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How does distillation work?

• Distillation is defined as:


– a process in which a liquid or vapour mixture of two or more substances is separated into
its component fractions of desired purity, by the application and removal of heat.

Lecture 15: Batch Distillation 1


Continuous distillation columns

Classified according to:


1. Nature of the feed that they are processing:
– binary column - feed contains only two components;
– multi-component column - feed contains more than two components.
2. Number of product streams they have:
– multi-product column - column has more than two product streams.
3. Where extra feed exits when used to help with the separation:
– extractive distillation - where the extra feed appears in the bottom product stream;
– azeotropic distillation - where the extra feed appears at the top product stream.
4. Type of column internals:
– tray column - trays of various designs used to hold up the liquid to provide better contact between vapour and
liquid;
– packed column - packings are used to enhance vapour-liquid contact.

Lecture 15: Batch Distillation 2


Main Components of Distillation Columns

• A vertical shell where separation of liquid


components is done.
• Column internals e.g.trays/plates and/or
packings which are used to enhance
component separations.
• A reboiler to provide the necessary
vaporization for the distillation process.
• A condenser to cool and condense the
vapour leaving the top of the column.
• A reflux drum to hold the condensed
vapour from the top of the column so that
liquid (reflux) can be recycled back to the
column.

Lecture 15: Batch Distillation 3


DISTILLATION
COLUMN

Lecture 15: Batch Distillation 4


COLUMNS, Diagrams

Fractional Distillation Column


Distillation Column Packings
Lecture 15: Batch Distillation 5
Batch Distillation
In differential distillation a feed mixture (an initial charge) of a given composition is placed in a single stage separator
(a still pot, retort or flask) and heated to boiling. The vapor is collected and condensed to a distillate. The composition of
the remaining liquid and the distillate are functions of time. There may be several reasons for running a batch process
such as this:
1) Small capacity doesn’t warrant continuous operation
2) Separation is to be done only occasionally
3) Separation is preparative to produce a new product
4) Upstream operations are batchwise or feedstocks vary with time or from batch to batch
5) Feed materials are not appropriate for a continuous flow system.
Total condenser Total condenser
Differential
Distillation Distillation
Reflux drum
Overhead vapor Overhead vapor
Distillate
1 Reflux
Rectifying section stages Distillate
2
QB
Feed Feed Stage
No reflux Liquid composition x(t)
Boilup No boilup Distillate composition y(t)
Stripping section stages
N No reboiler Distillate flow D(t)
Partial reboiler No cascade Liquid remaining W(t)
No feed stream
Bottoms No countercurrent flow

The Differential Distillation operation requires a much simpler apparatus, but is


complicated because the process is now a function of time.

Lecture 15: Batch Distillation 6


Batch Distillation
To analyze this process we must perform component balances Total condenser
in the form of rates:
Differential
Distillation
The rate of depletion of the liquid is equal to the rate of distillate output Overhead vapor Distillate
D(t), y=yD=xD
The instantaneous rate of depletion of a component in the liquid
is given by: QB
d dx dW
− (WxW ) = −W W − x W Liquid left in still
dt dt dt W(t), x=xw

Change in total Change in Change in the


amount of that composition total amount
component in the liquid of the liquid
in the liquid
The instantaneous rate of the component leaving in the distillate is:

DyD

Conservation of species requires that these two rates be equal to each other:

d dx dW
− (WxW ) = −W W − x W = DyD
dt dt dt

Lecture 15: Batch Distillation 7


Batch Distillation
Rate of depletion equals the component flow rate in Distillate Total condenser
Differential
d dx dW
− (WxW ) = −W W − x W = DyD
Distillation
dt dt dt Overhead vapor Distillate
Multiplying the above equation by dt gives: D(t), y=yD=xD

−WdxW − xW dW = y D Ddt QB

Liquid left in still


But we know that the rate of total liquid depletion is equal to the W(t), x=xw
flow rate of distillate:
dW = −Ddt

Which then gives:


WdxW + xW dW = y DdW

Rearranging to use separation of variables gives:


dxW dW
=
y D − xW W
The distillate composition and liquid composition are related through an equilibrium
equation (y=kx). We can then integrate both sides:
dx dW 1 x w
∫ x(k −1) = ∫ ln = ln
W (k −1) x 0 w0
Lecture 15: Batch Distillation 8
Distillation: The underlying physics of
the process
This process takes advantage of the differences in distribution of
components between vapour and liquid phase

pressure constant
dew point y
T T1
V T5
T4 T2
Tb(B)
T3
T3
T2
T1
T4
Tb(A)
L T5

xa ya
xA=0 xA=1 x
xB=1 xB=0 9
Lecture 15: Batch Distillation
Distillation: Basic elements of the process
Va , y a

