reflux ratio

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Lecture 4 Reflux Ratio and Column Design

reflux ratio

© All Rights Reserved

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1

Material covered

Continuous Multistage Distillation

1. Column design; reflux ratio determines the top and

bottom product compositions

2. Assumptions of the McCabe-Thiele method:

- Constant molal overflow (constant molar latent heat)

- No heat losses

- No heat of mixing

3. Determine graphically the number of stages needed

for a given separation knowing the reflux ratio and the

feed condition

1 1

1

+

+

+

=

+

R

x

x

R

R

y

D

n n

Top Operating Line (TOL)

b

W

b

b

m m

V

W

x

V

L

x y =

1

Bottom Operating Line (BOL)

F

x

q

x

q

q

y

1

1

1

=

q-line

Material covered

L

t

, V

t

L

b

, V

b

Feed

McCabe-Thiele Method

15-Oct-13

2

2. Draw q-line

3. Draw TOL from chosen

value of R

4. Now draw BOL

6. Count the number of

stages

there are 6 stages

required for this

particular reflux ratio

x

D

x

W

Material covered

McCabe Thiele Method

1. Identify (x

F

, x

F

), (x

D

, x

D

)

& (x

W

, x

W

)

5. Draw steps between

operating lines and

equilibrium curve

(x

W

, x

W

)

(x

F

, x

F

)

(x

D

, x

D

)

1

2

3

4

5

6

Distillation Column Design

McCabe-Thiele: a graphical method to estimate the # of stages

Assumptions of McCabe-Thiele method. Constant molal overflow

Equilibrium (x-y) data y vs. x on the same plate

Top Operating Line (TOL) y vs. x on different plates at top section

Bottom Operating Line y vs. x on different plates at bottom section

q-line y vs. x on feed plate

Fundamental assumptions and limitations: make sure to understand

them when designing a distillation process

R determines gradient of TOL

What are the theoretical limits of the reflux ratio?

Influence of the reflux ratio on the separation

15-Oct-13

3

Limiting Operating Conditions: Total Reflux

occurs when all top product return as

reflux, D=0 (no top product removed)

used for starting up columns; for keeping

column operating when other part of the

plant is shut down; for testing column

efficiency

L

0

Column

Reboiler

Condenser

Reflux

Heat out

Heat in

At total reflux (infinite R) TOL has a gradient of 1

TOL becomes y = x (45 diagonal line)

If R = , what happens to the TOL?

1 1

1

+

+

+

=

+

R

x

x

R

R

y

D

n n

What is R value in this case?

D

L

R

0

=

=

The TOL is the same as

the y = x line.

x

W

x

D

4 stages needed vs. 6

stages previously

At total reflux:

minimum number of

stages required for given

separation

but no product is formed!

Limiting Operating Conditions: Total Reflux

15-Oct-13

4

x

W

x

D

Decreasing R, increases

the gradient of TOL

R=0

eventually TOL, q-line

and equilibrium curve meet

at a point Pinch Point

How many stages are

required at R

min

?

Limiting Operating Conditions: Minimum Reflux

steps get smaller & smaller

as pinch point is approached

Decreasing R

q

l

i

n

e

Pinch Point

Find R

min

from either the

gradient or intercept of

TOL:

1 R

x

Intercept

min

D

+

=

infinite number of stages

Intercept

Pinch Point

How to find R

min

in this case?

x

D

TOL at R

min

does not intersect

with the q-line and equilibrium

curve

In this case, R

min

is dictated

by the presence of a pinch-

point

Limiting Operating Conditions: Minimum Reflux

q

l

i

n

e

For highly non-ideal binary

mixture, the pinch point may

occur at a stage above or

below the feed stage.

Gradient of TOL cannot be

reduced further as it would

cross over the equilibrium

curve. This violate 2

nd

law of

thermo because of a reversal

in the mass transfer direction.

15-Oct-13

5

V increases as R increases for a

given top product flowrate, D

How to achieve a higher value of V?

Vaporise more liquid in the reboiler at the

bottom of the column more energy required

How to change the reflux ratio?

Effect of Reflux Ratio

D L V

0

+ =

D

L

R

0

=

( )D R V 1 + =

D

V

Distillate

Bottom W

L

0

Feed

Reboiler

Condenser

Reflux

Heat out

Heat in

At TOTAL REFLUX (R=,V=L) minimum number of theoretical

stages required, but no top product.

Effect of Reflux Ratio

short column with large diameter; thus, lowest capital cost

infinite sizes of condenser, reboiler and column diameter;

thus, infinite operating cost

At MINIMUM REFLUX (R=R

min

) maximum product off-take, but an

infinite number of stages needed.

tall column with small diameter; thus, infinite capital cost

minimum vapour flow in column; hence minimum reboiler

and condenser sizes. Thus, lowest operating cost

15-Oct-13

6

Trade off Between Tray Number and Reflux

Two limiting conditions:

minimum reflux ratio, R

min

minimum number of trays, N

min

many columns can be used to

make exactly the same separation

Asymptotes show the limiting

conditions:

- as R R

min

, # of trays

- as R , # of trays minimum

column at point B is short

and fat, cheaper to construct

but uses lots of energy

Any point along the curve?

column at point A is tall

and thin, uses little energy but

expensive to construct

R

min

N

u

m

b

e

r

o

f

t

r

a

y

s

B (short

column)

N

min

A (tall column)

Reflux ratio

Optimum Reflux Ratio

R

min

C

o

s

t

s

Total cost

Operating cost

Capital cost

R

optimum

Is there an optimum reflux ratio?

