CHE 306

Chapter 3: Introduction to Column

Distillation
Dr. Sagheer Onaizi
 Distillation
 Over 90% of separations are done using
distillation
 Over 40,000 distillation columns operate in
the USA alone

2
 Distillation Cascade (1)

 Flash distillation is simple BUT Rich in light (more volatile) component(s)

produces a limited amount of
separation Compressors
 One can achieve more
separation by cascading more
flash separators
 Send vapor streams to
additional flash chambers with
increasing pressure
 Send liquid streams to
Throttle valves
additional flash chambers with
decreasing pressures
Rich in heavy (less volatile) component(s)
 Distillation Cascade (2)

 P1>P2>P3>P4>P5 Rich in light (more volatile) component(s)

 T1=T2=T3=T4=T5
Compressors
 V1 and L5 have high and low
concentrations of the more
volatile component, respectively
 What to do with all other streams?
 Solution: use intermediate
streams as additional feeds within
the same cascade
 For example: V4 is fed to stage 3 Throttle valves
after compression to higher
Rich in heavy (less volatile) component(s)
pressure
 Distillation Cascade (3)

 Only two product streams (V1 and

L5) are obtained in high yield and
high purity
 BUT:
 This isothermal distillation requires
large number of compressors (very
expensive)
 Solution:
 Operate at constant pressure
and force temperature to vary.
P1>P2>P3>P4>P5  Heat exchangers (which are much T1<T2<T3<T4<T5
T1=T2=T3=T4=T5 cheaper than compressors) can be P1=P2=P3=P4=P5
used to vary (heat or cool)
temperatures of the intermediate 5
streams
 Distillation Cascade (4)

 Problems: (Distillate)
 Many cascaded flash units will
be required to obtain high purity
V1 and L5
 Operation and design is
complicated
 Solution:
 Condense part of V1 and return
to stage 1 and evaporate part of
L5 and return to stage 5. (Bottom)
T1<T2<T3<T4<T5 T1<T2<T3<T4<T5
 Use reflux and boilup streams
P1=P2=P3=P4=P5 P1=P2=P3=P4=P5
to control liquid and vapor flow
rates in the column 6
 Distillation Cascade (5)

(Distillate)  Problem: (Distillate)

 Huge amount of energy will

be required to cool and heat
streams between stages
 Solution:
 Utilize the heat in the rising
vapor to evaporate light
component(s) in the falling
(Bottom)
liquid
T1<T2<T3<T4<T5  Heavy component(s) in the (Bottom)
P1=P2=P3=P4=P5 T1<T2<T3<T4<T5
vapor will condense due to P1=P2=P3=P4=P5
the reduction of the vapor 7
 Distillation Cascade (6)

(Distillate)
 Problems:
 Many heat exchangers will be required
to cool and heat streams between
stages
 Many flash drums
 Solution:
 Contact liquid with vapor in order to
directly utilize the heat in the rising
vapor to evaporate light component(s)
in the falling liquid without using heat
exchanger except at the top and
bottom stages
 Build a single column instead of many
(Bottom) separate single stages
T1<T2<T3<T4<T5  All heat required for distillation is This is a Distillation column
P1=P2=P3=P4=P5 applied to the bottom reboiler
 All required cooling is done in the top 8
condenser
 Distillation Column
Because of the repeated vaporizations and
condensations as we go upward in the
column, the top product (distillate) can be
highly concentrated (rich) in the more Rectifying
volatile component (enriching)
Section
The bottom product (bottoms) is highly
concentrated in the less volatile Feed stage
component, since the more volatile Stripping
component has been stripped out by the Section
rising vapors.
KiV/L > 1 Component i tends to
exit in the distillate
KiV/L < 1 Component i tends to
exit in the bottom
https://www.youtube.com/watch?v=iahkOxbZ4Rk 9
Distillation Column: Some
Limitations
 If the relative volatility is close to
unity or if there is an azeotrope,
little separation will take place
 If thermo‐sensitive components
are present, one has to use
vacuum or steam distillation
 If chemical reactions between
components take place in the
column, more complex reactive
distillation column has to be
designed. 10
 Distillation Equipment (1)
 Columns are built in metal
and have circular cross‐ sections
 Trays (stages) are built so that
liquid‐vapor contact occurs
 Sieve trays are sheets of metal
with holes punched into them to
allow vapor to pass through
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 Distillation Equipment (2)
Liquid flow down from tray
above in a downcomer
Liquid is contacted with
vapor as it flows across the
sieve tray
Rising vapor prevents
liquid from dripping
downward
Metal weir allows a
sufficient liquid level on
each tray 12
 Distillation Equipment (3)
The metal weir acts as a dam to
keep a sufficient level of liquid on
the plate (tray).
The liquid that flows over the weir
is a frothy mixture containing a lot
of vapor.
The vapor disengages in the
downcomer so that clear liquid
flows into the stage below.
The space above the tray allows for disengagement of liquid
from vapor and needs to be high enough to prevent excessive
entrainment (carryover of liquid from one stage to the next).
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 Distillation Equipment (4)
 Space between plates (called tray spacing) is
designed so that it avoids excessive entrainment
 Characteristics of the bubble regime:
 Low gas flow rates
 Liquid pool with rising gas bubbles
 Poor mixing
 Low efficiency
 Undesirable in commercial applications
 Characteristics of the foam regime:
 Higher gas flow rates
 Liquid phase is continuous with rapidly rising distinct gas
bubbles

