DISTILLATION COLUMN

Presenter: Dr. N.C. Trinh, Vietsovpetro JV

January 2021 [email protected]; Tel.: +84764147113
 Table of contents
2

1. Introduction. Learning outcomes

2. Types of distillation columns
3. Distillation Principles
4. Distillation column design
5. Case study
 References
3

 Charles_E._Thomas]_Process Technology Equipment and

Systems
 King (Wiley, 1980) on distillation design
 GPSA
 Kister (McGraw-Hill, 1990) on distillation operation
 Working Guide to Process Equipment 3rd Ed – McGraw-
Hill (2008)
 API training material – Distillation
 Giáo trình Các quá trình và thiết bị truyền khối -
ĐHBKTPHCM
 1. Introduction
4

❖ Distillate water
❖ Distillate mixture of ethanol-water
❖ Separate mixture of benzene –toluene
❖ Separate mixture of n-butane and i-butane
❖ Distillate crude oil
 1. Introduction
5

❖ For what purpose

distillation column is used?
❖ Why do people have to
use distillation column?
 The function of distillation
column types is to allow
lighter components to rise
up the column while heavier
components drop down or,
in other words, to separate
the various components in
the mixture by their boiling
points Distillation column March 2019
 1. Introduction
6

Definition of distillation
 Distillation is a widely used method for separating
mixtures based on differences of boiling point/
vapor pressure.
 To separate a mixture of liquids, the liquid can be
heated to force components, which have different
boiling points, into the gas phase.

 it consumes enormous amounts of energy, both in terms

of cooling and heating requirements
 it can contribute to more than 50% of plant operating
costs
 Learning outcomes
7

❖ After this lecture you should be able to:

• Know about types of distillation column. Advantages
and disadvantage of each type
• Describe the principles of distillation
• Identify equipment used for a distillation system
• Working of crude distillation column
• How to design a distillation column for binary system
 2.Types of distillation column
8

 Batch Columns
In batch operation, the
feed to the column is
introduced batch-wise.
That is, the column is
charged with a 'batch'
and then the
distillation process is
carried out. When the
desired task is
achieved, a next batch
of feed is introduced.
 2.Types of distillation column
9

 Continuous Columns
In contrast, continuous columns process a continuous
feed stream. No interruptions occur unless there is a
problem with the column or surrounding process units.
They are capable of handling high throughputs and
are the most common of the two types. We shall
concentrate only on this class of columns.
 2.Types of distillation column
10

Types of Continuous Columns

Continuous columns can be further classified according
to:
 the nature of the feed that they are processing,
binary column - feed contains only two
components
multi-component column - feed contains more
than two components
 the number of product streams they have
multi-product column - column has more than
two product streams
 2.Types of distillation column
11

Packed versus Plate Columns

-tray column - where trays of various designs are used to hold up the liquid to provide
better contact between vapor and liquid, hence betterseparation.
-packed column - where instead of trays, 'packings' are used to enhance contact
between vapor and liquid.
 For D < 0.6m packing is  Plates can be easier to
cheaper clean
 Packing can be made from  Packing can break more
inert/chem. resistant material so easily
good for corrosive  High liquid rates more
 Good efficiency with low ΔP so economical in plate column
good for vacuum  Low liquid rates less of a
 Packed column copes better with problem in plate column
foaming liquid (incomplete wetting of
 Holdup of liquid is low packing)
 2.Types of distillation column
12
 Packed Column

• Diameter < 4 ft
• Cannot handle dispersed solids in feed
• No interstage cooling
• Limited operating range
• not suitable for large temperature variations
• cheaper to construct
• design database is poor
• cheaper if corrosive fluids are involved
• pressure drop is smaller (good in vacuum operation)
Packed Column
 3. Principles of distillation
15

The liquid mixture will have different boiling point characteristics. Therefore, distillation
processes depends on the vapor pressure characteristics of liquid mixtures.

