Professional Documents
Culture Documents
Size Reduction
Introduction: Milling is a general trade name which normally means reduction of food grain
into various end products like meal, flour, splitted products etc. Milling includes cleaning,
grading, separating, mixing, pearling, polishing, dehusking, size reduction etc.
Definition: The breakdown of solid material through the application of mechanical forces is
known as size reduction.
The term size reduction is associated with all the means by which solid particles are cut or
broken into smaller pieces. In processing stages solids are reduced in size and shape by various
methods for different purposes. Reduction in size is brought about by mechanical means without
change in chemical properties of materials.
a) Size reduction may aid the extraction of a desired constituent from a composite structure.
Eg. Flour from wheat grains or juice from sugar cane.
b) Reduction to a definite size range may be a specific product requirement. Eg. As the
manufacture of icing sugar, in the preparation of species and in chocolate refining.
c) A decrease in particle size of material leads to an increase in surface of the solid. This
increase in surface is of assistance in many rate process e.g.
i) The drying time for moist solids is much reduced by increasing the surface area
of the solid.
ii) The rate of extraction of a desired solute is increased by increasing the contact
area between solid and solvent.
iii) Process time required for certain operations such as cooking, blanching etc. can
be reduced by cutting, shredding or dicing the process material.
d) Intimate mixing or blending is usually easier with smaller size ranges of particles an
important consideration in the production of formulated, packaged soups, cake mixes etc.
Size: To determine the size of food grains usually three mutual perpendicular lengths of
practical are measured. These may be called as longest, intermediate and smallest length or
length, breadth and thickness of the particle.
Dp = (l x b x t) 1/3
Screening: Screening is the unit operation in which a mixture of various sizes of solid
particles is separated into two or more fractions by passing over a screen. In general
processing screening is widely used for separating mixtures of granulated and powered
materials into size ranges.
Screen aperture: The space between the individual wires of a wire mesh screen is
known as screen aperture.
For determination of average particle size in ground food grains, a set of Indian Standard
Screens is arranged serially in stack. For food grain flour analysis, a set of IS Sieves No. 100,
70, 50, 40, 30, 20 and 15 with pan and cover is taken.
Fineness Modules: The fineness modulus indicates the uniformity of grind in resultant
product. It is determined by adding the weight fractions retained above each sieve and
dividing the sum by 100.
Average particle size (Dp): It is represented in terms of fineness modulus can be estimated
by the following equation
Dp = 0.135 (1.366)F.M.
Crushing efficiency: The ratio of the surface energy created by crushing to the energy
absorbed by the solid referred as crushing efficiency ƞc
The energy absorbed by a unit mass of the material is given by the following equation
e A p − Af
Ea =
ƞc
Where, e = Surface energy per unit area
The unit energy (E) requirement for size reducing machine is greater than the energy
absorbed by the solid (Ea)
The ratio of the energy absorbed to the input energy is known as the mechanical efficiency
ƞm
Ea e Ap − A
f
E= =
ƞm ƞc ƞm
The power required by the machine can be calculated by the following equation
f e Ap − Af
𝑃=𝐸𝑥𝑓=
ƞc ƞm
Rittinger’s Law: It is considered that for the grinding of solids, the energy required should be
proportional to the new surface produced and put n=2
OR A crushing law proposed by Rittingers states that the work required in crushing is
proportional to the new surface created.
Rittinger’s assumed that size reduction is essentially a shearing procedure. Therefore, energy
requirement is proportional to the square of the common linear dimension and thus the values of
n=2
1 1
𝐸 =c( − )
Xp Xf
Where Xp and Xf is length of product and feed
Rittinger’s law has been found to hold better for fine grinding, where a large increase in
surface results.
Kick’s Law: It is considered that the energy required for a given size reduction was proportional
to the size reduction ratio, which requires that n=1
OR It is based stress analysis of plastic deformation within elastic limit. He assumed that the
energy requirements for size reduction is a function of a common dimension of the material
therefore the value of n = 1.
Xf
𝐸 = c ln ( )
Xp
Where, Xp and Xf is length of product and feed
Kick’s law has been found to hold more accurately for coarser crushing.