There is a distinct foam, which has a large surface
area
 Higher efficiency
 Foam can fill entire space between stages leading to 14
excessive entrainment and column may flood
 Distillation Equipment (5)

 Characteristics of the froth regime:

 Higher vapor flow rate than foam regime
 Liquid flow is continuous with large pulsating voids
of vapor rapidly passing through
 Violent boiling at liquid surface and considerable Forth regime
splashing (liquid phase is continuous)
 Thoroughly mixed liquid phase
 Good efficiency if mass transfer is controlled by
liquid phase resistance
 Usual regime in commercial applications
 Characteristics of the spray regime:
 At even higher vapor flow rate than the froth regime
 Vapor phase is continuous
 Liquid occurs as discontinuous spray of droplets Spray regime
 Vapor is very well mixed but liquid droplets are not (gas phase is continuous)
 Low efficiency 15
 Distillation Equipment (6)

Small changes in the vapor flow rate may shift

the froth regime to either foam or spray
regime, which are undesirable.

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 Distillation Equipment (7)

Valve trays and bubble‐cap trays

 Partial condenser (instead of total

condenser)
 Total reboiler (instead of partial

reboiler)
 Multiple feeds
Side‐stream withdrawals
Intermediate reboilers or/and

condensers
Measurement (e.g., flow 17
 Heuristics
 Column pressure is desirable to be greater
than or equal to 1 atm because:
 Vacuum columns are more expensive
 There is little increase in column costs for pressures
between 1 and 7 bar
 The condenser pressure should be set so that
cooling water can be used in the condenser
 The reboiler pressure should be set so that
available steam or other hot utility can be
used for heating 18
 Specifications

Usual specified variables are:

 Column pressure
 Feed flow rate
 Feed composition
 Feed temperature or enthalpy or quality
 Reflux temperature or enthalpy (usually
reflux is saturated liquid)

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 Solving Distillation
Problems
In distillation, two types of problems are considered

Column
Design problems Simulation problems is already
built
Desired separation is set Predict how much
separation can be
Column is designed in achieved by manipulating
order to achieve the some parameters
desired separation
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Specifications and Calculated Variables for
Binary Distillation for Design Problems

V
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Specifications and Calculated Variables for
Binary Distillation for Simulation Problems

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 External Column Balances
(1)
 We will derive mass and
energy balances around the
entire column in order to compute:
D, B, QR and QC
 For binary systems, one can solve
these without doing stage‐by‐stage
calculations
 Column is assumed to be adiabatic
and operates at constant pressure
 Design problem: solve for D and B
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 External Column Balances
(2)

}
Overall mass balance:
F  BD
Mass balance on the
more volatile component:

Fz  BxB  DxD

 z  xB   xD  z 
D    F B    F
 xD  xB   xD  xB  24
 External Column Balances
(3)
Overall Energy balance: Condenser Energy balance:
V1 H1  V1hD  QC  QC  V1 H1  hD   V1
FhF  QR  DhD  BhB  QC
 z  xB   xD  z 
 L0  z  xB  D    F B    F
QC  1    F  xD  xB   xD  xB 
 D  xD  xB 
 L0 
QR  DhD  BhB  FhF  1   D V1  ( D  L0 )  1  L0 / D D
 D
 z  xB   xD  z   L0  z  xB 

QR   
 
FhD   
 FhB  FhF  1    F
 xD  xB   xD  xB   D  xD  xB 

In Condenser: energy is lost from process stream to utility stream

In Reboiler: energy is supplied from utility stream to process stream
 Points to Consider (1)
 Enthalpy (hi) is a state function that obeys Gibbs
phase rule [for binary system (C=2), one phase
(P=1), then 3 degrees of freedom (F = 3): T, P, and
composition].
F=C-P+2
 Stream V1 enters the condenser and experiences
ONLY a phase change => composition remains
unchanged (y1=xD=xo)
 D and Lo are both liquids (if a total condenser is
used) with the same composition => their enthalpies
are also the same (hD = ho) 26
 Example 3.1
A steady-state staged distillation column is to be used to
separate ethanol from water. The feed is a 30 wt% ethanol
and 70 wt% water mixture at 40 °C. Flow rate of feed is
10,000 kg/h. The column operates at a pressure of 1
kg/cm2 (= 1 atm). The reflux is returned to the column as a
saturated liquid. A reflux ratio of L/D = 3.0 is being used.
We desire a bottoms composition of xB = 0.05 (weight
fraction ethanol) and a distillate composition of x D = 0.80
(weight fraction ethanol). The system has a total condenser
and a partial reboiler.
Find D, B, Qc, and QR. 27
Solution (1)

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 Solution (2)

330

90
30 60

29
Solution (3)

30
End of Chapter 3

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