Vapour Pressure and Boiling

The vapor pressure of a liquid at a particular temperature is the equilibrium
pressure exerted by molecules leaving and entering the liquid surface. Here are
some important points regarding vapor pressure:
 energy input raises vapor pressure
 vapor pressure is related to boiling
 a liquid is said to ‘boil’ when its vapor pressure equals the surrounding pressure
 the ease with which a liquid boils depends on its volatility

 liquids with high vapor pressures (volatile liquids) will boil at lower temperatures
 the vapor pressure and hence the boiling point of a liquid mixture depends on the
relative amounts of the components in the mixture
 distillation occurs because of the differences in the volatility of the components in
the liquid mixture
 3. Principles of distillation
16

The Boiling Point Diagram

The boiling point diagram shows how the equilibrium compositions of the
components in a liquid mixture vary with temperature at a fixed pressure. Consider
an example of a liquid mixture containing 2 components (A and B) - a binary
mixture. This has the following boiling point diagram.

The boiling point of A is that at which the

mole fraction of A is 1. The boiling point
of B is that at which the mole fraction of
A is 0. In this example, A is the more
volatile component and therefore has a
lower boiling point than B. The upper
curve in the diagram is called the dew-
point curve while the lower one is called
the bubble-point curve.
 3. Principles of distillation
17

The dew-point is the temperature at which the saturated

vapour starts to condense.
The bubble-point is the temperature at which the liquid starts
to boil.
The region above the dew-point curve shows the equilibrium
composition of the superheated vapour while the region below the
bubble-point curve shows the equilibrium composition of the
subcooled liquid.
 3. Principles of distillation
18

For example, when a subcooled liquid with mole fraction of

A=0.4 (point A) is heated, its concentration remains constant until it
reaches the bubble-point (point B), when it starts to boil. The vapors
evolved during the boiling has the equilibrium composition given by
point C, approximately 0.8 mole fraction A. This is approximately
50% richer in A than the original liquid.
This difference between liquid and vapor compositions is the
basis for distillation operations.
 Boil and Cool 4 times
Finish Methanol Water VLE

1.0
Boiling a liquid with Xa
0.9
of 0.2 produces a
0.8 vapour with Ya of 0.57
0.7 Boiling a liquid with Xa
Ya (Meth vapour)

0.6 of 0.57 produces a

vapour with Ya of 0.82
0.5
1 2 3 4 Boiling a liquid with Xa
0.4
of 0.82 produces a
0.3 vapour with Ya of 0.93
0.2 Boiling a liquid with Xa
0.1
of 0.93 produces a
vapour with Ya of 0.98
0.0
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Xa (Meth liquid)

Start
Alternatively use T-x-y Diagram

Bubble
Methanol Water VLE (T-x-y)
Dew

105

100

95

90
Temp C

85

80

75

70

65

60
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Xa, Ya (Meth)
How to separate a binary mixture – Pot still

Boil the mixture, condense the vapour and collect the distillate. Repeat the
procedure until the desired purity is obtained.
 Each still is a step on the x-y curve
Methanol Water VLE
4
1.0

0.9 3
Step off each stage
0.8
using the x=y line gives
2
0.7 the same result
Ya (Meth vapour)

0.6
Each step is an ideal
0.5 stage in distillation
1
0.4 4 ideal stages to go
0.3 from 20% Meth to
95% Meth
0.2

0.1

0.0
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Xa (Meth liquid)
 How to improve the pot still?

• Remember that boiling results in a change of

composition, and condensing also results in a change of
composition.
• Therefore, combine the two processes inside the column
to improve the distillation process.
• A distillation column is designed to encourage vapour
liquid contact.
• Falling liquid meets rising vapour. Boiling and
condensing do not just occur in the reboiler and the
condenser. They happen inside the column also.
The Distillation Column
 3. Principles of distillation
25
 3. Principles of distillation
26

VAPOUR LIQUID EQUILIBRIA

Vapor-Liquid-Equilibrium (VLE) Curves
Constant pressure VLE data is obtained
from boiling point diagrams. VLE data of
binary mixtures is often presented as a
plot, as shown in the figure on the right.

