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DISTILLATION COLUMN DESIGN

 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.
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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 and this
implies that:
 Molal heats of vaporization of the components are
roughly the same
 Heat effects (heats of solution, heat losses to and
from column, etc.) are negligible
 for every mole of vapour condensed, 1 mole of
liquid is vaporised.
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 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
 Use of the constant molar overflow assumption
also ensures the operating lines are straight lines.
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 The Information required are:
 VLE data
 Feed conditions(temp,composition)
 Distillate and bottom compositions(xd,xb)
 Reflux ratio(R)
The steps to be followed are:
1.Determination of ROL
2.Determination of feed condition(q)
3.Determination of q-line
4.Determination of R
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5.Determination of SOL
6. Determination of the number of
theoretical stages
Let us consider a distillation column shown in
the figure below

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1.Determination of ROL

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2.Determination of the feed condition
 The feed enters the distillation column may
consists of liquid, vapor or a mixture of both.
 Some portions of the feed go as the liquid and
vapor stream to the rectifying and stripping
sections.
 The moles of liquid flow in the stripping
section that result from the introduction of
each mole of feed, denoted as ‘q’.
 The limitations of the q-value as per feed
conditions are shown in the Table below
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Table:Limitations of q-value as per feed conditions

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Calculation of q-value
I. When feed is partially vaporized:
 Other than saturated liquid (q = 1) and saturated
vapor (q = 0), the feed condition is uncertain.
 In that case one must calculate the value of q. The q-
value can be obtained from enthalpy balance around
the feed plate.
 By enthalpy balance one can obtain the q-value from
the following form of Equation:

 where HF, HV and HL are enthalpies of feed, vapor


and liquid respectively which can be obtained from
enthalpy-concentration diagram for the mixture.

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II.When feed is cold liquid or superheated vapor:
 q can be alternatively defined as the heat required
to convert 1 mole of feed from its entering
condition to a saturated vapor; divided by the
molal latent heat of vaporization.

 Based on this definition, one can calculate the q-


value from the following Equations for the case
whereby q > 1 (cold liquid feed) and q < 0
(superheated vapor feed) as:
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where Tbp is the bubble point, is the latent heat
of vaporization and Tdp is the dew point of the
feed respectively.

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3.Determination of the feed section
operating line (q-line):
 Consider the section of the distillation column at
the tray (called feed tray) where the feed is
introduced.
 In the feed tray the feed is introduced at F
moles/hr with liquid of q fraction of feed and
vapor of (1-q) fraction of feed Overall material
balance around the feed tray:

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 Component balances for the more volatile
component in the rectifying and stripping sections
are:

 At the feed point where the two operating lines


intersect can be written as:

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 From overall material balance:

 Therefore We obrain the feed line Equation :

 For a given feed condition, ZF and q are fixed,


therefore the q-line is a straight line with slope
-q / (1-q) and intercept ZF/(1-q). If x = ZF , then
from the above Equation y = ZF.

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 At this condition the q-line passes
through the point (ZF, ZF) on the 45
degree diagonal.
 Different values of q will result in
different slope of the q-line. Different
q-lines for different feed conditions are
shown in Figure below

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The Information required are:
VLE data
Feed conditions(temp,composition

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4. Determination of the stripping section operating
line (SOL):
Material balance between the m-th stage in the stripping
section and and the bottom of the column gives:

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5.Determination of number of theoretical stage
 Suppose a column is to be designed for the separation
of a binary mixture where the feed has a concentration
of zF (mole fraction) of the more volatile component
and a distillate having a concentration of xD of the more
volatile component whereas the bottoms having a
desired concentration of xB.
 Once the three lines (ROL, SOL and q-line) are drawn,
the number of theoretical stages required for a given
separation is then the number of triangles that can be
drawn between these operating lines and the
equilibrium curve.
 The last triangle on the diagram represents the reboiler.
A typical representation is given in Figure below

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Steps of drawing triangles
1. always start at the x = y line at the xd point.
2.At that point draw a horizontal line till it touches the
equilibrium graph. Then a vertical line straight down till
it touches the top operating line.
3.Carry on like this till you pass the Zf mark. Then you
have to draw the line straight down till it touches the
bottom operating line.
4.stop only after the vertical line passes the xb point
and you count the plates from top to bottom.
5.This is the theoretical number of plates which include
one as the reboiler.

