Distil Performance

3/15/2011
1
Column Pressure
How do we choose the operating pressure
of a column?

Usually based on:
(i) Temperature of overhead condenser
(ii) Temperature at bottom of column
Turton, 3
rd
edition
Column Pressure
1. If possible use cheapest coolant stream
available cooling water (or air) in the
condenser

2. If by following (1), the bottom temperature is
too high then reduce pressure so that bottom
temperature is acceptable and choose
warmest coolant (refrigerant)
Turton, 3
rd
edition
3/15/2011
2
Column Pressure - example
A column separates A (light) from B (heavy). At what
pressure would you operate this column?

log P*(mmHg) = a - b/(c+T)

A a = 6.80398 b = 803.810
c = 246.990

B a = 6.80896 b = 935.860
c = 238.730
Turton, 3
rd
edition
Vapor pressure
Turton, 3
rd
edition
Distilllation Column Overhead Condenser

A
log P*(mmHg) = 6.80398 - 803.810 /(246.990 + 49)
= 4.0975
P* = 12,516 mmHg = 242 psi

What is pressure and temperature at bottom of the column?
Q
T
32
40-45
49
Top product is ~ pure A
Assume vapor condenses to 49 C (120 F)

T-Q diagram
Condensing media:
For water inlet 32 C (90 F)
Maximum outlet: 45 C (115 F)

X
water
32
40-45
3/15/2011
3
What does AP
tray
depend on?

AP
tray
=
l
g (h
w
+ h
cr
) + k
g
v
o
2

Often this is the dominant
term
AP
tray
is not a function of the
operating conditions.
Turton, 3
rd
edition
Weir height
Contribution from gas flow
through tray orifices
AP
tray

Assume AP
col
= 5 psi : Pressure drop per tray is on the order of 7.6
cm (3 in) of water = 0.0007 bar (0.1 psi)

P
bot
= 242 + 5 = 247 psia = 12,770 mmHg

For B bottom product:
a - b/(c+T) = log(12,770)
T = b/[a- log(12,770)]-C = 935.860/[6.80896 log(12,770)] - 238.730

T = 107.5C

Top product is ~ pure A
Bottom product is ~ pure B
AP
col
= nAP
tray P
bot
= P
top
+ AP
col
Turton, 3
rd
edition
Distillation Column
3/15/2011
4
R.Turton and J.A. Shaeiwitz -
Copyright 2008
7
Number of
trays, n = 31
Turton, 3
rd
edition
Column Pressure
Acrylic Acid from Propylene
6 8
0.16
0.07
47
Why is column operating
under vacuum?
Acrylic Acid production

Why is column operating under vacuum?

Polymerization of acrylic acid above 90C

Must reduce pressure so that P
bot
:
P*(acrylic acid) = a-b/(c + 89 C)
P=0.16 bar

What about AP
col
?
AP
col
= P
bot
P
top
= 0.16 - 0.07 = 0.09 bar

Number of trays, n = 31
AP
tray
= 0.09/31 = 0.003 bar (= 1.2 of acrylic acid)

Turton, 3
rd
edition
3/15/2011
5
Algorithm for establishing Distillation Column
Pressure and Condenser Type
Seider, Ch. 7
Distillate and bottoms
compositions are
known (or estimated)
Calculate bubble-point
pressure (P
D
) of distillate
at 49C (120 F)
[assumes cooling water available at 32 C
(90 F), sufficient to cool and condensate a
vapor to 49 C (120 F)]
P
D
< 215 psia
(1.48 MPa, 14.8 bar)
P
D
> 215 psia (1.48
MPa or 14.8 bar)
Calculate dew-point
pressure (P
D
) of distillate
at 49C (120 F)
P
D
> 365 psia (2.51
Mpa or 25.1 bar)
P
D
< 365 psia
(2.51 MPa,
25.1 bar)
Estimate Bottom
Pressure (P
B
)

(add 10 psia to P
D
)
Choose a refrigerant so
as to operate partial
condenser at 415 psia
(2.86 MPa, 28.6 bar)
Use total condenser
(*)
(reset P
D
to 30 psia if P
D
<30 psia)
(**)

