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1 Extraction

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4 views

1 Extraction

Uploaded by

vpraveen6831
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Contents

1. Introduction to liquid-liquid extraction; Liquid-liquid equilibria.


2. Effect of temperature on liquid-liquid equilibria.
3. Design calculation of single stage extraction.
4. Design calculation of multistage extraction.
5. Selection of extractors.
Liquid-Liquid Extraction (LLE)
• Liquid-liquid extraction (LLE) is a mass transfer operation in which
a solution (feed: a mixture of solute and carrier liquid) is brought
into intimate contact with a second immiscible or slightly miscible
liquid (solvent) in order to achieve the transfer of solute(s) from
the feed to the solvent.
• The solute rich phase is called the extract.
• The residual liquid (feed stream) that may have the little of the
solute left in it is called the raffinate.
Extract phase

Raffinate phase
mixing settling
Extraction Mechanism
• Bringing the feed and the solvent into intimate contact by dispensing
one phase into the other as droplets.
• Separation of extract and raffinate phase (different densities).
• Removal and recovery of the solute from the extract phase in a
relatively pure form,
• Removal and recovery of solvent from each phase (by distillation
usually).
Economics
In a typical liquid-liquid extraction process, only about 15% of the
capital cost goes towards the extractor and the remaining 85% goes
towards distillation, other equipment of solvent recovery and product
purification.
Only 5% operating cost is required for extractor and remaining 95%
towards solvent recovery.
Where extraction favours over distillation

• The components to be separated have close boiling points. If the


relative volatility is close to unity, number of trays in distillation will
be large and extraction will be favoured.
• Separation of heat sensitive materials, such as antibiotics vitamins
etc. (Penicillin -> butyl acetate),
• Recovery of non-volatile solutes, usually from aqueous solutions,
in hydro metallurgy.
• Recovery of a solute from a very dilute solution.
• Removal of organics from aqueous streams of phenol from
aqueous wastes.
Examples of Solvent Extraction

Extraction of aromatics: Petroleum industry


BTX separation from petroleum fraction by furfural, sulpholane (T. H.
Thiophene), NMP, Diethylene glycol, MEK, MIBK etc.

Recovery and concentration of antibiotics:

Penicillin is produced by fermentation. The concentration in fermentation


broth is 20 to 35 gm/L.

Recovery concentration of penicillin is done using a solvent, such as, amyl


acetate, butyl acetate or MIBK.
Flow sheet diagram for penicillin production.

At a pH of about 2, penicillin
remains in the acid form and
has a low solubility in water.

But it is favorably
transported to an organic
solvent from aqueous
fermentation

broth because of a high distribution coefficient. A reversal of distribution


coefficient occurs at a pH above 7.0. This pH dependent distribution
ofpenicillin in the water ester pair is made use of to recover, purify and
concentrate from broth. The experiments are carried out at 40°C.
Examples of Solvent Extraction

Extraction of caprolactum:
It is used for the manufacture of Nylon-6.
It is synthesized from cyclohexane. (cyclohexane -> cyclohexanol ->
cyclohexanone -> cyclohexanone oxime -> caprolactum).
The last step of the process involves reaction of oxime with H,SO, and
forms caprolactum and (NH4)2SO4.
The reaction mixture separates into an organic rich phase (“lactum oil”
containing 65 — 70% caprolactum).
These two phases are fed at appropriate locations of a “Rotating disk
contractor” Toluene is used as solvent phase.
Caprolactum goes to the extract and (NH4)2SO4 remains in the raffinate.

These two streams are further treated to get caprolactum in a pure form
and to recover the solvent and (NH4)2SO4

Other applications: Food, Pharmaceuticals, Metallurgical,


Environmental and Organic and Inorganic industries.
Liquid-Liquid Equilibria (LLE)
A liquid-liquid extraction system contains at least three components —
solute (C), carrier liquid in the feed (A) and extracting solvent (B).
Classification of Ternary Systems
Three binary systems can be formed, A-B, B-C, C-A. Mutual miscibility
behaviour of the component determines the nature of equilibrium diagram.
Categories
The carrier solvent (A) and extracting solvent (B) are practically immiscible.
The solute (C) is miscible with carrier solvent (A) and extracting solvent (B)
in all proportions. > Type I
The solute (C) is completely miscible with carrier solvent (A) but both solute
(C) and carrier solvent (A) have limited miscibility with the extracting solvent
(B). Type II
Equilateral Triangular Co-ordinates

Composition
20% A (Carrier liquid);
20% B (Extracting solvent);
60% C (Solute)
Liquid-Liquid Equilibrium (Type I)
C is miscible with A and B, A and B
practically immiscible.
Curve RPS is equilibrium diagram.
G1 and H1 Two liquid phases in equilibrium
G1 is rich in carrier (Raffinate)
H1is rich in solvent (Extract)
G1 - H1 is Tie line
Point “P” demarcates the raffinate and
extract sides of equilibrium curve and is
called “plait point”.
The type of curve RPS is called “binodal”
because it has two arms RP and PS.
A liquid mixture having “overall composition”
corresponding to a point K is a two phase
mixture.
Keeping undisturbed, it separates into
two phases at equilibrium.
The compositions are G2 and H2.
Amounts are given by “Lever arm rule”.
Liquid-Liquid Equilibrium (Type II)

The solute (C) is completely miscible


with carrier solvent (A) but both solute
(C) and carrier solvent (A) have
limited/partially miscibility with the
extracting solvent (B).

A-B and B-C are partially miscible.


The raffinate and the extract arm of
the equilibrium diagram do not meet,
so there is no “Plait point”
Right angled triangular diagram (Type I)
Mass fractions of the solute in the two phases (raffinate and extract) at
Equilibrium are plotted against the corresponding mass fractions of the
solvent.

Concentrations of the extract


phase are denoted by yA, yB
and yC, and those of the
raifinate are xA xB and xc
The raffinate arm PQ is
obtained by plotting the set
of point (xB , xC )

The extract arm PR is obtained by plotting the set of point (yB , yC )


Equilibrium plot on solvent free basis

In this presentation of LLE data, the mass


ratios of solutes (X and Y) in the two
Phases are plotted vs the corresponding
mass ratios (z or Z) of the solvent, on
solvent free basis.
* The quantities X, Y, z and Z are defined below:
X = xc /(xA + xc), z = xB /(xA + xc), (for raffinate)
Y = yc /(yA + yc), Z = yB /(yA + yc),) (for extract)

where, x is the mass fraction of solute in The plot X-z and Y-Z are called
raffinate. y is the mass fraction of solute in Maloney-Schubert diagram or
extract. Janecke diagram.
Problem 1 : Draw the Janecke diagram for a liquid-liquid system using the
following equilibrium data, Also show the tie lines in the diagram.
C

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