Crushing operation the energy requirement suggested by Kick’s law appears to be too low,
whereas that required by Rittinger’s equation appears to be excessive.
Bond’s Law: Bond reported a method for estimating the power required for crushing and
grinding operation. According to this law the work required to form particles of size D p from
very large feed is proportional to the square root of the surface to volume ratio of
the product.
𝑝 1 1
= 0.3162 𝓌𝑖 ( − )
𝑓 √𝐷𝑝 𝐷𝑓
Where P= Power in kW
f= Feed rate in t/hr
Dp= 80% of product passes through mesh of diameter in mm
Df = 80% of feed passes through mesh of diameter in mm
𝓌𝑖 = Work index
Size reduction of solids involves creating smaller mass units from larger mass units of the same
material. To bring this about, the larger mass units need to be subjected to stress by the
application of force. Three types of force may be applied, i.e. compression, impact and shear.
Compressive forces are generally used for the coarse crushing of hard materials. Careful
application of compressive forces enables control to be exercised over the breakdown of the
material, e.g. to crack open grains of wheat to facilitate separation of the endosperm from the
bran. Impact forces are used to mill a wide variety of materials, including fibrous foods. Shear
forces are best applied to relatively soft materials, again including fibrous foods. All three types
of force are generated in most types of mill, but generally one predominates. For example, in
most roller mills compression is the dominant force, impact forces feature strongly in hammer
mills and shear forces are dominant in disc attrition mills
Compressive forces are used for the coarse crushing of hard materials.
Impact force can be regarded of a variety of food materials.
Attrition or shear forces are extensively used in machines for the comminution of softer,
non-abrasive materials in the smaller size ranges, i. e. Fine grinding. .
The extent of the breakdown of a material may be expressed by the reduction ratio,
which is the average size of the feed particles divided by the average size of the products
particles.
The term average size depends on the method of measurement. In the food industry, screening or
sieving is widely used to determine particle size distribution in granular materials and powders.
In this case, the average diameter of the particles is related to the aperture sizes of the screens
used. Size reduction ratios vary from below 8:1 in coarse crushing to more than 100:1 in fine
grinding. The objective in many size reduction operations is to produce particles within a
specified size range.
1) Mechanical Properties of the Feed: Friable and crystalline materials may fracture easily
along cleavage planes. Larger particles will break down more readily than smaller ones.
Roller mills are usually employed for such materials. Hard materials, with high moduli of
elasticity, may be brittle and fracture rapidly above the elastic limit. Generally, the harder
the material, the more difficult it is to breakdown and the more energy is required. Hard
materials are usually abrasive and so the working surfaces should be made of hard
wearing material, such as manganese steel, and should be easy to remove and replace.
Such mills are relatively slow moving and need to be of robust construction. Disc mills,
pin-disc mills or cutting devices are used to break down fibrous materials.
2) Moisture Content of the Feed: The moisture content of the feed can be of importance in
milling. If it is too high, the efficiency and throughput of a mill and the free flowing
characteristics of the product may be adversely affected. In some cases, if the feed
material is too dry, it may not breakdown in an appropriate way. For example, if the
moisture content of wheat grains are too high, they may deform rather than crack open to
release the endosperm. Or, if they are too dry, the bran may break up into fine particles
which may not be separated by the screens and may contaminate the white flour. Wheat
is usually ‘conditioned’ to the optimum moisture content before milling. Another
problem in milling very dry materials is the formation of dust, which can cause
respiratory problems in operatives and is a fire and explosion hazard. In wet milling, the
feed material is carried through the action zone of the mill in a stream of water.
3) Temperature Sensitivity of the Feed: A considerable amount of heat may be generated
in a mill, particularly if it operates at high speed. This arises from friction and particles
being stressed within their elastic limits. This heat can cause the temperature of the feed
to rise significantly and a loss in quality could result. Some mills are equipped with
cooling jackets to reduce these effects. Cryogenic milling involves mixing solid carbon
dioxide or liquid nitrogen with the feed. This reduces undesirable heating effects. It can
also facilitate the milling of fibrous materials, such as meats, into fine particles.