(*)
Unless a vapor
distillate is required
(**)
To avoid near vacuum
operation
Use partial
condenser

Calculate bubble-
point temperature
(T
B
) of bottoms at
P
B

Lower pressure P
D

appropriately
T
B
< bottoms
decomposition
or critical
temperature
T
B
> bottoms
decomposition or critical
temperature
Reboiler T ~ T
b
heavy component
Condenser T ~ T
b
light component
Performance of Separation Units
Distillation columns
scale-up/down
reflux ratio
flooding/weeping
Turton, 3
rd
edition, ch. 18
V
D
B
V
F
L = B + V
L = V - D
R = L/D
R = L/B
L
L
reflux
Boil-up
3/15/2011
6
McCabe-Thiele Analysis
y
x
x
D
/(1+R)
x
D
Feed line slope
= -q/(1-q)
x
B
x
F
Turton, 3
rd
edition, ch. 18
1 +
=
=
+
=
R
R
x y
y x
L D
L
V
L
F D
F D
( )x
x
y
1 1 +
=
o
o
F D
F D
x y
y x
R
=
min
R
R
V
L
achial
+
= |
.
|
\
|
1
Column Pressure and
Temperature
Reboiler temp ~ boiling point of
heavy component
Condenser temp ~boiling point
of light component

Increasing column pressure:
increases both temp.
decreases relative volatility and
hence make separation more
difficult
Slope = L/V
Slope = L/V
V
D
B
V
F
L = B + V
L = V - D
R = L/D
R = L/B
L
L
reflux
Boil-up
Distillation of Benzene from Toluene
Flows in kmol/h
Composition in benzene mole fraction
Reflux ratio=2.38
Pressure = 2 bar

Benzene recovery:
I=DX
D
/(Fx
F
) = 30(0.885)/(100(0.321))=0.827
Diameter = 0.83 m
Contains 20 sieve plates with 0.61 m plate spacing
Feed is introduced in plate 13
Tower operates with a reflux ratio of 2.38
= 70 (mass balance)
X
B
=0.079
1
N
Analyze this operation: Number of theoretical plates?
where is the feed added? Column oversized/undersized? Effect of
changing L/V?
McCabe-Thiele construction:

Speed of computation using
McCabe-Thiele method is far
slower than for process
simulators.
However, it remains an important
analytical tool.

3/15/2011
7
Distillation of Benzene from Toluene
Flows in kmol/h
Reflux ratio=2.38
Pressure = 2 bar

Benzene recovery:
I=DX
D
/(Fx
F
) = 30(0.885)/(100(0.321))=0.827
Diameter = 0.83 m
= 70 (mass balance)
X
B
=0.079
McCabe-Thiele construction yields 13 THEORETICAL stages (12 + reboiler).
Average plate efficiency is 12/20=0.6 (60%)

Feed is added in plate 13 (actual). Equivalent to theoretical plate number 8: 13x0.6=8

R=L/D
q=fraction of feed that is liquid
Turton, 3
rd
edition, ch. 18
1
N
X
B
=0.079
X
D
=0.885
Z
F
=0.321

Some observations from previous process:

-Feed is not being introduced at optimum location in
the column. The optimal location is plate 6
(theoretical) or 10 (6/0.6) actual

-Separation steps near the feed plate are small

3/15/2011
8
Flows in kmol/h
Reflux ratio=2.38
Pressure = 2 bar
I=DX
D
/(Fx
F
) = 30(0.885)/(100(0.321))=0.827
Diameter = 0.83 m
= 70 (mass balance)
X
B
=0.079
R=L/D
Current situation (feed at plate 13 vs optimum at
plate 10):
The tower appears to
be oversized for the
present separation. It
could process a
lower quality of feed
and improve
benzene recovery
Turton, 3
rd
edition, ch. 18
There are more than the optimum # of stages in the
rectifying (top) section: This means that the tower
was designed to process a lower concentration of
feed or to produce a higher concentration distillate
stream (benzene)
Flows in kmol/h
Reflux ratio=2.38
Pressure = 2 bar
I=DX
D
/(Fx
F
) = 30(0.885)/(100(0.321))=0.827
= 70 (mass balance)
X
B
=00.79
R=L/D
Operating line moves away from equilibrium this increases separation of
each stage (larger step size).
Turton, 3
rd
edition, ch. 18
Increasing L/V:
The concentration of benzene in the bottom stream (x
B
) will be lowered
If x
D
remains the same:
Increasing L/V:
3/15/2011
9
Scale-up/down of Column
McCabe-Thiele Analysis
y
x
x
D
/(1+R)
Feed line slope
= -q/(1-q)
x
F
x
D