 1, 2 x1
y1 =
1 + x1 ( 1, 2 − 1)
 4. Distillation column design
27

 As mentioned, distillation columns are designed using VLE data for

the mixtures to be separated.
 The vapor-liquid equilibrium characteristics (indicated by the shape
of the equilibrium curve) of the mixture will determine the number of
stages, and hence the number of trays, required for the separation.
This is illustrated clearly by applying the McCabe-Thiele method to
design a binary column.
 4. Distillation column design
28

McCABE-THIELE DESIGN METHOD

The McCabe-Thiele approach is a graphical one, and uses the VLE plot
to determine the theoretical number of stages required to effect the
separation of a binary mixture. It assumes constant molar overflow
 4. Distillation column design
29

The design procedure is simple. Given the VLE diagram of the binary
mixture, operating lines are drawn first.
 Operating lines define the mass balance relationships between the
liquid and vapor phases in the column.
 There is one operating line for the bottom (stripping) section of the
column, and on for the top (rectification or enriching) section of the
column.
 4. Distillation column design
30

Operating Line for the

Rectification Section
The operating line for the
rectification section is
constructed as follows. First
the desired top product
composition is located on the
VLE diagram, and a vertical
line produced until it intersects
the diagonal line that splits
the VLE plot in half. A line with
slope R/(R+1) is then drawn
from this instersection point as R is the ratio of reflux flow (L) to distillate flow
shown in the diagram below. (D) and is called the reflux ratio and is a
Ln D measure of how much of the material going up
y n +1 = xn + xD the top of the column is returned back to the
Vn +1 Vn +1 column as reflux.
 4. Distillation column design
31
 4. Distillation column design
32

Operating Line for the Stripping

Section
The operating line for the stripping section is
constructed in a similar manner. However, the
starting point is the desired bottom product
composition. A vertical line is drawn from this
point to the diagonal line, and a line of slope
Ls/Vs is drawn as illustrated in the diagram
below.
Ls is the liquid rate down the stripping section
of the column, while Vs is the vapour rate up
the stripping section of the column. Thus the
slope of the operating line for the stripping L B
section is a ratio between the liquid and
y m +1 = x m − xb
vapor flows in that part of the column.
V V
 4. Distillation column design
33
 4. Distillation column design
34

Equilibrium and Operating Lines

The McCabe-Thiele method assumes that the liquid on a tray and the vapor above it are
in equilibrium. How this is related to the VLE plot and the operating lines is depicted
graphically in the diagram on the right.
 4. Distillation column design
35

Number of Stages and Trays

Doing the graphical construction repeatedly will give rise to a number of 'corner'
sections, and each section will be equivalent to a stage of the distillation. This is the
basis of sizing distillation columns using the McCabe-Thiele graphical design
methodology as shown in the following example.

Given the operating lines for both stripping

and rectification sections, the graphical
construction described above was applied.
This particular example shows that 7
theoretical stages are required to achieve
the desired separation. The required
number of trays (as opposed to stages) is
one less than the number of stages since
the graphical construction includes the
contribution of the reboiler in carrying out
the separation.
 4. Distillation column design
36

The actual number of trays required is given by the formula:

(number of theoretical trays)/(tray efficiency)
Typical values for tray efficiency ranges from 0.5 to 0.7 and
depends on a number of factors, such as the type of trays being used,
and internal liquid and vapor flow conditions. Sometimes, additional
trays are added (up to 10%) to accommodate the possibility that the
column may be under-designed.
 4. Distillation column design

The Feed Line (q-line)

The diagram above also shows that the binary feed should be introduced
at the 4'th stage. However, if the feed composition is such that it does not
coincide with the intersection of the operating lines, this means that the
feed is not a saturated liquid. The condition of the feed can be deduced
by the slope of the feed line or q-line. The q-line is that drawn between
the intersection of the operating lines, and where the feed composition
lies on the diagonal line
4. Distillation column design

Depending on the state of the feed, the

feed lines will have different slopes.
For example,
q = 0 (saturated vapour)
q = 1 (saturated liquid)
0 < q < 1 (mix of liquid and vapour)
q > 1 (subcooled liquid)
q < 0 (superheated vapour)
The q-lines for the various feed
conditions are shown in the diagram
on the left.
 4. Distillation column design

