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Azeotrope mixtures

Minimum boiling point

Maximum boiling point

Azeotropic Distillation

Azeotrope mixtures

Liquid and vapor are exactly the same at a

certain temperature

It is a special class of liquid mixture that boils at

a constant temperature at a certain composition

Cannot be separated by a simple/conventional

distillation

Azeotropic Distillation

An introduction of a new component called

entrainer is added to the original mixture to form

an azeotrope with one or more of feed component

The azeotrope is then removed as either the

distillate or bottoms

The purpose of the introduction of entrainer is to

break an azeotrope from being formed by the

original feed mixture

Function of entrainer:

To separate one component of a closely boiling point

To separate one component of an azeotrope

Azeotropic Distillation

Azeotropic distillation is a widely practiced process

for the dehydration of a wide range of materials

including acetic acid, chloroform, ethanol, and many

higher alcohols.

The technique involves separating close boiling

components by adding a third component, called an

entrainer, to form a minimum boiling.

Normally ternary azeotrope which carries the water

overhead and leaves dry product in the bottom.

The overhead is condensed to two liquid phases; the

organic, "entrainer rich" phase being refluxed while

the aqueous phase is decanted.

Azeotropic Distillation

A common example of distillation with an azeotrope

is the distillation of ethanol and water.

Using normal distillation techniques, ethanol can

only be purified to approximately 89.4%

Further conventional distillation is ineffective.

Other separation methods may be used are

azeotropic distillation or solvent extraction

Azeotropic Distillation

The concentration in the vapor phase is the same as

the concentration in the liquid phase (y=x)

At this point, the mixture boils at constant

temperature and doesnt change in composition

This is called as minimum boiling point (positive

deviation)

Azeotropic Distillation

The characteristic of such mixture is boiling point

curve goes through maximum phase diagram

Example: Acetone-chloroform

Azeotropic Distillation

The most common examples:

Ethanol-water (89.4 mole%, 78.25 oC, 1 atm)

Carbon Disulfide-acetone (61 mol% CS2, 39.25oC, 1 atm)

Benzene-water (29.6 mol% water, 69.25 oC, 1 atm)

Azeotropic Distillation

Let say binary mixture: A-B formed an azeotrope

mixture

Entrainer C is added to form a new azeotrope with

the original components, often in the LVC, say A

The new azeotrope (A-C) is separated from the

other original component B

This new azeotrope is then separated into entrainer

C and original component A.

Hence the separation of A and B can be achieved

Azeotropic Distillation

Example: Acetic acid-water using entrainer n-butyl

acetate

Boiling point of acetic acid is 118.1 oC, water is 100 oC &

n-butyl acetate is 125 oC

The addition of the entrainer results in the formation of

a minimum boiling point azeotrope with water with a

boiling point = 90.2 oC.

The azeotropic mixture therefore be distilled over as a

vapor product & acetic acid as a bottom product

The distillate is condensed and collected in a decanter

where it forms 2 insoluble layers

Azeotropic Distillation

Example: Acetic acid-water using entrainer n-butyl

acetate

Top layer consist of nearly pure n-butyl acetate in

water, whereas bottom layer of nearly pure water

saturated with butyl acetate

The liquid from top layer is returned to column as reflux

and entrainer

The liquid from bottom layer is sent to another column

to recover the entrainer (by stream stripping)

multi component distillation

The calculation is a trial and error process

where

1. T is assumed

2. Value of relative volatility of each component

are then calculated using K values at the

assume T.

3. Then calculate value of Kc where

Kc= 1/(relative volatility x liq mole fraction)

value of Kc

5. Compare with T value read from table that

corresponds to the Kc.

6. If value is differ, the calculated T is used for the

next iteration.