:
x
B
What happens
when reflux
ratio increases
but number of
trays stays the
same?
Turton, 3
rd
edition, ch. 18
Flows in kmol/h
Reflux ratio=2.38
Pressure = 2 bar
I=DX
D
/(Fx
F
) = 30(0.885)/(100(0.321))=0.827
Diameter = 0.83 m
= 70 (mass balance)
X
B
=0.079
R=L/D
Computer simulation:
Flowrate
(kmol/h)
Mole fraction Concentration
Inputs
F 100 z
F
0.321
Outputs from Simulation
L
0
71.5 X
0
0.885
V
N+1
96.4 y
N+1
0.079
V
1
101.5 Y
1
0.885
L
n
166.4 x
N
0.079
Turton, 3
rd
edition, ch. 18
3/15/2011
10
Mill Situation
(see working example)

You are told that benzene in feed will vary
between 25 and 40%. However, you are
required to keep D and x
D
constant.
You are asked to asses the effect of such
changes in feed concentration on the
operation of the distillation process
Performance
diagrams
3/15/2011
11
Mill Situation:
You are told that benzene in feed will vary between 25 and
45%. However, you are required to keep D and x
D

constant.
Reflux is chosen as dependent
variable (most common way to
regulate the performance of a
distillation column)
Observations (after running a
number of simulations):

For constant recovery I :
As z
F
increases, the reflux L
0

decreases.

For a constant feed
concentration z
F
:
As I increases, the reflux
increases

You can set up a number of other situations
(estimate reflux rate to obtain desired
distillate conditions, etc.)
Example: Find changes needed to get 90%
recovery at same z
F
.
R
e
f
l
u
x

r
a
t
e

Feed mole fraction, z
F
Constant recovery, I
Benzene
recovery:
Base Case
Weeping gas velocity: 0.35 m/s
Flooding gas velocity: 1.07 m/s
Operation
What other factors must we consider when
column operations change?
Capacity of the column to process more or less
material is limited (bounded) by:
Flooding (scale-up)
Weeping (scale-down)
Turton, 3
rd
edition, ch. 18
3/15/2011
12
Operation
J.D. Seader and E.J. Henley, Separation Process Principles, John Wiley and Sons, NY 1998
scale
down
scale
up
Benzene
recovery:
Base Case
Example: Find
changes needed to
get 90% recovery
at same z
F
(0.321)
3/15/2011
13
Benzene
recovery:
Base Case
Turton, 3
rd
edition, ch. 18
Example: Find
changes needed to
get 90% recovery
at same z
F
(0.321)
New Feed rate:
F=x
D
D/z
F
I= 91.9

New reflux L
0

(from figure):
L
0
=81 (point b)

The distillation can be
operated at a recovery
of 0.9; this reduces the
feed that can be
processed by 8.1%
keep D and x
D
constant
Benzene
recovery:
Example: Find the
maximum recovery
possible for the
distillation equipment for
a feed concentration
z
F
=0.275
3/15/2011
14
What if we want to change the feed rate to the
column?
If we want to keep all the purities the same
then the reflux ratio must stay the same.
Scale-down
How do we adjust the condenser and reboiler
so as to keep the reflux ratios the same? (to
keep all the product purities the same

V
D
B
V
F
L = B + V
L = V - D
R = L/D
R = L/B
L
L
reflux
Boil-up
Turton, 3
rd
edition, ch. 18
Top of column
Q
D
= V
D
=D(1+R)
D

Bottom of column
Q
B
= V
B
= B(R-1)
B

What if we do not adjust any of the utility
flows while increasing/reducing the feed to
the column?
Scale-down case
F = B + D
Fx
f
= Bx
B
+ Dx
D

