Crystallization

Is a solid-liquid separation
process, in which mass transfer
of a solute from the liquid
solution to a pure crystalline
phase occurs

Is the formation of solid

particles within a homogenous
phase

Is a unit operation used to

separate solutes from solution

Is the removal of a solute such

as a salt from a solution by
precipitating the solute from the
solution

Adsorption involves, in general, the

accumulation (or depletion) of solute
molecules at an interface (including
gas-liquid interfaces, as in foam
fractionation, and liquid-liquid
interfaces, as in detergency).
Adsorbate or solute - the material
being adsorbed
Adsorbent - the solid material being
used as the adsorbing phase
Physical Adsorption

Illustration

Industrial Application

Powdered salt for food industry

Production of sugar
Silicon crystal wafer production

Adsorption
A component of a gas or liquid
stream is removed and
adsorbed by a solid adsorbent
A separation process that
involves concentration of a
solute from a bulk vapor or
liquid phase on to the surface of
a porous solid.
The most common form of gassolid equilibrium

Occurs when the intermolecular

forces of attraction between the
fluid molecules and the solid
surface are greater than
attractive forces between
molecules of the fluid itself
A physical separation
process in which the adsorbed
material is not chemically
altered.
Reversible Process
The adsorption rate is generally
quite rapid
Also known as Van der Waals
adsorption

Chemical adsorption/ Chemisorption

Results from a chemical

interaction between the
adsorbate and adsorbent.

Only a monomolecular layer of

adsorbate appears on the
adsorbing medium

Frequently irreversible

Also known as Activated

adsorption

Factors Affecting Adsorption

Surface area of adsorbent

Adsorbate Solubility

Contact time or residence time.

Size of the molecule with

respect to size of the pores.

pH

Presence of other solutes

Commercial adsorbents
1. Activated carbon. This is a
microcrystalline material made
by thermal decomposition of
wood, vegetable shells, coal,
and so on, and has surface
areas of 300 to 1200 m2/g with
average pore diameters of 10 to
60 . Organics are mostly
adsorbed by activated carbon.
2. Silica gel. This adsorbent is
made by acid treatment of
sodium silicate solution and
then drying. It has a surface
area of 600-800 m2/g and
average pore diameters of 20 to
50 . It is primarily used to
dehydrate gases and liquids and
to fractionate hydrocarbons.
3. Activated alumina. To prepare
this material, hydrated
aluminum oxide is activated by
heating to drive off the water. It
is used mainly to dry gases and
liquids. Surface areas range
from 200-500 m2/g, with
average pore diameters of 20 to
140 .
4. Molecular sieve zeolites. These
zeolites are porous crystalline
aluminosilicates that form an
open crystal lattice containing
precisely uniform pores, which
makes it different from other
types of adsorbents, which have
a range of pore sizes. Different
zeolites have pore sizes from
about 3 to 10 . Zeolites are
used for drying, separation of

hydrocarbons, mixtures, and

many other applications.
5. Synthetic polymers or resins.
These are made by
polymerizing two major types of
monomers. Those made from
aromatics such as styrene and
divinylbenzene are used to
adsorb nonpolar organics from
aqueous solutions. Those made
from acrylic esters are usable
with more-polar solutes in
aqueous solutions.

Industrial Applications

Column Contact use a bed of

adsorbent to purify solutions
Slurry Contact use a powdered
adsorbent slurry to adsorb
desired materials
Gas Purifications
Gas bulk separation
Liquid purifications
Liquid bulk separation
Air-conditioning
Decolorization of cane refinery
syrups
Production of liquid sugar
Recovery of flavonoids, plant
extracts, colorants, aroma
Recovery of antibiotics and
proteins
Synthetic resin
Water purification
Waste water treatment

Centrifugation
Centrifugation is a process by which
solid particles are settled or filtered
from a liquid using centrifugal force as
a driving force.
It could also be that liquid particles are
settled from another liquid using the
same driving force.

Depending on the rotational speed

and distance from the axis of rotation,
the centrifugal force can be many
times greater than the force of gravity,
allowing even very small particles or
particles slightly denser than the fluid
to settle.

Chemical Procedures and Processes

Types of Centrifuges

Fuel and Biofuel Industry

Centrifugal Settling or Sedimentation

Under centrifugal force, the

solid phase assumed to be
denser than the liquid phase
settles out to the bowl wall.

Concurrently, the lighter, more

buoyant liquid phase is
displayed towards the smaller
diameter.

Centrifugal Filtration

In a filtering centrifuge,
separating solids from liquid
does not require a density
difference between the two
phases.
In both cases, the solids and
liquids move toward the bowl
under centrifugal force.
But in this type, the solids are
retained by the filter medium,
while the liquid flows through
the cake solids and the filter.

