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15-Oct-13

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Material covered
Continuous Multistage Distillation
1. Column design; reflux ratio determines the top and
bottom product compositions
2. Assumptions of the McCabe-Thiele method:
- Constant molal overflow (constant molar latent heat)
- No heat losses
- No heat of mixing
3. Determine graphically the number of stages needed
for a given separation knowing the reflux ratio and the
feed condition
1 1
1
+
+
+
=
+
R
x
x
R
R
y
D
n n
Top Operating Line (TOL)
b
W
b
b
m m
V
W
x
V
L
x y =
1
Bottom Operating Line (BOL)
F
x
q
x
q
q
y
1
1
1

=
q-line
Material covered
L
t
, V
t
L
b
, V
b
Feed
McCabe-Thiele Method
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2. Draw q-line
3. Draw TOL from chosen
value of R
4. Now draw BOL
6. Count the number of
stages
there are 6 stages
required for this
particular reflux ratio
x
D
x
W
Material covered
McCabe Thiele Method
1. Identify (x
F
, x
F
), (x
D
, x
D
)
& (x
W
, x
W
)
5. Draw steps between
operating lines and
equilibrium curve
(x
W
, x
W
)
(x
F
, x
F
)
(x
D
, x
D
)
1
2
3
4
5
6
Distillation Column Design
McCabe-Thiele: a graphical method to estimate the # of stages
Assumptions of McCabe-Thiele method. Constant molal overflow
Equilibrium (x-y) data y vs. x on the same plate
Top Operating Line (TOL) y vs. x on different plates at top section
Bottom Operating Line y vs. x on different plates at bottom section
q-line y vs. x on feed plate
Fundamental assumptions and limitations: make sure to understand
them when designing a distillation process
R determines gradient of TOL
What are the theoretical limits of the reflux ratio?
Influence of the reflux ratio on the separation
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Limiting Operating Conditions: Total Reflux
occurs when all top product return as
reflux, D=0 (no top product removed)
used for starting up columns; for keeping
column operating when other part of the
plant is shut down; for testing column
efficiency
L
0
Column
Reboiler
Condenser
Reflux
Heat out
Heat in
At total reflux (infinite R) TOL has a gradient of 1
TOL becomes y = x (45 diagonal line)
If R = , what happens to the TOL?
1 1
1
+
+
+
=
+
R
x
x
R
R
y
D
n n
What is R value in this case?
D
L
R
0
=
=
The TOL is the same as
the y = x line.
x
W
x
D
4 stages needed vs. 6
stages previously
At total reflux:
minimum number of
stages required for given
separation
but no product is formed!
Limiting Operating Conditions: Total Reflux
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x
W
x
D
Decreasing R, increases
the gradient of TOL
R=0
eventually TOL, q-line
and equilibrium curve meet
at a point Pinch Point
How many stages are
required at R
min
?
Limiting Operating Conditions: Minimum Reflux
steps get smaller & smaller
as pinch point is approached
Decreasing R
q

l
i
n
e
Pinch Point
Find R
min
from either the
gradient or intercept of
TOL:

1 R
x
Intercept
min
D
+
=
infinite number of stages
Intercept
Pinch Point
How to find R
min
in this case?
x
D
TOL at R
min
does not intersect
with the q-line and equilibrium
curve
In this case, R
min
is dictated
by the presence of a pinch-
point
Limiting Operating Conditions: Minimum Reflux
q

l
i
n
e
For highly non-ideal binary
mixture, the pinch point may
occur at a stage above or
below the feed stage.
Gradient of TOL cannot be
reduced further as it would
cross over the equilibrium
curve. This violate 2
nd
law of
thermo because of a reversal
in the mass transfer direction.
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V increases as R increases for a
given top product flowrate, D
How to achieve a higher value of V?
Vaporise more liquid in the reboiler at the
bottom of the column more energy required
How to change the reflux ratio?
Effect of Reflux Ratio
D L V
0
+ =
D
L
R
0
=
( )D R V 1 + =
D
V
Distillate
Bottom W
L
0
Feed
Reboiler
Condenser
Reflux
Heat out
Heat in
At TOTAL REFLUX (R=,V=L) minimum number of theoretical
stages required, but no top product.
Effect of Reflux Ratio
short column with large diameter; thus, lowest capital cost
infinite sizes of condenser, reboiler and column diameter;
thus, infinite operating cost
At MINIMUM REFLUX (R=R
min
) maximum product off-take, but an
infinite number of stages needed.
tall column with small diameter; thus, infinite capital cost
minimum vapour flow in column; hence minimum reboiler
and condenser sizes. Thus, lowest operating cost
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Trade off Between Tray Number and Reflux
Two limiting conditions:
minimum reflux ratio, R
min
minimum number of trays, N
min
many columns can be used to
make exactly the same separation
Asymptotes show the limiting
conditions:
- as R R
min
, # of trays
- as R , # of trays minimum
column at point B is short
and fat, cheaper to construct
but uses lots of energy
Any point along the curve?
column at point A is tall
and thin, uses little energy but
expensive to construct
R
min
N
u
m
b
e
r

o
f

t
r
a
y
s
B (short
column)
N
min
A (tall column)
Reflux ratio
Optimum Reflux Ratio
R
min
C
o
s
t
s

