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Distillation
A separation technique based on differences in boiling point
which results in differences in vapor pressure. It is covered by
chapter 11 in the text book.
Pages to be covered in the text 599-621
Partial pressure (PA) of component A is the pressure that A would exert at the same
temperature, if present in the same volumetric concentration as in the mixture.
Daltons law: Total pressure is equal to the sum of the partial pressures
= iPPRaults law and Henrys law: Relates partial pressure to the liquid phase concentration
Raults law for high values of xi, and Henrys law for low values
iiixPP o=
iiHxP=Raults: Henrys:
Partial pressures, and Daltons,
Raults and Henrys laws
Binary system: equilibrium
Relative volatility:2
1
2
2
1
1
12K
K
xy
xy
=
Where:
( )( )11
11
2
2
1
1
2
112
1
1
yx
xy
xy
xy
K
K
===
121 =+xx 121 =+yyand
( )11 121112
1+
=
x
xy
( )11212
1
1
1y
yx
=
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Vapor liquid equilibrium (VLE):Binary system
Different types types of VLE
Distillatiom
Fn, zi,nVn, yi,n
Ln, xi,n
Stage n
Vn, yi,n
Ln, xi,n
Ln+1, xi,n+1
Vn-1, yi,n-1
Qn
Column
Reboiler
Total-
condensor
F, xF
W, xW
D, xD
rectifier
l
stripper
L
D
LR=Reflux
ratio
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Column: Binary
Balances over thewhole column
Reboiler
Total-
condenser
F, xF
W, xW
D, xDL
Total balance: WDF +=
WDF WxDxFx +=
condenserWDreboilerF QWhDhQFh ++=+Energy balance:
Component balance:
Equilibrium stage:
Binary stagen
Vn, yn
Vn+1, yn+1Ln, xn
Ln-1, xn-1
Total balance: nnnn VLVL +=+ + 11
Energy balance:
Component balance: nnnnnnnn yVxLyVxL +=+ ++ 1111
nnnnnnnn HVhLHVhL +=+ ++ 1111
Equilibrium relation: )( nn xfy =
Equilibrium stage:Binary steg n
Vn, y
n
Vn+1, yn+1Ln, xn
Ln-1, xn-1
It is assumed that there is constant molar overflow
Total balance: VLVL +=+
Energy balance:
Component balance: nnnn VyLxVyLx +=+ + 11
nnnn VHLhVHLh +=+ + 11
Equilibrium relation : )( nn xfy =
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Binary distillation: How many stages
are necessary for separation?
Reboiler
Total-condenser
F, xF
W, xW
D, xDL
1. - Sorels method
algebraic
2. - McCabe-Thieles method
graphical
McCabe-Thieles mehtodConstant molar overflow
upper operating line (system A)
F, xF
W, xW
D, xD
ym+1 xm
yn+1 xn
A
B
y L
Vx
D
Vxn n D+ = +1
R L
D=
V L D= +
L R D=
( )V R D= + 1
y R
Rx
Rxn n D+ = +
++1 1
1
1
McCabe-Thieles mehtod
Constant molar overflow
Draw in the upper operating line
in the equilibrium diagram
y R
Rx
x
Rn n
D+ = +
++1 1 1
x
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
y
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0
xD
upper operating liney
n+1=x
Dx xn D=
y R
Rx xn D D+ =
+
+ =1
1
1
x n = 0
y x
Rn
D+ =
+1
1
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q line
For a two phase feed (assumed in equilibrium)
F hF = LF hL + VF hvwhere,
hF = specific enthalpy of feed
hL = specific enthalpy of saturated liquid
hv = specific enthalpy of saturated vapor
Generalize by defining q:
q = Enthalpy change reqd to vaporize 1 mole of feed/
molar enthalpy of vaporization
= (hv - hF) / (hv - hL)
q > 1Sub-cooled Liquid
q = 1Saturated LiquidhL
0 < q < 12-phase feed
q = 0Saturated Vaporhv
q
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Total reflux
Minimum reflux
Optimum reflux ratio is usually1.2-1.5 times minimum
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Merill R. Fenske, 1932
In the design of any (distillation) column it is importantto know at least two things. One is the minimum
number of plates required for the separation if no
product, or practically no product, is withdrawn from
the column. This is the condition of total reflux. The
other point is the minimum reflux that can be used to
accomplish the desired separation. While this case
requires the minimum expenditure of heat, it
necessitates a column of infinite height. Obviously, all
other cases of practical operation lie in between these
two conditions.
Multi-component distillation
The availability of large electronic computers
has made possible the rigorous solution of
the equilibirum-stage model for
multicomponent, multi-stage distillation
column to an exactness limited only by the
accuracy of the phase-equilibrium and
enthalpy data utilized.
Buford D. Smith, 1973
Binary vs. Multicomponentdistillation
Binary:
Unique equilibrium curve under constant pressure
Feed and distillate compositions for onecomponent known => bottoms product may bechoosen, D and W calculated by MB
Multicomponent:
Equilibrium depends on all components
Not same freedom of choice.
Complete composition of top and bottom productcannot be fixed => trial&error calculations
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Multi-component distillation
Component1
2
3
4
5
.
.
.
LK (Light Key) primary goes overhead
HK (Heavy Key) primarily goes to bottoms
tex
tex
HHK (Heavy Heavy Keys) main component in botten
LLK (Light Light Keys) main component in heads
Separation is between LK and HK
Ex: methanol, ethanol, n-propanol, water & n-butanol. Split between ethanol och water.
Minimum reflux ratio
Binary: Rm gives pinch at F
Multicomp: Two pinches, one in stripping andone in rectifying section
i. If no components lighter than LK;
stripping pinch near feed plate
ii. If no components heavier
than HK; rectifying pinch
near feed plate
F
W
D
M
Ny
LK
xLK
Multi-component distillationShort-cut method
Gillilands correlation (Stages vs Reflux)
Erbar-Maddox correlation (L/V vs. Nmin/N)
Fenskes equation (Nmin)
Underwoods method (Rmin)
Colburns method (Rmin)
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Gillilands correlation
Gilliland found a graphical correlation between N
and Ras a function of Nmin and Rmin :
56680
1750750
1
.
minmin
R
RR..
N
NN
+
=
+
Underwoods method
qx
i r,i
F,ir,i =
1
1+=
Mini r,i
D,ir,i Rx
And r is a reference component
is a root betweenLKand HK
Distillation: Rigorous methods
Fn, zi,nVn, yi,n
Ln, xi,n
stage n
Vn, yi,n
Ln, xi,n
Ln+1, xi,n+1
Vn-1, yi,n-1
Qn
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"Inside-out" algorithm
There is an inner and outer calculation loop for each tray.
In the inner loop there are calculations with
the MESH-equations. These are done using
simplified expression for equilibrium realtions
,etc..
In the outer loop these values are corrected
for the more rigourous expressions.
Example of simplified expressions
T
BAK
KK
r
rrii
=
=
ln
,
Equilibrium:
Enthalpy:*)(
*
TTDCH
HHH
iiii
iii
=
+=
Different flowsheeting programs
ASPEN
ChemCAD
Hysys - Hysim
Pro II
Massball
Gems - Wingems - Mops
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Method
Condenser
Pressure
R/Rmin
LK & HK
"Recovery":
Condenser
Pressure
Number of
trays
Feed tray
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Specification of top and bottom of column
Distillation
and reflux
rates
Temperature
in top and
bottom
Number of interations is usually 20.