Top of column
Q
D
= V
D
=D(1+R)
D

Bottom of column
Q
B
= V
B
= B(R-1)
B

V
B
V
F
L = B + V
L = V - D
R = L/D
R = L/B
L
L
reflux
Boil-up
Turton, 3
rd
edition, ch. 18
3/15/2011
15
Scale-down of Column
How is the performance altered with a reduction in feed?
(scale down of all flows)
V
B
V
F
L = B + V
L = V - D
R = L/D
R = L/B
L
L
( )
( )
( ) | |
( ) | |
constant
1 1
1 1
1
1
1 , 1 ,
1 , 1 ,
1
2
1
2
1 ,
2 ,
1 ,
2 ,
1
2
1
2
1
2
=
+
+
=
'
'
= =
A
A
=
o i
o i
B
B
steam
steam
lm
lm
h h
h h
U
U
R B
M R B
m
m
T
T
A
A
U
U
Q
Q
T
Reboiler
Q/Q
tot
Steam side (kept constant)
Boil-up, base case
Boil-up, scale-down case
The pressure in the bottom of the column will increase!
The pressure drop is assumed to remain constant after scale-down because the
weir height is not changed.
AT1
AT2
<1
1 ,
2 ,
1 ,
2 ,
cw
cw
cw
p
p
m
m
M
m
m
M
= =
( )
( )
( ) | |
( ) | |
1 ,
8 . 0
1 ,
1 , 1 ,
1
2
1
2
1 ,
2 ,
1 ,
2 ,
1
2
1
2
1
2
1 1
1 1
1
1
o cw i
o i
D
D
cw
p
cw
p
lm
lm
h M h
h h
U
U
R D
M R D
T c m
T c m
T
T
A
A
U
U
Q
Q
+
+
=
+
+
=
A
A
=
A
A
=
Q/Q
tot
T
Condenser
If AP is the same, then P and T in the condenser is increased.
<1
Eqns. are solved for M and T
Condensate (scale-down)
Turton, 3
rd
edition, ch. 18
Scale-down of Column

1 ,
2 ,
1 ,
2 ,
cw
cw
cw
p
p
m
m
M
m
m
M
= =
( )
( )
( ) | |
( ) | |
1 ,
8 . 0
1 ,
1 , 1 ,
1
2
1
2
1 ,
2 ,
1 ,
2 ,
1
2
1
2
1
2
1 1
1 1
1
1
o cw i
o i
D
D
cw
p
cw
p
lm
lm
h M h
h h
U
U
R D
M R D
T c m
T c m
T
T
A
A
U
U
Q
Q
+
+
=
+
+
=
A
A
=
A
A
=
Reduce cw flowrate and

reduce steam pressure
( )
( )
( ) | |
( ) | |
constant
1 1
1 1
1
1
1 , 1 ,
1 , 1 ,
1
2
1
2
1 ,
2 ,
1 ,
2 ,
1
2
1
2
1
2
=
+
+
=
'
'
= =
A
A
=
o i
o i
B
B
steam
steam
lm
lm
h h
h h
U
U
R B
M R B
m
m
T
T
A
A
U
U
Q
Q
V
B
V
F
L = B + V
L = V - D
R = L/D
R = L/B
L
L
Q/Q
tot
T
T
Condenser
Reboiler
Q/Q
tot
Turton, 3
rd
edition, ch. 18
3/15/2011
16
R.Turton and J.A. Shaeiwitz -
Copyright 2008
31
47C and 0.07 bar
Turton, 3
rd
edition
What if we do not adjust any of the utility flows
while increasing/reducing the feed to the column?
Scale-down case
F = B + D
Fx
f
= Bx
B
+ Dx
D