Total cost
Operating cost
Capital cost
R
optimum
Is there an optimum reflux ratio?
Reflux ratio
Optimum reflux ratio is the R which minimizes total cost;
f(energy and material of construction costs)
Typically R = 1.05 1.3 times R
min
with 1.2 R
min
being a good rule of thumb
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the stage at which a
change in gradient between
TOL and BOL occurs
In this case, the feed is
introduced on the 5
th
stage
from the top
Where to introduce the Feed?
Feed
Reflux drum
Condenser
Distillate D
Bottoms W
Reflux L
0
Boilup V
b
Flow, x
D
F, x
i
,T, P,
phases?
Flow, x
W
L
b
V
t
R (L
0
/D)
Feed conditions
x% of F = vapour
x
boilup ratio
(V
b
/W)
Reboiler
Related to
operating T and P
Design Considerations
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What determines the pressure at which the column operates?
Feed
Reflux drum
Condenser
Distillate D
Bottoms W
Reflux
L
0
Boilup V
b
Flow, x
D
F, x
i
,T,
P,
phases
?
Flow, x
W
L
b
V
t
Reboiler
- Feed conditions
T P - VLE equilibrium
P related to T
distillate
What if P = P*
MVC
?
- Condenser & coolant
T related to P
What if T < T
bubble
?
What if T > T
decomposition
?
- Reboiler
Design Considerations: Operating Pressure
The ethanol-water system
exhibits an azeotrope
This occurs at the point
where y
i
= x
i
Conventional distillation is
therefore limited by the
presence of an azeotrope
Azeotropes
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Changing the operating pressure can change the VLE, and can
potentially remove the azeotrope:
This forms the basis of pressure-swing distillation, although there
are a number of other techniques for overcoming the azeotrope
Azeotropes
P
1
Azeotrope
x 1 0
1
y
P
2
x 1 0
1
y
Which of the 2 condenser arrangements will give a top product as vapour?
Vapour leaving partial condenser
has composition different from
vapour entering (y
D
x
0
)
Partial condenser acts as a
stage
Total
condenser
Partial
condenser
Design Considerations: Condenser
Liquid leaving total
condenser has same
MVC composition as
vapour entering (x
D
= y
1
)
x
D
y
1
y
1
y
D
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Design Considerations: Condenser
Most common is a horizontal shell-and-tube heat
exchanger with cooling water in tubes and condensing
vapour in shell.
If condensate is very corrosive, or operating pressure high,
cooling water can be in shell and condensing vapour in
tubes.
A separate reflux drum to collect condensate and control
split between reflux and top product.
Normally all vapour is condensed but occasionally a partial
condenser is used.
Enough vapour is condensed to provide reflux, with
uncondensed vapour forming the top product.
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What is the key difference between the 2 types of reboiler arrangements shown below?
Total reboiler: all the
incoming liquid is converted
to vapour no change in
composition
Partial reboiler: the vapour
leaving is in equilibrium with
the bottom product
acts as a stage in the
distillation column,
Design Considerations: Reboiler
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Kettle Reboiler
Tube bundle at bottom of the shell; covered by the liquid to be boiled, leaving a
vapour space above it.
Heating fluid, normally steam is on the tube side.
Liquid from the bottom of the column is passed to the boiler and the vapour
generated returned to the column.
The remaining liquid forms the bottom product and is normally removed over a weir.
Vapour returned to column is in equilibrium with the bottom product, hence the kettle
reboiler acts as one theoretical stage.
Sometimes, the bundle is placed directly in the bottom of column to avoid piping.
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Thermosyphon Reboiler
Liquid withdrawn from bottom of column, and partially vaporised in the reboiler.
Both vapour and liquid are returned to the column as a two-phase mixture.
Phase separation only occurs in the column, above the liquid level in the base.
Vertical and horizontal thermosyphon are used. In vertical type, liquid to be boiled is
on tube side while heating fluid on shell side.
Bottom product normally drawn at the column base. This stream is not in equilibrium
with the vapour, so the thermosyphon reboiler acts as less than a theoretical stage.
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Fh
F
+ Q
R
= Dh
D
+ Wh
W
+ Q
C
+ Q
lost
Overall energy balance:
= 0
Energy balance over total condenser:
Q
C
= V
t
H
vap
Energy balance over partial reboiler:
Q
R
= V
b
H
vap
What about partial condenser / total reboiler?
where H
vap
= average molar heat of
vaporization of the cpns being separated.
Calculations can also be made using both
heats of vaporization knowing the
compositions of the streams
If saturated liquid feed: Q
R
~ Q
C
Design Considerations: Heat Duties
Total condenser
D
W
F
Partial reboiler
V
t
L
b
V
b
L
0
Q
C
Q
R
Example 1
A continuous distillation column is used to separate a mixture
containing 40 mol% A and the rest B to give a distillate of 95 mol%
A and bottom product of 96 mol% B. The column is operated at
1.5 times the minimum reflux ratio and at 1 atm pressure. It has a
total condenser and a partial reboiler The feed is an equimolar
mixture of liquid and vapour. Assume the mixture has a relative
volatility of 2.2, determine the number of theoretical plates and
location of the feed plate.
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Continuous multistage distillation
1. What are the limiting conditions for distillation? How
to determine the minimum reflux ratio?
2. Where to introduce the feed?
3. What are the additional elements that should be
considered in the design of a continuous distillation
column?
What have you learnt?