La, xa=xd
condenser

Ln-1 xn-1
Vn yn Overhead product D, xd

Ln xn
Vn+1 yn+1

F , zf

Lm-1 xm-1
Vm ym

Bottom product B, xb
Lm xm
Vm+1 ym+1

Vb , y b boiler

Lb, xN
Lecture 15: Batch Distillation 10
Distillation: Operating lines
Va , y a
Rectifying section

La, xa=xd=y1=ya
condenser

Ln-1 xn-1
Overhead product D, xd
Vn yn
R=La/D
Ln xn
Vn+1 yn+1

F , zf

Lm-1 xm-1
Vm ym

Bottom product B, xb
Lm xm
Vm+1 ym+1

Vb , y b boiler

Lb, xN
Lecture 15: Batch Distillation 11
Distillation: Operating lines

Ln D
Vn +1 yn +1 = Ln xn + Dx D ⇒ yn +1 = xn + xD
Vn +1 Vn +1
This equation is a straight line (V=const, L=const, L/V=const) if:

- Two components have similar and constant molar


enthalpies of vaporization (latent heats)

- Component sensible enthalpies changes and heats of mixing


are negligible (compared to latent heats)

- The column is well insulated (adiabatic)

- Pressure is uniform throughout the column

Lecture 15: Batch Distillation 12


Distillation: Operating lines

Va , y a
L D
yn +1 = xn + x D La, xa condenser
V V Overhead product D, xd
R=L/D
Ln xn Vn+1 yn+1

L L L L/D R
R= ; = = = Reflux ratio
D V L + D L / D + D / D R +1

R 1
yn +1 = xn + xD
R +1 R +1

Lecture 15: Batch Distillation 13


Distillation: Operating lines

R 1
yn +1 = xn + xD
R +1 R +1
y

slope=R/(R+1)

1
xD
R +1

xD
x
Lecture 15: Batch Distillation 14
Distillation: Operating lines
Va , y a

La, xa
condenser

Ln-1 xn-1
Overhead product D, xd
Vn yn
R=La/D
Ln xn
Vn+1 yn+1

F , zf

Lm-1 xm-1
Stripping section

Vm ym

Bottom product B, xb
Lm xm
Vm+1 ym+1

Vb , y b boiler

Lb, xN
Lecture 15: Batch Distillation 15
Distillation: Operating lines

L xm =V ym +1 + Bx B Lm xm
Vm+1 ym+1
Bottom product B, xb
boiler

L B
ym +1 = xm − xB y

V V
L
slope= V

yB

xN
Lecture 15: Batch Distillation
xB x 16
Distillation: Feed stage considerations
L V L V L V

F F F

bubble point dew point


liquid feed vapour feed

L V L V L V

F F F

subcooled superheated partially vaporized


liquid feed vapour feed feed

Lecture 15: Batch Distillation 17


Distillation: Feed stage considerations
L V
L −L V −V
q= = 1+ F
F F

Lecture 15: Batch Distillation 18


L −L
Distillation: Feed stage considerations q=
L V
F
L V L V

F F F

dew point
bubble point
q=1 vapour feed q=0
liquid feed

L V L V L V

F F F

subcooled superheated partially vaporized


liquid feed
q>1 vapour feed
q<0 feed 0<q<1

Lecture 15: Batch Distillation 19


Distillation: Feed stage considerations
F
L V
L = L + qF ⇒ L − L = F
V = V + (1 − q ) F ⇒ V − V = (1 − q ) F
L V