4) Hardness and Abrasiveness of feed: Although not a primary consideration in food
processing operation, knowledge of the hardness of the feed material can be important in
selecting comminution equipment. Hard materials are more difficult to comminute. More
energy is required and residence times in the action zone must be longer. Hard materials
are usually abrasive so wear of working surfaces can be pronounced.
The size of agricultural products may be reduced by several ways, but mainly the following four
methods are used in a size reduction machines.
I. Crushing:-
When an external force applied on the material excess of its strength, the material fails because
of its rupture in many directions. The particles produced after crushing are irregular in shape and
size. The type of material and method of force application affects the characteristics of the new
surfaces and particles. Food grain flour, grits and meal, ground feed for livestock are made by
crushing process. Crushing is also used to extract oil from oilseeds and juice from sugarcane.
II. Impact:-
When the material is subjected to sudden blow of force in excess of its strength, it fails, like
cracking of nut with the help of hammer. Operation of hammer mill is an example of the
dynamic force application by impact method.
III. Shearing:-
It is the process of size reduction which combines cutting and crushing. The shearing units
consist of a knife and a bar. If the edge of the knife or the shearing edge is thin enough and
sharp, the size reduction process nears to that of cutting, whereas a thick and dull shearing edge
performs like a crusher. In a good shearing unit the knife is usually thick enough to overcome the
shock resulting from material hitting. In an ideal shearing unit the clearance between the bar and
the knife should be as small as practicable and the knife as sharp and thin as possible.
IV. Cutting:-
In this method, the size reduction is accomplished by forcing a sharp thin knife through the
material. In the process minimum deformation and rupture of the material results and the new
surface created is more or less undamaged. An ideal cutting device is a knife of excellent
sharpness and it should be as thin as practicable. The size of fruits and vegetables are reduced by
cutting.
Classification of Size reduction equipment: Machines of various types and sizes are available
for the comminution of food materials.
1) Crushers
a) Jaw crusher
b) Gyratory crushers
c) Crushing rolls
2) Grinders
a) Attrition mill or Burr mill or Plate mill
b) Hammer mill
c) Ball mill
d) Rod mill
e) Colloid mills
1) Crushers: This type of reducing machines squeeze or press the material unit it breaks.
Crushers are mostly used to break large pieces of solid materials into small lumps.
Crushers are used in industrial operations like mines etc.
a) Jaw crusher: In a jaw crusher feed is admitted between two jaws, which are open at
the top like V. One of the jaws is fixed and somewhat vertical as shown in fig. While
the other is the swinging jaw. This jaw reciprocates in a horizontal plane, and makes
and angle of 20 to 30o with the fixed jaw. The movable jaw is operated by an
eccentric unit so as to impart great compressive force. The solids which to be broken
is caught between the two jaws. Large lumps of solid materials are caught between
the upper parts of the jaw and subsequently broken and dropped into the narrower
space below. The broken pieces are further reduced next time when jaws come closer.
The number of strokes given to the movable jaw by eccentric unit ranges between 250
to 400 times per minute.
b) Crushing rolls: In this machine, Two or more heavy steel cylinder revolves
towards each other. Particles of feed are nipped and pulled through the rolls
experiencing compressing force which cuts them.
The throughput of these units is governed by roller length and diameter and by the
speed of rotation. With larger diameters, speeds of 50-300 RPM are usual. Size
reduction ratio are low usually below an overload compression spring protects the
rollers surface from damage, but hard, foreign bodies should remove before crushing.
In agricultural operations crushing rolls are mainly used for extraction of juice from
sugarcane. The crushing rolls are of two types
1) Smooth roll crusher: Two heavy smooth faced metal rolls rotating towards each other
at same speed on parallel horizontal axes the working elements of the smooth roll
crusher. It is shown in fig. The size of the particles/ material that can be caught by the
rolls depends upon the coefficient of friction between the material and the roll surface.
The rolls exert force and to avoid any damage to roll surface because of some
unbreakable material coming with the feed at least one of the rolls should be spring
loaded.