Chemical processing which

produces raw products such as
acids, salts, oil refinery byproducts, polymers, oil-watersolids, and so on.

Fuel and Biofuel industry

including synthetic fuels,
biodiesel, ethanol, cellulosic
ethanol, algae biomass
dewatering; fuel and lube oil
purification
Food Technology and Processing
Food Processing which deals
with refining of vegetable oils,
dairy (milk, cheese, etc.);
poultry, swine and beef
rendering; yellow, white, and
brown grease separation; fruit
and vegetable juice; beer, wine
and liquor clarification, etc.
Pharmaceutical and Biotechnological
Industries
Pharmaceutical and
Biotechnology industries that
manufacture drugs, vaccines,
medicines, penicillin, mycelia, Ecoli bacteria, algae, enzymatic
waste

Drying
Industrial Applications

Refers to the removal of

relatively small amount of water
from materials (Evaporation
large amount)

Water is usually removed as

vapor by air

Water Processing
Wastewater processing deals
with separation of municipal,
farm, DAF (dissolved air
flotation), trap grease, drilling
mud, and environmental
wastewater sludges.

May also refer to the removal of

other organic liquids, such as
benzene, from solids

Used in preservation techniques

known as Dehydration

Classification of Drying Processes

Batch the material is inserted

into the drying equipment and
drying proceeds for a given
period of time
Continuous the material is
continuously added to the dryer
and dried material is
continuously removed

Category of Drying Processes

Heat is added by direct contact

with heated air at atmospheric
pressure, and the water vapor
formed is removed by the air

Vacuum drying, the removal of

water proceeds more rapidly at
low pressure and heat is added
indirectly by contact with a
metal wall or by radiation.

Freeze drying, water is sublimed

from frozen material

Applications:

Serve as a preservation techniques product must contain less than 10% of

moisture to suppress the development
of unwanted microorganisms.
e.g.
Dried Salt 0.5%H2O; Dried
Casein (powdered milk) - 8% H2O
For Non Food Products:

use to remove the excess water in

wood (as part of Timber
processing), paper and pulp
industry, to prevent the
development of the molds
reduction in volume and weight of
the material

Extraction
a process where two immiscible or
partly miscible liquids are brought
in contact with each other so that
the soluble substance(s) in one
liquid (raffinate phase) passes into
the other liquid (extract phase) by
diffusion.

What are the reasons to use

extraction?

Separation not feasible by

distillation

Break azeotropes

Energy requirements of
distillation are prohibitive

A complex distillation sequence

is required

The material is heat sensitive

The material is non-volatile

Applications:

Biotechnology - Recovery of
carboxylic acids from biomass
such as fermentation broths,
recovery of oil from algae
broths, extraction of valuable
products from fermentation
broth.
Pharmaceuticals- Recovery of
active materials from
fermentation broths, purification
of vitamin products
Chemical- Washing of
acids/bases, polar compounds
from organics; Recovery of
acrylic acid; Recovery of tightly
hydrogen-bonded organics from
water such as formaldehyde,
formic acid and acetic acid
Effluent Treatment- Recovery
of phenol, DMF, DMAC;
Recovery of acetic acid from
dilute solutions
Polymer processingRecovery of caprolactam for
nylon manufacture, separation
of catalyst from reaction
products

Petroleum- Lube oil quality

improvement, separation of
aromatics/ aliphatics (BTX),
separation of olefins/ paraffins,
separation of structural isomers
Food- Decaffeination of coffee
and tea, separation of essential
oils (flavors and fragrances )
Inorganic- Purification of
phosphoric acid
Metals- Recovery of cobalt and
nickel, recovery of rare earth
elements
Nuclear- Purification of
uranium

Filtration
It is the separation of a fluid-solids
mixture involving passage of most
of the fluid through a porous
barrier, which retains most of the
solid particulates contained in the
mixture.
Suspended solid particles in a fluid
of liquid or gas are physically or
mechanically removed by using a
porous medium that retains the
particles as a separate phase or
cake and passes the clear filtrate.
The suspended solid particles can
be very fine or much larger, very
rigid or plastic particles, spherical
or very irregular in shape
aggregates of particles or
individual particles.
The feed or slurry solution may
carry a heavy load of solid
particles or a very small amount.
Filtration and filters can be
classified several ways:

1. By driving force. The filtrate is

induced to flow through the
filter medium by hydrostatic head
(gravity), pressure applied upstream of

the filter medium, vacuum or reduced

pressure applied downstream of the
filter medium, or centrifugal force
across the medium. Centrifugal
filtration is closely related to
centrifugal sedimentation, and both
are discussed later under
Centrifuges.
2. By filtration mechanism.
Although the mechanism for
separation and accumulation of solids
is not clearly understood, two models
are generally considered and are the
basis for the application of theory to
the filtration process. When solids are
stopped at the surface of a filter
medium and pile upon one another to
form a cake of increasing thickness,
the separation is called cake
filtration. When solids are trapped
within the pores or body of the
medium, it is termed depth, filtermedium, or clarifying filtration.
3. By objective. The process goal of
filtration may be dry solids (the cake is
the product of value), clarified liquid
(the filtrate is the product of value), or
both. Good solids recovery is best
obtained by cake filtration, while
clarification of the liquid is
accomplished by either depth or cake
filtration.
4. By operating cycle. Filtration may
be intermittent (batch) or continuous.
Batch filters may be operated with
constant-pressure driving force, at
constant rate, or in cycles that are
variable with respect to both pressure
and rate. Batch cycle can vary greatly,
depending on filter area and solids
loading.
5. By nature of the solids. Cake
filtration may involve an accumulation
of solids that is compressible or
substantially incompressible,
corresponding roughly in filter-medium

filtration to particles that are

deformable and to those that are rigid.
The particle or particle aggregate size
may be of the same order of
magnitude as the minimum pore size
of most filter media (1 to 10 m and
greater), or may be smaller (1 m
down to the dimension of bacteria and
even large molecules). Most filtrations
involve solids of the former size range;
those of the latter range can be
filtered, if at all, only by filter-medium
type filtration or by ultrafiltration
unless they are converted to the
former range by aggregation prior to
filtration.
Applications:

Metal and mineral processing

Filtration of seawater
Fouling prevention in furnaces

Settling/Sedimentation
(Particle-Fluid Separation)
The particles are separated from the
fluid by gravitational forces acting on
the particles.
The particles can be solid particles or
liquid drops. The fluid can be a liquid
or gas and it may be at rest of motion.
The purpose is to remove the particles
from the fluid stream so that the fluid
is free of particle contaminants.
Sedimentation is the partial separation
or concentration of suspended solid
particles from a liquid by gravity
settling.
Differential Settling and Separation of
Solids in Classification
1. Sink-and-float methods. A liquid
is used whose density is
intermediate between the

heavy or high-density material

and that of the light-density
material. In this liquid, the
heavy particles will not float but
settle out from the medium,
while the light particles will
float.
2. Differential settling methods.
The separation of solid particles
into several size fractions based
upon their settling velocities in
a particular medium is called
differential settling or
classification. The density of the
medium is less than that either
of the two substances to be
separated.
Applications

Removal of solids from liquid

sewage wastes
Settling of crystals from the
mother liquor
Settling of solid particles from a
liquid food
Settling of a slurry from a
soybean leaching process
Mining
Biological science
Beverage production
Air pollution control

Leaching

Leaching is concerned with the

extraction of a soluble constituent
from a solid by means of a solvent.
In leaching, soluble material is
dissolved from its mixture with an
inert solid by means of a liquid
solvent.
The method used for the extraction
is determined by the proportion of
soluble constituent present, its
distribution throughout the solid,

the nature of the solid and the

particle size.
the amount of soluble material
removed is often greater than in
ordinary filtration washing, and the
properties of the solids may
change considerably during the
leaching operation.

Processes Concerned
Dissolving the soluble
constituent.
Separating the solution, so
formed, from the insoluble solid
residue.
Washing the solid residue in
order to free it of unwanted
soluble matter or to obtain as
much of the soluble material as
possible as the product.

V2 , x2 V1 , x1

extractor

L0 , N 0 , y0 , B L1 , N1 , y1 , B

There are four important factors

to be considered:

Particle size- It is generally

desirable that the range of particle
size should be small so that each
particle requires approximately the
same time for extraction and, in
particular, the production of a large
amount of fine material should be
avoided as this may wedge in the
interstices of the larger particles
and impede the flow of the solvent.

Solvent- The liquid chosen should

be a good selective solvent and its

viscosity should be sufficiently low

for it to circulate freely.

Temperature- In most cases, the

solubility of the material which is
being extracted will increase with
temperature to give a higher rate
of extraction.

Agitation of the fluid- Agitation

of the solvent is important because

this increases the eddy diffusion

and therefore the transfer of
material from the surface of the
particles to the bulk of the solution,
as discussed in the following
section. Further, agitation of
suspensions of fine particles
prevents sedimentation and more
effective use is made of the
interfacial surface.