Vy = Lx + Dx D rectifying section

V y = L x − BxB stripping section

D
y (V − V ) = ( L − L ) x + DxD + BxB F

B
FzF
q zF
y= x+
q −1 1− q
Feed line
Lecture 15: Batch Distillation 20
q>1
Distillation: Feed line behavior
q=1

x
y=
q zF
y= x+ 0<q<1
q −1 1− q
q=0
x=zf
x=zf

q zF
y= zF + = zF q<0
q −1 1− q
y=zf

Lecture 15: Batch Distillation 21


Distillation: Complete picture

R 1
yn +1 = xn + xD
R +1 R +1
y
q zF y1
y= x+
q −1 1− q

L B
yn +1 = xm − xB
V V zf

1 yB
xD
R +1
xB xN zf xD
x

Lecture 15: Batch Distillation 22


Distillation: Complete picture

R 1
yn +1 = xn + xD
R +1 R +1
y
L B
yn +1 = xm − xB y1
V V
q zF
y= x+
q −1 1− q zf

yB

xB xN zf xD
x

Lecture 15: Batch Distillation 23


Limiting cases: total reflux

Total reflux=Minimum number of stages

D=0
y
F=0 R=L/D=∞
y1
L/V=1
Ln + D = Vn +1
Ln = Vn +1
B=0
zf
Total reflux
R 1
yn +1 = xn + xD
R +1 R +1 yB
If R=L/D= ∞ then R/(R+1)=1; also L=V

xB xN zf xD
y n +1 = xn
x

Lecture 15: Batch Distillation 24


Limiting cases: total reflux

Total reflux=Minimum number of stages

D=0
y
F=0 R=L/D=∞
y1
L/V=1
Ln + D = Vn +1
Ln = Vn +1
B=0
zf
Total reflux
R 1
yn +1 = xn + xD
R +1 R +1 yB
If R=L/D= ∞ then R/(R+1)=1; also L=V

xB xN zf xD
y n +1 = xn
x

Lecture 15: Batch Distillation 25


Distillation: Minimum number of stages

a) Graphical methods y

D, xD

F, z R=L/D

B, xB
xB xD
x

b) Short cut methods: Fenske Equation

Lecture 15: Batch Distillation 26


Distillation: Fenske Equation
Under total reflux condition: operating line equations become:

y n +1 = xn
y m +1 = xm
Consider relative volatility coefficient for a binary mixture of A and B:

yA / xA y y
α AB = ⇒ α AB B = A
y B / xB xB x A
For a binary mixture, yA+yB=1, and xA+xB=1, so skipping the A, B subscripts and rewriting everything
for the light component A:

1− y y
α AB =
1− x x

Lecture 15: Batch Distillation 27


Distillation: Fenske Equation

1− y y
α AB =
1− x x
For a particular stage n+1:

1 − yn +1 yn +1 yn +1 xn +1
α n +1, AB = ⇒ = α n +1, AB
1 − xn +1 xn +1 1 − yn +1 1 − xn +1
At the same time: y n +1 = xn

xn xn +1
So = α n +1, AB
1 − xn 1 − xn +1

Lecture 15: Batch Distillation 28


Distillation: Fenske Equation

xn xn +1
= α n +1, AB
1 − xn 1 − xn +1

xD x1
= α1, AB
1 − xD 1 − x1

x1 x2
= α 2, AB
1 − x1 1 − x2

xD xn +1
= α1, ABα 2, AB  α n +1, AB
1 − xD 1 − xn +1

Lecture 15: Batch Distillation 29


Distillation: Fenske Equation

xD xB
= α1, ABα 2, AB  α N +1, AB
1 − xD 1 − xB

xD N min +1 xB
= (α )
1 − xD 1 − xB

ln[ xD (1 − xB ) / xB (1 − xD )
N min = −1
ln α AB
Fenske equation

Lecture 15: Batch Distillation 30


Distillation: Limiting cases

If we decrease reflux ratio, then

y
q zF
y= x+ y1
q −1 1− q

R 1
yn +1 = xn + xD
R +1 R +1 zf
L B
yn +1 = xm − xB
V V yB

xB xN zf xD
x

Lecture 15: Batch Distillation 31


Limiting cases: minimum reflux

If we decrease reflux ratio, then we


are arriving at a condition where both
the rectifying, stripping and feed line y
intersect at the equilibrium line.
y1

In order for this process to take place we


need an infinite number of plates

zf

The minimum reflux


ratio condition
yB

xB xN zf xD
x

Lecture 15: Batch Distillation 32


Limiting cases: minimum reflux

R 1
yn +1 = xn + xD
R +1 R +1 y
y1

At this point: xn=x and yn+1 =y*


y*
Rmin 1
y* = x+ xD zf
Rmin +1 Rmin +1
xD − y *
Rmin = yB
y * −x
xB xN zf xD
x x
Lecture 15: Batch Distillation 33
Optimum Reflux

Lecture 15: Batch Distillation 34


Lecture 15: Batch Distillation 35