2) Grinders:
a) Attrition mill :-
In an attrition mill the grains are rubbed between the grooved flat faces of rotating
circular disks. These mills are also known as burr or plate mills. The axis of the
roughed disk may be horizontal or vertical. In attrition mill one plate is stationery and
fixed with body of the mill, while other one is rotating disk. The material is fed
between the plates and is reduced by crushing and shearing. Mills with different
patterns of grooves, corrugations on the plates perform a variety of operation. The
disks of burr mills are usually 20-137 cm in diameter and operating speed at 350-700
rpm. These mills are used for making whole grain & dehusked grain flour but their use
in spices grinding is limited. Double runner disk type attrition mills are also available.
These are used for grinding of soft materials. Its operating speed between 1200-7000
rpm, hence the capacity of such mills is large.
Since much of the milling carried out in the food industry is for the production of very
small particle size, this type of mill finds extensive applications. Two types of disc
mill are shown in fig.
i) Single disc mill: In this device the food stock passes into a narrow
gap between a high speed, rotating grooved disc and the stationary
casing of the mill. The gap is adjustable, depending on feed size and
product requirements.
ii) Double disc mill: In this modification the casing contains two
rotating disc. The disc rotates in opposite directions giving a greater
degree of shear than that attainable in the single disc mill.
The fineness of grinding in burr mills is controlled by the type of plates & the gap
between them. The spacing between the plates is adjustable.
Advantages:-
a) Lower initial cost.
b) Lower power requirement.
Disadvantage:-
a) Foreign matter may cause damage.
b) Operation without feed may result in burr wear.
b) Hammer mill:-
Hammer mills are used for various types of size reduction jobs. These mills contain a
high speed rotor rotating inside a cylindrical casing. The shaft is usually kept
horizontal. Materials are fed into the mill from the top of casing and is broken by the
rotating hammers & fall out through a screen at the bottom. The material of feed is
broken by fixed or swinging hammer which are pinned to a rotor. The hammers are
rotated between 1500-4000 rpm. Strike & grind the material until it becomes small
enough to pass through the bottom screen as shown in figure.
Fineness of grinding is controlled by the screen size. Hammers are either rigidly fixed
to shaft or swinging in case of swinging hammer mill. There is less chance of damage
of hammer if some unbreakable solid materials comes to milling chamber along with
feed. Hammer mill can grind almost anything like food grains, hard rock, sticky clay,
steel chips. The kinetic energy of the rotating hammers is used to disintegrate the feed.
The capacity and power requirement of hammer will depend on the nature of the feed
to be ground. Commercial mills reduce solids between 60 to 240 kg/kWhr of energy
consumption.
Advantages:-
a) Design & Work is very simple and versatile
b) Freedom from damage during empty operations
c) Less chance of damage of mill due to foreign object or material
Disadvantages:-
a) High power requirement
Uses:-
a) Poultry feed grinding
b) Spices grinding
c) Wet sorghum and millets grinding
d) Potato, Banana flour making.
c) Colloid mill:
In principle a colloid mill consists of a stationary surface (stator) and a rotating surface
(rotor) separated by a small adjustable clearance through which the crude emulsion is
passed. The premixed emulsion ingredients pass through a narrow gap between a
stationary surface (stator) and a rotating surface (rotor). In doing so the liquid is
subjected to shear and turbulence which brings about further disruption of the droplets
of the internal phase and disperses them throughout the external phase. The gap between
the stator and rotor is adjustable within the range
50–150 µm. One type of colloid mill is depicted as shown in fig. The rotor turns on a
vertical axis in close proximity to the stator. The clearance between them is altered by
raising or lowering the stator by means of the adjusting ring. Rotor speed ranges from
3000 rpm for a rotor 25 cm in diameter to 10 000 rpm for a smaller rotor 5 cm in
diameter. Rotors and stators usually have smooth stainless steel surfaces. Carborundum
surfaces are used when milling fibrous materials. Colloid mills are usually jacketed for
temperature control. This type of mill, also known as a paste mill, is suitable for
emulsifying viscous materials. For lower viscosity materials the rotor is mounted on a
horizontal axis and turns at higher speeds, up to 15 000 rpm. Mills fitted with rotors and
stators with matching corrugated surfaces are also available. The clearance between the
surfaces decreases outwardly from the centre. The product may be discharged under
pressure, up to 700 kPa. Incorporation of air into the product is limited and foaming
problems reduced in this type of mill.