7. After the final T is known, the vapor composition

is calculated from

Yi= (relative volatility x liq mole fraction)/(relative

volatility x liq mole fraction)

Discuss

example 11.7-1

Bubble point@boiling point

=temperature at which liquid begins to vaporize

Dew point

=temperature at which liquid begins to condense out of the

vapor

Three or more components in the products

The designer generally choose two components whose

concentrations or fractional recoveries in the distillate and

bottom products are a good index of the separation achieved

These two components are called key components

They must differ in volatility

Light key (L) is more volatile (vapor)

The heavy key (H) is less volatile (liquid

xL

xBL

xDH and

xDH means most of the heavy key ends up at the

distillate

Normally the key components are adjacent in the

rank order of volatility. Such choice is called a sharp

separation

In sharp separations the keys are only components

that appear in both products in appreciable

concentrations

The vapor-liquid equilibria for a mixture are

described by distribution coefficients or K factors

y ie

where; K

x ie

K is the ratio of mole fractions in the vapor and liquid

phases at equilibrium

If Raoults Law and Daltons Law hold, Ki can be

calculated from the vapor pressure and total pressure of

the system.

Pi = xiPi

; yi = Pi/P

y i pi pi pi

Ki

x i p.pi

p

y i / xi

Ki

ij

y j / xj Kj

the relative volatility of the

components

ij

Pi

P j

1. For bubble point (initially boiling point of a liquid

mixture)

N

i 1

i 1

2. y i K i x i 1.0

-----(1)

yi

1 .0

xi

i 1

i 1K i

N

----(2)

4. A temperature is assumed

5. Obtain Ki values from chart

point)

8. If Kixi > 1.00, a lower temperature is chosen until

equation (1) is satisfied

9. If (yi/ Ki) > 1.00, a higher temperature is chosen until

equaition (2) is satisfied

10.The bubble point and dew point are obtained when

equation (1) and (2) is satisfied

11.The compositions can be determined with the formula:

yi

K i xi

N

K i xi

i 1

or

xi

yi / Ki

N

y i /K i

i 1

Example

Find the bubble-point and the dew point temperatures and

the corresponding vapor and liquid compositions for a mixture

of 33 mole % n-hexane, 37 mole % n-heptane and 30 mole %

n-octane at 1.2 atm total pressure. (The equilibrium K values

for hydrocarbon system is given)

Choose T = 105 C, where the vapor pressure of the

middle component at 1.2 atm. Construct and fill in the

table:

Component

1 Hexane

2 Heptane

3 Octane

Pi at

Ki = Pi/P

105C,

1.2 atm

xi

yi =Kixi

2.68

1.21

0.554

0.33

0.37

0.30

0.7359

0.3737

0.1386

2.23

1.01

0.462

contribution comes from hexane, pick a temperature

where Ki is lower by a factor (1/1.248)

Example;

1/1.248 x 2.23 = Pi/1.2

Pi = 2.14 atm where T = 96 C

Component

1 Hexane

2 Heptane

3 Octane

Pi at

96C, 1.2

atm

2.14

0.93

0.41

Ki =

Pi/P

xi

yi =Kixi

1.8

0.33 0.5940

0.755 0.37 0.2868

0.342 0.30 0.1025

=

0.9833

yi

calculated

0.604

0.292

0.104

=

1.00

yi

K i xi

N

K i xi

i 1

Therefore, the vapor in equilibrium with the liquid is 60.4

mol % n-hexane, 29.2 mole % n-heptane and 10.4 mole %

n-octane.

Choose a higher T = 105 C as first guess

Component

1

2

3

Hexane

Heptane

Octane

Pi at

105C, 1.2

atm

2.68

1.21

0.554

Ki = Pi/P

xi

xi =yi/Ki

2.23

1.01

0.462

0.33

0.37

0.30

0.148

0.366

0.655

=

1.169

In order to reduce yi/Ki , Ki has to increase by a

factor 1.169

Therefore, K3 = 0.458 x 1.169 = 0.535

K3 = Pi/P

17 %

higher

which give T = 110 C

Componen

t

Hexane

Heptane

Octane

P i

Ki

yi

yi/Ki

3.0 2.5

0.33 0.132

1.38 1.15 0.37 0.3217

0.64 0.535 0.30 0.5625

= 1.0162

xi calculated

0.130

1.317

= 1.00

composition of the liquid in the equilibrium with the

vapor is calculated by formula;

xi

yi / Ki

N

y i /K i

i 1

which 13.0 mole % n-hexane, 31.7 mole % nheptane and 55.3 mole % n-octane.

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