1111= 0.001521
xDWW
xHWW
(0.507)35.5
Material balance of component A & D:
x ADD + x AW W = 40
x DDD + x DW W = 15
x ADD = 39.961
x DDD = 0.023
Solving :
x AW W = 0.039
x DW W = 14.977
FKKKSA

Example 11.7-2
Components

xF

xFF

yD

yDD

A
B(L)
C(H)
D

0.40
0.25
0.20
0.15

40.0
25.0
20.0
15.0
F=100

0.62
0.349
0.031
0
yD=1.00

40.0
22.5
2.0
0
D=64.5

xW

xWW

0
0
0.070
2.5
0.507
18.0
0.423
15.0
xW=1.00 W=35.5

Revised distillate and bottoms compositions:


Components

xF

xFF

yD

yDD

A
B(L)
C(H)
D

0.40
0.25
0.20
0.15

40.0
25.0
20.0
15.0
F=100

0.6197
0.3489
0.0310
0.0004
yD=1.00

39.961
22.5
2.0
0.023
D=64.484

FKKKSA

xW

xWW

0.0011
0.039
0.0704
2.500
0.5068
18.00
0.4217
14.977
xW=1.00 W=35.516

MINIMUM REFLUX RATIO,RMIN


Underwoods shortcut method for calculating Rmin:
Assumes constant flows in both sections of tower
Uses constant average (at Tave. = [Ttop + Tbottom ]/2)
x
1q= i iF

i
where:


i
xiD = mole fraction of component i in distillate taken at R =
R m + 1=

i iD

xiF = mole fraction of component i in the feed


i = relative volatility of the top and the bottom of the tower
To determine Rmin:
1. By trial-and-error, assume ( LK HK )
2. Calculate 1-q for various
3. Use obtained to calculate Rmin
FKKKSA

Example 11.7-3

Using the conditions and results given in


Example 11.7-2, calculate the following:
(a)Minimum reflux ratio using the Underwood
method.
(b)Number of theoretical stages at an operating
reflux ratio R of 1.5Rm using the ErbarMaddox correlation.
(c)Location of feed tray using the method of
Kirkbride.

Example 11.7-3
Components

xF

xFF

xiD

xiDD

A
B(L)
C(H)
D

0.40
0.25
0.20
0.15

40.0
25.0
20.0
15.0
F=100

0.6197
0.3489
0.0310
0.0004
yD=1.00

39.961
22.5
2.0
0.023
D=64.484

Tb.p. = 132oC & Tdp = 67oC

xW

xWW

0.0011
0.039
0.0704
2.500
0.5068
18.00
0.4217
14.977
xW=1.00 W=35.516

Tave. = (132 + 67)oC/2 = 99.5oC

Components

xiF

xiD

Ki

xiW

A
B(L)
C(H)
D

0.40
0.25
0.20
0.15
xiF=1.00

0.6197
0.3489
0.0310
0.0004
yD=1.00

3.12
1.38
0.60
0.28

5.20
2.30
1.00
0.467

0.0011
0.0704
0.5068
0.4217
xiW=1.00

FKKKSA

Example 11.7-3

3.12

1.38

o.60

0.28

FKKKSA

Example 11.7-3
Components

xiF

xiD

Ki (99.5oC)

i (99.5oC)

xiW

A
B(L)
C(H)
D

0.40
0.25
0.20
0.15
xiF=1.00

0.6197
0.3489
0.0310
0.0004
yD=1.00

3.12
1.38
0.60
0.28

5.20
2.30
1.00
0.467

0.0011
0.0704
0.5068
0.4217
xiW=1.00

x
5.2(0.4) 2.3(0.25) 1.0(0.2) 0.467(0.15)

1q=
= 1 0=1=
+
+
+



5.20 2.3 1.0 0.467
i
1. By trial-and-error, assume ( LK HK )
2. Calculate 1-q for various

(sum)
5.2(0.4)
2.3(0.25)
1.0(0.2)
0.467(0.15)

(assumed) 5.20 2.3


1.0
0.467

1.210
1.200
1.2096
FKKKSA

i iF

0.5213

0.5200
0.5213

0.5275
0.5227
0.5273

-0.9524

-1.0000
-0.9542

-0.0942
-0.0955
-0.0943

+0.0022
-0.0528
+0.0001

Example 11.7-3
Components

xiF

xiD

Ki (99.5oC)

i (99.5oC)

xiW

A
B(L)
C(H)
D

0.40
0.25
0.20
0.15
xiF=1.00

0.6197
0.3489
0.0310
0.0004
yD=1.00

3.12
1.38
0.60
0.28

5.20
2.30
1.00
0.467

0.0011
0.0704
0.5068
0.4217
xiW=1.00

= 1.2096
3. Use obtained to calculate Rmin

R m + 1=

x
= 5.20(0.6197) + 2.30(0.3489) + 1.00(0.0310) + 0.467(0.15)
5.201.2096 2.301.2096 1.001.2096 0.4671.2096

i
x
R m + 1= i iD =1.395

i

i iD

Rmin = 0.395

FKKKSA

SHORTCUT METHOD NUMBER OF STAGES


Correlation of Erbar & Maddox:

Feed plate location using Kirkbride method:


log

Ne
Ns

= 0.206 log

x
x

HF

LF

W x
D x

LW

HD

where:
Ne = number of theoretical stages above the feed plate
NS = number of theoretical stages below the feed plate
FKKKSA

Example 11.7-3

R = 1.5Rmin = 1.5(0.395) = 0.593


R/(R+1) = 0.593/(0.593+1) = 0.3723
Rmin/(Rmin+1) = 0.395/(0.395+1)
Rmin/(Rmin+1) = 0.2832
Nmin/N = 0.49 = 5.404/N
N = 11.0 theoretical stages

0.37

or 10 theoretical trays plus a reboiler

0.49
FKKKSA

Example 11.7-3
Components

xiF (F=100 mol/h)

A
B(L)
C(H)
D

0.40
0.25
0.20
0.15
xiF=1.00

xiD (D=64.484 mol/h) xiW (W=35.516 mol/h)


0.6197
0.3489
0.0310
0.0004
yD=1.00

0.0011
0.0704
0.5068
0.4217
xiW=1.00

N = 11.0 theoretical stages


Ne + NS = 11.0 theoretical stages
2

x
Wx

Ne
LW

HF


log
= 0.206 log


x
Ns
D
x


HD
LF
2

Ne
0.2 35.516 0.0704
log
= 0.206 log

= 0.07344

0.25 64.484 0.0310


Ns

Ne
= 1.184 Ne = 1.184Ns
1.184NS + NS = 11.0
Ns
NS = 5.0
Ne = 6.0
Feed tray = 6.0 trays from the top
FKKKSA