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 Therefore from the above diagram:
 No of theoretical stages=8
 Required no of trays=no of stages -1=7
 This is because the graphical construction
includes the contribution of the reboiler in
carrying out the separation.
 The actual no of trays required is given by:
 Actual no of trays
no of theoretical 𝑡𝑟𝑎𝑦𝑠 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑
=
𝑂𝑣𝑒𝑟𝑎𝑙𝑙 𝑡𝑟𝑎𝑦 𝑒𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦

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Location of feed point
 In the step by step construction we can
either at the top (rectifying line)or
bottom(strriping line),but most of the time
we start from the top.
 The transfer (change) from ROL to SOL must
be made at the real feed plates.
 The feed stage is thus located nearest to
the intersection of the operating lines and
q-line as possible.

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 From the Figure it may be seen that, when
stepping off plates down the top operating line
AB, the bottom operating line CE cannot be
used until the value of xn on any plate is less
than xe.
 Again it is essential to pass to the lower line CE
by the time xn = xb.
 The best conditions are those where the
minimum number of plates is used.
 From the geometry of the figure, the largest
steps in the enriching section occur down to
the point of intersection of the operating lines
at x = xq.
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 Below this value of x, the steps are larger on the
lower operating line.
 Thus, although the column will operate for a feed
composition between xe and xb, the minimum
number of plates will be required if xf = xq .
 For a binary mixture at its boiling point, this is
equivalent to making xf equal to the composition
of the liquid on the feed plate

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The importance of the reflux ratio
1.Influence on the number theoretical stages
 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
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 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.

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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).
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2.Calculation of minimum reflux ratio
 The minimum reflux ratio can be calculated either
from a graph or using Underwood equation.
I.Graphical method
 The figure given below represents conditions where the q-
line is vertical, and the point E lies on the equilibrium
curve and has co-ordinates (xf , yf ).
 The slope of the line AE is then given by:

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 If the q-line is horizontal as shown in Figure below,
the enrichment line for minimum reflux is given by
AC, where C has coordinates (xc, yc). Thus:

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II. Using underwood equation
 For ideal mixtures, or where over the
concentration range concerned the relative
volatility may be taken as constant, Rm may
be obtained analytically from the physical
properties of the system as discussed by
UNDERWOOD.
 Thus, if xnA and xnB are the mole fractions
of two components A and B in the liquid on
any plate n, then a material balance over the
top portion of the column above plate n gives:
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 Under conditions of minimum reflux, a column
has to have an infinite number of plates,or
alternatively the composition on plate n is equal
to that on plate n + 1.
 Dividing the first equation by the second
equation and using the relations x(n+1)A = xnA
and x(n+1)B = xnB,

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 In this analysis, α is taken as the volatility of A
relative to B. There is, in general,therefore a
different value of Rm for each plate.
 In order to produce any separation of the feed,
the minimum relevant value of Rm is that for
the feed plate, so that the minimum reflux
ratio for the desired separation is given by:
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This relation may be obtained by putting:
y = αx/[1 + (α − 1)x] in the first equation for
Rm discussed in the graphical method where
q-line is vertical to give:

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Total reflux: Fenske’s Method
 This is a short cut method to obtain the minimum
number of stages.
 For conditions in which the relative volatility is
constant, FENSKE derived an equation for
calculating the required number of plates for a
desired separation.
 Since no product is withdrawn from the still, the
equations of the two operating lines become:

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𝑥𝑑 1−𝑥𝑏
log{ }
𝑥𝑏 1−𝑥𝑑
Nm+1=
log ᾀ𝑎𝑣

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Example1:
A liquid mixture of benzene toluene is being
distilled in a fractionating column at 101.3 k Pa
pressure. The feed of 100 kmole/h is liquid and it
contains 45 mole% benzene (A) and 55 mole%
toluene (B) and enters at 327.6 K. A distillate
containing 95 mole% benzene and 5 mole%
toluene and a bottoms containing 10 mole%
benzene and 90 mole% toluene are to be
obtained. The amount of liquid is fed back to the
column at the top is 4 times the distillate product.
The average heat capacity of the feed is 159 KJ/kg
mole. K and the average latent heat 32099 kJ/kg
moles. Calculate
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Solution
 F=D+B
 100 = D + B
 F xF = D xD + B xB
 Therefore, D = 41.2 kg mole/h, B = 58.8 kg mol/h
 y = [R/(R+1)] x + xD/(R+1) = 0.8 x +0.190
 q = 1+ cpL (TB-TF)/Latent heat of vaporization
 TB = 366.7 K from boiling point of feed, TF = 327.6
K ( inlet feed temp)
 Therefore q = 1.195 and Slope of q line = 6.12