Top of column
Q
D
= V
D
=D(1+R)
D

Bottom of column
Q
B
= V
B
= B(R-1)
B

Material balance control will
adjust D + B to equal F
Same cooling water flow
and steam pressure causes
same amount of
condensation and reboil
what happens to R and R?
R and R will increase what happens to the
separation?
V
B
V
F
L = B + V
L = V - D
R = L/D
R = L/B
L
L
Turton, 3
rd
edition, ch. 18
3/15/2011
17
Operation
For Scale-up
must be aware of flooding limit
normal design is between 75 85% of flooding, so
scale-up window is small
for vacuum operations changes in column pressure
have a large effect on flooding
For Scale-down
weeping becomes an issue at 30-40% of flooding,
depending on type of tray
generally can avoid weeping problems by using higher
than necessary condenser and reboiler duties
Turton, 3
rd
edition
Number of Sequences of Ordinary Distillation Columns
Benzene, T
b
=80.1 C
Toluene, T
b
110.8 C
Biphenyl, T
b
=254.9 C
Most volatile,
taken as
overhead
Toluene, Tb 110.8 C
Biphenyl, Tb=254.9 C
Least volatile
Pure products produced (large
differences in volatility)
Other separation sequences are
possible!
ethylenzene
p-Xylene
m-Xylene
o-Xylene
p-Xylene
m-Xylene
o-Xylene

Non-pure products produced
(p- and m- xylene T
b
s are
separated by only 0.8 C)
Seider, Ch. 7
3/15/2011
18
Synthesis of all possible ordinary distillation sequences for multicomponent feed that is to
be separated into P final products (nearly pure components or multicomponent mixtures)
Lets order the feed components in decreasing volatilities and assume that this correlates with the normal
boiling point (near ideal liquid solution).

We come up with an equation for the number of different sequences of ordinary
columns N
s
to produce a number of products P:

For example, for P=5 (A, B, C, D, E), the number of separation points is 5-1=4:
A-B, B-C, C-D, D-E
j= # of final products that must be developed from the distillate of 1
st
column
Thus P-j is the # of final products that must be developed from the bottoms of the first
column.

Let N
i
= the # of different sequences for I final products (thus, the number of sequences for
a given separation point in the 1
st
column is N
j
N
P-j
. Note that in the first separator P-1
different separation points are possible.

Thus, the number of different sequences for P products is:

| |
)! 1 ( !
)! 1 ( 2
1
1

= =
=

P P
P
N N N
P
j
j P j s
Seider, Ch. 7
| |
)! 1 ( !
)! 1 ( 2
1
1

= =
=

P P
P
N N N
P
j
j P j s
Number of different sequences for P products:
Number of
Products, P
Number of
separators in the
sequence, (P-1)
Number of
different
Sequences, N
s
2 1 1
3 2 2
4 3 5
5 4 14
6 5 42
7 6 132
8 7 429
9 8 1430
10 9 4862
Seider, Ch. 7
3/15/2011
19
Number of
Products, P
Number of
separators in
the sequence,
(P-1)
Number of
different
Sequences,
Ns
2 1 1
3 2 2
4 3 5
5 4 14
6 5 42
7 6 132
8 7 429
9 8 1430
10 9 4862
Direct sequence
(commonly used in
industry)
pure" distillates (free of high-boiling compounds)
If purity of D is
critical: add
rerun (or
finishing)
column
Sequence 2
Sequence 3
Sequence 4
Sequence 5: Indirect Sequence
(least desirable due to difficulties in achieving
purity for bottom products) Seider, Ch. 7
Heuristics for Determining Favorable Sequences
For P=3 or 4: designing and costing all sequences can be best to choose the most
economical one. However, in most case the direct sequence is often the choice.

Otherwise, use following heuristics:
1 Remove thermally unstable, corrosive, or chemically reactive
components early in the sequence
2 Remove final products one by one as distillates (direct
sequence)
3 Sequence separation points to remove, early in the
sequence, those components of greatest molar % in the feed
4 Sequence separation points in the order of decreasing
relative volatility so that the most difficult splits are made in
the absence of the other components
5 Sequence separation points to leave last those separations
that give the highest-purity products
6 Sequence separation points that favor near equimolar
amounts of distillate and bottoms in each column
When energy costs are high,
this heuristics often leads to
the most economical
sequence.
Note the marginal vapor Rate Method, Chapter 7 Seider
Seider, Ch. 7
3/15/2011
20
Example:
Large variations in relative volatility and
molar % in process feed. Heuristics 4
dominates over heuristic 3 and leads to
this sequence.

H4: Sequence separation points in the
order of decreasing relative volatility so
that the most difficult splits are made in
the absence of the other components
Seider, Ch. 7

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3/15/2011

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