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Distillation

Topics

Types of Distillation
Action on an Ideal Plate
Mass Balance in a Distillation Column
Determination of Ideal Number of
Plates McCabe Thiele Analysis

The methods of distillation

Differential or batch distillation


Flash or equilibrium distillation
Continuous Rectification Binary
systems

Differential distillation

The simplest examples of batch distillation at a


single stage.
Starting with a still pot, initially full, heated at a
constant rate. In this process the vapour formed
on boiling the liquid is removed at once from the
system.
Since this vapour is richer in the more volatile
component, with this result the composition of
the product progressively alters.
Thus, whilst the vapour formed over a short
period is in equilibrium with the liquid
At the end of the process the liquid, which has
been vaporized, is removed as the bottom
product.

Differential Distillation

Let S be the number of mols of material in


the still and x be the mol fraction of
component A.
Suppose an amount dS, containing a mol
fraction y of A, be vaporised.
Then a material balance on component A
gives:
ydS = d (Sx)
= S dx + x dS

Differential Distillation

The integral on then right-hand side


can be solved graphically if the
equilibrium relationship between y and
x is available.
Thus, if over the range concerned the
equilibrium relationship is a straight
line of the form y= m x + c

Differential distillation

This process consists of only a single


stage, a complete separation is
impossible unless the relatively
volatility is finite. Application is
restricted to conditions where a
preliminary separation is to be
followed by a more rigorous
distillation, where high purifies is not
required, or where the mixture is very
easily separated

Flash vaporisation
or Equilibrium Distillation

This method is frequently carried out as a


continuos process.
Consist of vaporizing a definite fraction of liquid
feed in such a way that the vapour evolved is in
equilibrium with the residual liquid.
The feed is usually pumped through a fired heater
and enters the still through a valve where the
pressure is reduced.
The still is essentially a separator in which the
liquid and vapour produced is reduced by
reduction in pressure with sufficient time to reach
equilibrium. The vapour is removed from the top
of the separator and is then usually condensed,
while the liquid leaves from the bottom.

Flash or Equilibrium
Distillation

It is used in petroleum refining, in


which petroleum fractions are heated
in pipe stills and the heated fluid
flashed in to vapour and residual
streams, each containing many
components.

Continuous Distillation
with Reflux

Flash distillation is used most for


separating components that boil at
widely different temperatures.
It is not effective separating
components of comparable volatility,
which requires the use of distillation
with reflux

Action on an Ideal Plate

By definition a vapour leaving a plate are


brought into equilibrium.
\Assume that the plates are numbered
serially from top down and that the plate
under consideration is the nth plate from
the bottom.
Then the immediately above plate n is plate
n-1, and the immediately below is n+1.

Material Balance diagram for plate n


Vn-1,yn-1
Ln-2,Xn-2

Plate n-1

Vn,yn
Ln-1,Xn-1

Plate n

Vn+1,yn+1
Ln,xn
Plate n+1

For example if two fluid enter plate n and two leave it,
the liquid, Ln-1 mol/h, from plate n-1 and the stream of
vapour, Vn+1 mol/h, from plate n+1 are brought into
intimate contact.
A stream of vapour, Vn mol/h, rises to plate n-1 and a
stream of liquid, Ln mol/h, descends to plate n+1.
Since the vapour streams are the V phase, their
considerations are denoted by y; the liquid streams are
the L phase and their concentrations are denoted by x.
Then the concentrations of the streams entering and
leaving the nth plate are as follows:
Vapour leaving plate, yn
Liquid leaving plate, xn
Vapour entering plate, yn+1
Liquid entering plate, xn-1

Boiling-Point Diagram showing


rectification on ideal plate

xn xn-1

yn+1 yn

Number of Plates Required in


a Distillation Column

To develop a method for the design of distillation units


to give the desired fractionation, it is necessary to
determine the numbers of trays.
Before that the heat and material flows over the trays,
the condenser and the reboiler must be established
Thermodynamic data is required to establish how much
mass transfer is needed to establish equilibrium
between the stream leaving each tray.
The diameter of the column will be dictated by the
necessity to accommodate the desired flow rates, to
operate within the available drop in pressure, while at
the same time affecting the desired degree of mixing of
the stream on each tray.

Summary of the material


balances for two
components systems

Let the process be analysed simply for


a binary mixture of A and B as follows:
Let F be the number of mols per unit
of feed of mol fraction xf of A.
D be the number of mols per unit time
of vapour formed with y the mol
fraction of A and

B be the number of mols per unit time of liquid


with x the mol fraction of A. Then an overall
mass balance gives:
F=D+B
Component A balance
FxF = D xD + B xB
Eliminating B and D from these equations give
the follow:

D xF xB

F xD xB
B xD xF

F xD xB

Net flow rates. Quantity D is the difference


between the flow rates of the streams entering
and leaving the top of the column. A material
balance around the condenser and accumulator
in the gives:

D Va La

The difference between the flow rates of vapour


and liquid anywhere in the upper section of the
column is also equal to D. This surface includes
the condenser and all plates above n+1. A total
material balance around this control surface
gives:
D Vn 1 Ln

Similar material balances for A give the following


equations:

DxD VaYa La xa Vn1 yn1 Ln xn

Quantity D xD is the net flows rate of the


component A upward in the upper section of the
column. It too is constant throughout this part of
the equipment. In the lower section of the
column the net flow rates are also constant but,
are in a downward direction.