Tumbling Mills
A typical tumbling mill consists of a cylindrical shell, sometimes with conical ends,
which rotates slowly about a horizontal axis and is filled to about 50% of its volume with
a solid grinding medium. As the shell rotates the loose units of the grinding medium are
lifted up on the rising side of the shell to a certain height. They then cascade and cataract
down the surface of the other units. The material being comminuted fills the void spaces
between the units of the grinding medium. Size reduction takes place between these units
in the jostling as they are lifted up and in the rolling action and impact as they fall down.
The most commonly used grinding media are balls and rods. Contamination of the feed
material due to wear of the grinding medium is a problem with tumbling mills and needs
to be monitored.
1) Ball mills:
The ball mill is cylindrical or conical shape slowly rotating about a horizontal axis. Half
of its volume is filled with solid grinding balls as shown in figure. The shell is usually
made of steel lined with high carbon steel plates, porcelain or silica rock. For medium
and fine reduction of abrasive materials ball mills are used. In a ball mill size reduction
is achieved by impact of the balls when they drop from near the top of the shell. The
balls are carried up at the side of the shell nearly to the top. By gravity the balls drop on
the feed underneath. The energy consumed in lifting the balls is utilized for grinding job.
When the ball mill is rotated, the balls are carried by the mill wall nearly to the top,
where they are released by gravitational pull and drop to the bottom and picked up again.
Centrifugal force keeps the ball in contact with the mill wall. Most of the grinding is
done by impact of balls due to centrifugal force. If the speed of rotation of mill is faster
the balls are carried to more distance. The rotational speed at which the centrifuging
occurs is known as critical speed. The rotational speed of the ball mills are kept at 65 to
80% of the critical speed, with the lower values for wet grinding in viscous suspension.
2) Rod Mills: Grinding rods, usually made of high carbon steel, are used instead of balls in
rod mills. They are 25–125 mm in diameter and may be circular, square or hexagonal in
cross-section. They extend to almost the full length of the shell and occupy about 35% of
the shell volume. In such mills, attrition forces predominate but impacts also play a part in
size reduction. They are classed as intermediate grinders and are more useful than ball
mills for milling sticky materials.
1) Open circuit grinding: This is the simplest method of operating a mill. No ancillary
classifying system are used so the capital outlay for the plant is low. Feed enters the mill
passes through the action zone and is discharged as product. No recycle of oversize particles
(having a size range greater than that desired) is possible.
2) Free crushing: With this method of operation residence time in the action zone is kept
short. When used in conjunction with open circuit grinding, this is commonly accomplished
by allowing the feed material to fall through the action zone under gravity. Unnecessary
breakdown of small particles is limited so the formation of undersize particles (particles
smaller than the desired size range) is reduced. This mode of operation is more economic.
3) Choke feeding: In choke feeding the discharge of product is restricted by inserting a screen
in the outlet from the machine. For a given feed material remains choked in the action zone
of the mill until reduced to a size capable of passing the screen.
4) Closed circuit grinding: The residence time of material in the mill is kept short, either by
gravity fall or by rapid transport through the action zone in an air or water stream. The
discharge stream from the mill passes to a classifying system where oversize material is
removed and recycled back to the mill. In this way the mill works bigger particles so
wasteful power consumption is minimized.
5) Wet Milling: If the feed material is wet or can be wetted without harm this method of
operation may be considered. The feed stock is ground as a suspension in a carrier liquid
stream often water. Dust problems associated with dry milling are overcome ad hydraulic
classification techniques such as sedimentation and centrifugation may be employed for
separating desired size fractions.
1) Slicing: Sliced fruits are much in demand as a dessert dish. They present an attractive
appearance the portions produced being of a convenient size for eating. Rotary cutting
knives are usually employed the knives being set to cut the material being presented to
them often on a vibrating belt into parallel slices of the desired thickness.
2) Dicing: It is the cutting of material into cube usually follows a preliminary slicing
operation which produces slice of desired thickness. These slices are then fed onto a
conveyor belt containing a series of studs which hold the slices in position as the belt
carries them against a rotary knife assembly which cuts them into strips. The strips then
pass through a further cutting zone at right angles to the stripping section.