Reflux ratio

Optimum reflux ratio is the R which minimizes total cost;

f(energy and material of construction costs)

Typically R = 1.05 1.3 times R

min

with 1.2 R

min

being a good rule of thumb

15-Oct-13

7

the stage at which a

change in gradient between

TOL and BOL occurs

In this case, the feed is

introduced on the 5

th

stage

from the top

Where to introduce the Feed?

Feed

Reflux drum

Condenser

Distillate D

Bottoms W

Reflux L

0

Boilup V

b

Flow, x

D

F, x

i

,T, P,

phases?

Flow, x

W

L

b

V

t

R (L

0

/D)

Feed conditions

x% of F = vapour

x

boilup ratio

(V

b

/W)

Reboiler

Related to

operating T and P

Design Considerations

15-Oct-13

8

What determines the pressure at which the column operates?

Feed

Reflux drum

Condenser

Distillate D

Bottoms W

Reflux

L

0

Boilup V

b

Flow, x

D

F, x

i

,T,

P,

phases

?

Flow, x

W

L

b

V

t

Reboiler

- Feed conditions

T P - VLE equilibrium

P related to T

distillate

What if P = P*

MVC

?

- Condenser & coolant

T related to P

What if T < T

bubble

?

What if T > T

decomposition

?

- Reboiler

Design Considerations: Operating Pressure

The ethanol-water system

exhibits an azeotrope

This occurs at the point

where y

i

= x

i

Conventional distillation is

therefore limited by the

presence of an azeotrope

Azeotropes

15-Oct-13

9

Changing the operating pressure can change the VLE, and can

potentially remove the azeotrope:

This forms the basis of pressure-swing distillation, although there

are a number of other techniques for overcoming the azeotrope

Azeotropes

P

1

Azeotrope

x 1 0

1

y

P

2

x 1 0

1

y

Which of the 2 condenser arrangements will give a top product as vapour?

Vapour leaving partial condenser

has composition different from

vapour entering (y

D

x

0

)

Partial condenser acts as a

stage

Total

condenser

Partial

condenser

Design Considerations: Condenser

Liquid leaving total

condenser has same

MVC composition as

vapour entering (x

D

= y

1

)

x

D

y

1

y

1

y

D

15-Oct-13

10

Design Considerations: Condenser

Most common is a horizontal shell-and-tube heat

exchanger with cooling water in tubes and condensing

vapour in shell.

If condensate is very corrosive, or operating pressure high,

cooling water can be in shell and condensing vapour in

tubes.

A separate reflux drum to collect condensate and control

split between reflux and top product.

Normally all vapour is condensed but occasionally a partial

condenser is used.

Enough vapour is condensed to provide reflux, with

uncondensed vapour forming the top product.

19

What is the key difference between the 2 types of reboiler arrangements shown below?

Total reboiler: all the

incoming liquid is converted

to vapour no change in

composition

Partial reboiler: the vapour

leaving is in equilibrium with

the bottom product

acts as a stage in the

distillation column,

Design Considerations: Reboiler

15-Oct-13

11

Kettle Reboiler

Tube bundle at bottom of the shell; covered by the liquid to be boiled, leaving a

vapour space above it.

Heating fluid, normally steam is on the tube side.

Liquid from the bottom of the column is passed to the boiler and the vapour

generated returned to the column.

The remaining liquid forms the bottom product and is normally removed over a weir.

Vapour returned to column is in equilibrium with the bottom product, hence the kettle

reboiler acts as one theoretical stage.

Sometimes, the bundle is placed directly in the bottom of column to avoid piping.

21

Thermosyphon Reboiler

Liquid withdrawn from bottom of column, and partially vaporised in the reboiler.

Both vapour and liquid are returned to the column as a two-phase mixture.

Phase separation only occurs in the column, above the liquid level in the base.

Vertical and horizontal thermosyphon are used. In vertical type, liquid to be boiled is

on tube side while heating fluid on shell side.

Bottom product normally drawn at the column base. This stream is not in equilibrium

with the vapour, so the thermosyphon reboiler acts as less than a theoretical stage.

22

15-Oct-13

12

Fh

F

+ Q

R

= Dh

D

+ Wh

W

+ Q

C

+ Q

lost

Overall energy balance:

= 0

Energy balance over total condenser:

Q

C

= V

t

H

vap

Energy balance over partial reboiler:

Q

R

= V

b

H

vap

What about partial condenser / total reboiler?

where H

vap

= average molar heat of

vaporization of the cpns being separated.

Calculations can also be made using both

heats of vaporization knowing the

compositions of the streams

If saturated liquid feed: Q

R

~ Q

C

Design Considerations: Heat Duties

Total condenser

D

W

F

Partial reboiler

V

t

L

b

V

b

L

0

Q

C

Q

R

Example 1

A continuous distillation column is used to separate a mixture

containing 40 mol% A and the rest B to give a distillate of 95 mol%

A and bottom product of 96 mol% B. The column is operated at

1.5 times the minimum reflux ratio and at 1 atm pressure. It has a

total condenser and a partial reboiler The feed is an equimolar

mixture of liquid and vapour. Assume the mixture has a relative

volatility of 2.2, determine the number of theoretical plates and

location of the feed plate.

15-Oct-13

13

Continuous multistage distillation

1. What are the limiting conditions for distillation? How

to determine the minimum reflux ratio?

2. Where to introduce the feed?

3. What are the additional elements that should be

considered in the design of a continuous distillation

column?

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