Liquid extraction

INTRODUCTION

SUMMARY

PAGES

Introduction

General principles

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GENERAL
SUMMARY

Nadine LE BOLAY
Gilbert CASAMATTA

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Introduction
INTRODUCTION

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A process is often made up of a reaction step followed by separations.

When analyzing the process inINTRODUCTION
details, one can see that it consists of
a reactor fed with reagents and energy.
The products of the reactions (main reaction, but also secondary
reactions) flow out of the reactor, as well as the reagents that have
not reacted.
The purpose is then to separate the different products leaving the
reactor. In that way, separation equipment (generally several items)
are implemented.

Reagents
Energy

Reactor

Products
+
Reagents

S
E
P

S
E
P

In most cases, distillation is carried out. However, in certain

conditions, it is not suitable. Then, one may choose other separation
techniques, such as absorption, adsorption or liquid extraction, also
called solvent extraction.
It is particularly the case when:
-Liquids have boiling points with are close to each other
-Their boiling points have a high value
-The mixture forms an azeotrope
-Distillation must be performed under high vacuum conditions
-The products are heat-sensitive (recovery of antibiotics or vitamins)
-The mixture to be processed is a very diluted aqueous solution (the
latent heat of vaporization of water is very high)
-

We will study the case of liquid extraction

which is a physico-chemical separation of constituent
mixtures during a homogeneous phase

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GENERAL PRINCIPLES
GENERAL
PRINCIPLES

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Let us consider a homogeneous liquid mixture constituted by a diluent A

and a solute B which are miscible. The objective is to recover the solute.
Let us add a liquid solvent phase, non miscible with A.
Under the effect of agitation, the solvent phase is dispersed as
droplets in the diluent phase.
A part of the solute is transferred from the diluent phase to the
solvent phase.
When agitation is stopped, the two phases are separated by
decantation, the lighter phase (it will be supposed here that the
solvent is lighter than the diluent) being concentrated in the upper part
of the vessel.
The solvent phase is called the extract, the diluent phase is called the
raffinate. The two phases are at equilibrium. This equilibrium is
defined by an ideal stage.

S
Extract

A + B

+ B

+ eB
Raffinate

A stage is considered as ideal when the contact

between the phases is long enough in order
to reach the solute distribution equilibrium
between the extract and the raffinate

In practice, the diluent and the solvent are often partially miscible.
A small volume of the diluent may thus be contained in the extract, while
a small volume of the solvent may be present in the raffinate. The
extraction will thus be followed by as many separations as necessary in
order to recover the different constituents. At that stage, separations
may eventually be distillations if the limitation imposing extraction use no
longer exists (for example, the solvent and the solute do not form an
azeotrope which existed between the diluent and the solute).
The phases containing mainly the solvent can be recycled in the
extraction apparatus.

Extract

+ B +

S
E
P

S + eB (recycling)

S
E
P

eS + eA (recycling)

eA
B + eS

eA

+ eB + eS
Raffinate

eB
A + eS

Numerous solvents are used in liquid extraction. However all of them are
not suitable. The feed phase being imposed, the solvent choice must be
optimized. This choice is influenced by:
-its physico-chemical properties (allowing an easy recovery of the solute
or of the solvent),
-a negligible solubility of the solvent in the diluent (post-extraction
processes have to be as cheap as possible),
-physical characteristics offering acceptable dispersion and separation
times of the post-contact phases (viscosity, interfacial tension, density
difference compared to the feed),
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-favorable properties (Mass transfer kinetics equilibrium after contact

less than a few minutes - ; Economy cheap and available solvent - ;
Safety of use low toxicity, low flammability, low volatility, low
corrosion in comparison with usual construction materials -),
but particularly a property called selectivity.
The selectivity b is defined as the ratio:

[
b =

Solute B concentration

Diluent A concentration
Solute B concentration
Diluent A concentration

Extract

Raffinate

The necessary and sufficient condition for an extraction to be possible

is that b is greater than 1. The higher the value of b compared to 1,
the easier the extraction.

The selectivity can be written in a different form:

b=

Concentration of solute B/E

Concentration of solute B/R

This ratio is called the distribution

coefficient of the solute between
the extract and the
raffinate phases, m

Concentration of diluent A/R

Concentration of diluent A/E

As for the second ratio,

it is always greater than 1
(there is more diluent in the
raffinate than in the extract)

Consequently, a sufficient condition for a solvent to be selective is: m

greater than 1.
It should be noted that the higher the value of m, the higher the value
of b and thus the more selective the solvent.

No solvent offers all possible favorable conditions. Thus, a

compromise has to be found between all the constraints.

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Once the solvent has been chosen, the extraction process has to be
defined and designed. Four extraction techniques will be studied in this
course:

Countercurrent
with reflux

Single
stage
Crosscurrent

Countercurrent

To design an extraction apparatus, it is necessary to:

- determine the number of ideal stages
- determine the phases flowrates, as well as the solute
distribution between the phases
- choose the most adapted apparatus
- study the hydrodynamics of the apparatus
- determine the size and the configuration of the
apparatus
In the following chapters, we will learn how to determine the number of
ideal stages, the transfer of the solute in the extract, and the
flowrates of the phases with respect to the feed flow rate.

The other concepts will be studied in another course.

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The course will be divided into 6 chapters:

- CHARACTERISTICS AND PROPERTIES OF SOLVENTS

- LIQUID EQUILIBRIUM
- SINGLE STAGE EXTRACTION
- CROSS-CURRENT EXTRACTION
- COUNTER-CURRENT EXTRACTION
- COUNTER-CURRENT EXTRACTION WITH REFLUX

END OF THE INTRODUCTION

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