3) Shredding: Shredding the food material is torn into small fragments the average size of
the pieces depending on the type machine and on residence time in the action zone.
Shredding often precedes dehydration the increase in surface aiding rate process.
Hammer mills are commonly used as shredders.
4) Pulping: Pulping is another comminution operation widely used in the processing of
lower grade fruits separated during grading. The fruit which edible but unacceptable for
whole fruit processing, may be used in jam manufacture. A combination of pulping and
sieving is used with many fruits and vegetables. A common form of pulper consists of a
cylindrical perforated screen contacting high speed rotating brushes. Material is fed to the
inside of the cylinder the brushes forcing pulped material through the perforations. Stalks
skins and stones pass over the screening surface as reject.
i) Wheat The structure of the wheat grain is complex but, in the context of this section,
it can be assumed to consist of three parts, i.e. the outer layer or bran, the white
starchy endosperm and the embryo or germ. According to Meuser. “The objectives of
milling white flour are: 1. To separate the endosperm, which is required for the flour,
from the bran and embryo, which are rejected, so that the flour shall be free from bran
specks, and of good colour, and so that the palatability and digestibility of the product
shall be improved and its storage life lengthened. 2. To reduce the maximum amount
of endosperm to flour fineness, thereby obtaining the maximum extraction of white
flour from the wheat.” The wheat grain contains about 82% of endosperm, but it is
not possible to separate all of it from the bran and embryo. In practice, the extraction
rate is in the range 70–80%. Prior to milling, the wheat grains are cleaned to remove
metal fragments, stones, animal matter and unwanted vegetable matter and
conditioned to the optimum moisture content for milling. A mill consists of two
sections, a break section and a reduction section. The clean grain is fed to the break
section, which usually consists of four or five pairs of fluted rolls. The rolls rotate
towards each other at different\ speeds. As the grains pass through the first pair of
break rolls they are split open. Some large fragments of endosperm (semolina) are
released together with a small amount of small particles, less than 150 µm in size,
which is collected as flour. The fragments of bran coming from these rolls will have
endosperm attached to them. The fractions from the first break rolls are separated by
sieving Sorghum, millets and maize and rye may be dry milled using modified flour
milling systems.
ii) Rice Unlike most milled cereal products, in the production of milled rice the
endosperm is kept as intact as possible. Brown rice is dehulled using rubber covered
rolls or by means of abrasive discs. The bran and embryo are then removed, a process
known as whitening. This may be achieved by means of abrasive cones or rolls
iii) Maize This cereal is wet milled to produce a range of products including starch, oil
and various types of cattle feed. Cleaned maize is steeped in water, containing 0.1–
0.2% sulphur dioxide, at 50 oC for 28–48 h. The steeping softens the kernel and
facilitates separation of the hull, germ and fibre from each other. The SO2 may disrupt
the -SS- bonds in the protein, enabling starch/protein separation. After steeping, the
steep water is concentrated by vacuum evaporation and the protein it contains is
recovered by settling. The steeped maize is coarsely milled in a Foos Mill. The grain
is cracked open and the germ released. The germ is recovered by settling or by means
of hydrocyclones. Oil may be extracted from the germ by pressing. The degermed
material is strained off from the liquid and milled in an impact or attrition mill.
iv) Oil Seeds and Nuts: It is common practice to flake or grind oilseeds prior to
extraction, either by pressing or solvent extraction, in order to rupture the oil cells.
Hammer mills and attrition mills are sometimes used for the preliminary breakdown
of large oil seeds such as copra or palm. However, flaking rolls are usually used to
prepare seeds for extraction. A common arrangement used for cottonseed, flaxseed
and peanuts consists of five rolls located one above the other. The seed is fed in
between the top two rolls and then passes back and forth between the rolls down to
the bottom of the stack. Each roll supports the weight of the rolls above it, so the
seeds are subjected to increasing pressure as they move down the stack. The top roll
is grooved, but the others have smooth surfaces.
v) Sugar Cane: Large, heavy duty, two- or three-roll crushers are used to break and
tear up the cane to prepare it for subsequent milling for the extraction of the sugar.