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 From the graph (Figure below):
• Total no of theoretical stages is 8 at operating reflux
(Red color)
• Total no of theoretical stages is 6 at total reflux (Black
color)
 Overall efficiency at operating conditions:
• Eo (Operating) = No of ideal stage/ No of actual trays
= 7.9/10 = 0.79
 Overall efficiency at total reflux conditions:
• Eo (total relux) = No of ideal stage/ No of actual trays
= 5.9/10=0.59
 Overall efficiency increased: 0.79-0.59 = 0.20
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Example2:
A mixture of benzene and toluene containing 40 mole
per cent benzene is to be separated to give a product
containing 90 mole per cent benzene at the top, and a
bottom product containing not more than 10 mole per
cent benzene. The feed enters the column at its boiling
point, and the vapour leaving the column which is
condensed but not cooled, provides reflux and product.
It is proposed to operate the unit with a reflux ratio of 3
kmol/kmol product. It is required to find the number
of theoretical plates needed and the position of entry
for the feed. The equilibrium diagram at 100 kN/m2 is
shown in Figure below.

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Solution

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• With the two equations (i) and (ii) and the equilibrium
curve, the composition on the various
• plates may be calculated by working either from the
still up to the condenser, or in the reverse
• direction. Since all the vapour from the column is
condensed, the composition of the vapour yt
• from the top plate must equal that of the product xd ,
and that of the liquid returned as reflux xr .
• The composition xt of the liquid on the top plate is
found from the equilibrium curve and, since it
• is in equilibrium with vapour of composition, yt = 0.90,
xt = 0.79.
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Factors that affect distillation column performance

The performance of a distillation column is


determined by many factors, for example:
 Number of trays or stages
 Feed conditions
 state of feed
 composition of feed
 trace elements that can severely affect the VLEof
liquid mixtures
 Internal liquid and fluid flow conditions
 State of trays (packings)
 Weather conditions

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Factors that affect distillation column performance
1.EFFECTS OF THE NUMBER OF TRAYS OR STAGES
 Here we will expand on the design of
columns by looking briefly at the effects
of:
 the number of trays, and
 the position of the feed tray, and on the
performances of distillation columns.
A. Effects of the Number of Trays
It can be deduced from the previous section on distillation
column design that the number of trays will influence the
degree of separation. This is illustrated by the following
example.

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B.Effect of Feed Tray Position

 Here we look at how the position of the


feed tray affects separation efficiency.

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 As the feed stage is moved lower down the
column, the top composition becomes less rich
in the more volatile component while the
bottoms contains more of the more volatile
component.
 However, the changes in top composition is
not as marked as the bottoms composition.
 The preceding examples illustrate what can
happen if the position of the feed tray is
shifted for this particular system.
 They should not be used to generalize to other
distillation systems, as the effects are not
straightforward
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2.Feed Conditions

• The state of the feed mixture and feed composition affects


the operating lines and hence the number of stages
required for separation.
• It also affects the location of feed tray. During operation, if
the deviations from design specifications are excessive,
then the column may no longer be able handle the
separation task.
• To overcome the problems associated with the feed, some
column are designed to have multiple feed points when the
feed is expected to containing varying amounts of
components.

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3.Vapor flow conditions

 Adverse vapor flow conditions can cause: Foaming


Entrainment
Weeping/dumping
Flooding
Foaming
 Foaming refers to the expansion of liquid due to passage of
vapor or gas.
 Although it provides high interfacial liquid-vapour 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.
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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.
Weeping/Dumping

 This phenomenon is caused by low vapor flow.


 The pressure exerted by the vapour 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.

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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 down comer, causing an
increase in liquid holdup on the plate a bove.
 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.

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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.

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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.
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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.
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Other Factors

 These are some of the more important factors that


can cause poor distillation column performance.
 Other factors include changing operating conditions
and throughputs, brought about by changes in
upstream conditions and changes in the demand for
the products.
 All these factors, including the associated control
system, should be considered at the design stages
because once a column is built and installed,
nothing much can be done to rectify the situation
without incurring significant costs.
 The control of distillation columns is a field in its
own right, but that's another story.
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