Using Operating Lines and the Feed Line in McCabe-Thiele

Design
If we have information about the condition of the feed mixture, then
we can construct the q-line and use it in the McCabe-Thiele design.
However, excluding the equilibrium line, only two other pairs of lines
can be used in the McCabe-Thiele procedure. These are:
 feed-line and rectification section operating line
 feed-line and stripping section operating line
 stripping and rectification operating lines
This is because these pairs of lines determine the third.
4. Distillation column design
 4. Distillation column design

OVERALL COLUMN DESIGN

 Determining the number of stages
required for the desired degree of
separation and the location of the
feed tray is merely the first steps in
producing an overall distillation
column design. Other things that
need to be considered are tray
spacings; column diameter;
internal configurations; heating
and cooling duties. All of these can
lead to conflicting design
parameters.
 4. Distillation column design
Minimum Reflux Ratio
The minimum reflux is obtained when the feed
line, equilibrium curve and the operating line
of the enriching section meet at one point. The
minimum reflux is the minimum allowable reflux for
the separation. For saturated feed, the operating
lines for different values of reflux are shown in
Figure 2. The slope of the enriching section
operating line is R/(R+l). For the four different cases
of operating lines demonstrated in this picture, the
slope, R/(R + 1), decreases as we move from 1 to 4
(R 1 > R2 > R3 >R4 ). For a case like number 4, where the
two operating lines cross each other on the left side
of the equilibrium curve, distillation separation
cannot be achieved. Thus, the lowest value of R
(minimum reflux ratio=R3 ) is where the· two
operating lines meet with the equilibrium curve.
As a result, the minimum reflux ratio can be
calculated from the following equation:
4. Distillation column design

Reflux Conditions
As the reflux ratio is increased, the gradient of operating
line for the rectification section moves towards a maximum
value of 1. Physically, what this means is that more and
more liquid that is rich in the more volatile components are
being recycled back into the column. Separation then
becomes better and thus less trays are needed to achieve
the same degree of separation. Minimum trays are
required under total reflux conditions, i.e. there is no
withdrawal of distillate.
 4. Distillation column design

Reflux Conditions
On the other hand, as reflux is decreased, the
operating line for the rectification section
moves towards the equilibrium line. The ‘pinch’
between operating and equilibrium lines
becomes more pronounced and more and more
trays are required. This is easy to verify using
the McCabe-Thiele method.
The limiting condition occurs at minimum reflux
ratio, when an infinite number of trays will be
required to effect separation. Most columns
are designed to operate between 1.2 to 1.5
times the minimum reflux ratio because this is
approximately the region of minimum
operating costs (more reflux means higher
reboiler duty).
4. Distillation column design
Heat balance
 4. Distillation column design -computation method

1. Assume 99% LK goes overheard, 99% HK goes in bottoms.

All components lighter goes with LK. Heavier goes with HK.

2. Do a material balance on column. Determine mole fraction

of light key in Distillate, (xLK)D etc
4. Distillation column design -computation
method
49

Relative Volatility
Relative volatility is a measure of the differences in volatility between 2 components,
and hence their boiling points. It indicates how easy or difficult a particular separation
will be. The relative volatility of component ‘i’ with respect to component ‘j’ is defined
as

yi = mole fraction of component ‘i’ in the vapour

xi = mole fraction of component ‘i’ in the liquid
Thus if the relative volatility between 2 components
is very close to one, it is an indication that they have
very similar vapor pressure characteristics. This
means that they have very similar boiling points
and therefore, it will be difficult to separate the
two components via distillation.
The larger a is, the easier is the separation
4. Distillation column design -computation method
Explanation of calculation Minimum no. of
stages, Nmin

 Infinity energy Total reflux. Stage i:

 Repeat for all N stages

 Fenske’s formula for minimum no. of stages

Assumption: Constant relative volatility

 Applies also to column sections
 4. Distillation column design -computation method

3. Minimum stages

4. Minimum reflux ratio

Separation factor examples

 Example: Binary separation with purities: 90% light in top

and 90% heavy in bottom:

 Example: Binary separation with purities: 99.9% light in

top and 98% heavy in bottom:
Separation factor examples
 Efficiency of tray

tb = f ( ,  )

Relative volatility y 1− x
= .
1− y x

Viscosity of mixture 
=f(T)
1 + 2 + 3
tb =
3
1 , 2 , 3 : Efficiency of top, feed and bottom tray
 Column dimension calculation

1. Column diameter

g tb
D = 0.0188
( y w y ) tb

gtb: Average vapor flowrate (kg/h)

(y w y ) tb Vapor velocity (kg/m2.s)
 Column dimension calculation

2. Column Height

H = n tt (H d + ) + (0.8  1.0)(m)

 Tray thickness

Hd Space between trays

0.8-1 Space from top and bottom

5. Factors affecting distillation column operation

Vapor Flow Conditions

Adverse vapor flow conditions can cause

 Foaming

 Entrainment

 Weeping/dumping

 Flooding
5. Factors affecting distillation column operation

Foaming
Foaming refers to the expansion of liquid due to
passage of vapor or gas. Although it provides high
interfacial liquid-vapor contact, excessive foaming often
leads to liquid buildup on trays. In some cases, foaming
may be so bad that the foam mixes with liquid on the
tray above. Whether foaming will occur depends
primarily on physical properties of the liquid mixtures,
but is sometimes due to tray designs and condition.
Whatever the cause, separation efficiency is always
reduced.
FACTORS AFFECTING DISTILLATION COLUMN
OPERATION

Entrainment
Entrainment refers to the liquid carried by vapor up to
the tray above and is again caused by high vapor flow
rates. It is detrimental because tray efficiency is reduced:
lower volatile material is carried to a plate holding
liquid of higher volatility. It could also contaminate high
purity distillate. Excessive entrainment can lead to
flooding.
5. Factors affecting distillation column operation

Weeping/Dumping
This phenomenon is caused by low vapor flow. The pressure
exerted by the vapor is insufficient to hold up the liquid
on the tray. Therefore, liquid starts to leak through
perforations. Excessive weeping will lead to dumping.
That is the liquid on all trays will crash (dump) through to
the base of the column (via a domino effect) and the
column will have to be re-started. Weeping is indicated
by a sharp pressure drop in the column and reduced
separation efficiency.
5. Factors affecting distillation column operation

Flooding
Flooding is brought about by excessive vapor flow, causing
liquid to be entrained in the vapor up the column. The
increased pressure from excessive vapor also backs up
the liquid in the downcomer, causing an increase in liquid
holdup on the plate above. Depending on the degree of
flooding, the maximum capacity of the column may be
severely reduced. Flooding is detected by sharp
increases in column differential pressure and significant
decrease in separation efficiency.
5. Factors affecting distillation column operation

Column Diameter
Most of the above factors that affect column operation is
due to vapor flow conditions: either excessive or too low.
Vapor flow velocity is dependent on column diameter.
Weeping determines the minimum vapor flow required
while flooding determines the maximum vapor flow allowed,
hence column capacity. Thus, if the column diameter is not
sized properly, the column will not perform well. Not only
will operational problems occur, the desired separation
duties may not be achieved.
5. Factors affecting distillation column operation

State of Trays and Packings

Remember that the actual number of trays required for a
particular separation duty is determined by the efficiency
of the plate, and the packings if packings are used. Thus,
any factors that cause a decrease in tray efficiency will
also change the performance of the column. Tray
efficiencies are affected by fouling, wear and tear and
corrosion, and the rates at which these occur depends on
the properties of the liquids being processed. Thus
appropriate materials should be specified for tray
construction.
5. Factors affecting distillation column operation

Weather Conditions
Most distillation columns are open to the atmosphere. Although
many of the columns are insulated, changing weather
conditions can still affect column operation. Thus the reboiler
must be appropriately sized to ensure that enough vapor can
be generated during cold and windy spells and that it can be
turned down sufficiently during hot seasons. The same applies
to condensers.
66

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