The net flow of total material equals B; that


of the component A is BxB. The following
equations apply:

B Lb Lb Lm Vm1
Bx B Lb xb Vb yb Lm xm Vm1 ym1

Operating lines

There are two sections in the column; there


are also two operating lines, one for the
rectifying section and other for the stripping
section.

Ln
Va ya La xa
yn 1
xn
Vn 1
Vn 1

For the first section (rectifying section) the


operation line is represented by:
y n 1

Ln
Dx D

xn
Ln D
Ln D

Substituting for DxD in the equation above and


eliminating Vn+1

Vm 1 ym 1 Lm xm Bx B
For the section below the feed plate, a material balance
over control surface II gives

Ln
Dx D
yn 1
xn
Ln D
Ln D

Rearranging this equation and taking into account that


the slope is the ratio of liquid flow to the vapour flow,
and also eliminating Vm+1
ym 1

Lm
Bx B
xm
Lm B
Lm B

Feed Line

The conditions of the vapour rate or


the liquid rate may change depending
of the thermal condition of the feed.
It is related to the heat to vaporise
one mole of feed divided by molar
latent heat (q)

Various type of feed


conditions

Cold feed, q>1


Feed at bubble point (saturated
liquid), q=1
Feed partially vapour, 0<q<1
Feed at dew point (saturated vapour),
q=0
Feed superheated vapour q<0

Feed Line

Feed Line

Cold feed : It is assumed that the entire


feed stream adds to the liquid flowing down
the column.
Feed at bubble point: no condensation is
required to heat the feed.
Feed partial vapour: the liquid portion of the
feed becomes part of the L and the vapour
portion becomes part of V

Feed Line

Feed saturated vapour the entire feed


becomes part of the V
Feed superheated: part of the liquid
from the rectifying column is vaporized
to cool the feed to a state of saturated
vapour.

Feed Line Equation

If xq = xF, and yq =xF then;


The point of intersection of the two
operating lines lies on the straight line of
slope (q/q -1) and intercept (xF, yF)

q
xF
yq
xq
q 1
q 1

Reflux Ratio

The analysis of fractionating columns is


facilitated by the use of a quantity called reflux
ratio.
Two ratios are used, one is the ratio of the reflux
to the overhead product and the other is the
ratio of the reflux to the vapour.
Both ratios refer to quantities in the rectifying
section. The equations for those ratios are
L V D
RD
D
D

and

L
L
RV
V LD

Reflux Ratio

If the operation lines equations are divided D,


the result is, for constant molar overflow,

RD
xD
yn 1
xn
RD 1
RD 1

This equation is an operation line of the


rectifying section

Reflux Ratio

The y intercept of this line is xD/(RD+1).


The concentration xD is set by the
conditions of the design.
RD, the reflux ratio, is an operating
variable that can be controlled at will
by adjusting the split between reflux
and overhead product or by changing
the amount of vapour formed in the
reboiler for a given flow rate of the
overhead product.

Reflux Ratio
A

point at the upper end of the


operating line can be obtained
by setting xn equal to xD in the
equation above.

Reflux Ratio

A point at the upper end of the operating line


can be obtained by setting xn equal to xD in the
previous equation.
RD
xD
xD RD 1
yn 1
xD

RD 1
RD 1
RD 1

or

yn 1 xD

The operating line for the rectifying section then


intersects the diagonal at point (xD, xD)

Reflux Ratio

The operation lines represented by those


two equations are plotted with the
equilibrium curve on the x-y diagram.
Those equations also show that unless Ln
and Lm are constant, the operating lines are
curved.
The lines can be plotted only if the change
in these internal streams with concentration
is known.

Reflux Ratio

Minimum
Reflux
a

e
b
Total
(Maximum)
Reflux

xF

Influence of the Number of


Reflux Ratio

Any change in
R will
therefore
modify the
slope of the
operation line
as can be
seen from the
Figure

g
a
d

e
f

Maximum or Total Reflux

If no product is withdrawn from the


still (D=0), the column is said to
operate under conditions of total
reflux and, as seen from equation ,
the top operating line has its
maximum slope of unity, and coincides
with the line x=y.

The step become very close to the


plate above, these conditions are
known as minimum reflux and Rm
denotes the reflux ratio.
Any small increase in R beyond Rm
will give a workable system, though a
large numbers of plate will be
required.

Important deductions

The minimum number of plates is


required for a given separation at
conditions of total reflux
There is a minimum reflux ratio below
which it is impossible to obtain the
desired enrichment, however many
plates are used.

Calculation of Minimum
Reflux Ratio Rm

Based on the previous figure, the slope of


the line ad is given by

Rm
xD xF
xD y F

or Rm
Rm 1 xD xF
y F xF

McCabe - Thiele

Construction the operation lines:


Locate the feed line
Calculate the y-axis intercept xD/(RD + 1)
of the rectifying line and plot that line
through the intercept and the point
(xD, xD)
Draw the stripping line through point
(xB,xB) and the intersection of the
rectifying line with the feed line.

Effect the feed condition on


feed line

If the feed is a cold liquid, the feed line slopes


will be upward and to the right;
if the feed is a saturated liquid, the line is
vertical;
if the feed is a mixture of liquid and vapour,
the lines slopes upward and to the left and
the slope is the negative of the ratio of the
liquid to the vapour;
if the feed is saturated vapour the line is
horizontal and
if the feed is superheated vapour. The lines
slope downward and to the left.

McCabe - Thiele

Feed Plate location


After the location of the feed plate
the construction of the number of
ideal trays is found by the usual
step-by-step construction.
The process can begin at the top and
also a total condenser is used.

McCabe - Thiele

END

Summary

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