The surfaces of the rolls are grooved to grip the cane and very high pressures are
applied to the cane, 8–12 t dm–2. Following this initial crushing, the cane may be
further broken down in shredding devices, which tear open the cane cells and release
some of the juice. These devices are essentially large-capacity hammer mills, with
rotors turning at 1000–1200 rpm, carrying hammers pivoted to discs or plates. To
extract the juice, the shredded cane is passed through a series, usually five, of triple-
roll mills. These are heavy-duty rolls, with grooved surfaces which exert high
pressure, 15–30 t dm–2 on the cane, expressing the juice. This is not a size reduction
operation as such, but is an example of another use of roller mills. Mills may be
jacketed and cooled. Cryogenic milling, using liquid nitrogen, can result in higher
quality products. Sugar crystals may be ground in impact mills to produce icing
sugar. Particles of milk powder, lactose and dry whey may be reduced in size in
impact mills.
Mixers
Introduction: Mixing is a unit operation widely used in food processing. In addition to blending
components together, mixing operations may bring about other desirable changes in the materials
being mixed, such as mechanical working (as in dough mixing), promotion of heat transfer (as in
freezing ice cream) facilitating chemical or biological reactions (as in fermentation). The
components in a mixing operation may be liquids, pastes, dry solids or gases. The degree of
uniformity attainable in a mixing operation varies, depending on the nature of the components. In
the case of low viscosity miscible liquids or highly soluble solids in liquids a high degree of
uniformity is attainable. Less intimate mixing is likely to occur in the case of viscous liquids,
pastes and dry solids. Efficient utilisation of energy is another criterion of mixing. This is more
easily attainable in the case of low viscosity liquids as compared with pastes and dry solids.
OR It is an operation in which two or more components are interspersed in space with one
another.
1) Stationary vessel containing a moving stirrer, agitator, paddle i.e. an impeller or impeller
assembly mounted on a rotating shaft. Impellers mounted in vertical tanks are widely
used for mixing low viscosity liquids, free flowing liquid/solid suspensions and for the
dispersion of gases in liquids.
2) Stationary vessel containing moving paddles, vanes, knives, screws etc. These mixers
have been developed for mixing higher consistency materials such as viscous liquids,
doughs, pastes, fats etc.
3) Moving vessel containing moving and/or stationary paddles, vanes, knives, screws etc.
Mixers in this category are used for very high consistency mixes such as doughs, pastes
and plastic materials.
These three classes of mixer cater for low, intermediate and high consistency mixes.
Classification Mixers:
A) Mixers of Low and Moderate Viscosity Liquids: The impeller mixer is the most
commonly used type of mixer for low viscosity liquids (viscosity less than 10 Ns/ m2).
Such a mixer consists of one or more impellers, fixed to a rotating shaft and immersed in
the liquid. As the impellers rotate, they create currents within the liquid, which travel
throughout the mixing vessel. If turbulent conditions are created within the moving
streams of liquid, mixing will occur. Turbulence is usually most vigorous near the
impeller and the liquid should pass through this region as often as possible. The fluid
velocity in the moving streams has three components: (a) a radial component acting in a
direction at right angles to the shaft, (b) a longitudinal component acting parallel to the
shaft and (c) a rotational component acting in a direction tangential to the circle of
rotation of the shaft.
If an impeller agitator is mounted on a vertical shaft located centrally in a mixing vessel,
the liquid will flow in a circular path around the shaft. If laminar conditions prevail, then
layers of liquid may form, the contents of the vessel rotate and mixing will be inefficient.
Under these conditions a vortex may form at the surface of the liquid. As the speed of
rotation of the impeller increases this vortex deepens. Rotational flow may cause any
suspended particles in the liquid to separate out under the influence of centrifugal
force.Rotational flow, and hence vortexing, may be reduced by locating the mixer off
centre in the mixing vessel and/or by the use of baffles. Baffles usually consist of vertical
strips fixed at right angles to the inner wall of the mixing vessel. These break up the
rotational flow pattern and promote better mixing. Usually four baffles are used, with
widths corresponding to 1/18th (5.55%) to 1/12th (8.33%) of the vessel diameter.
Three main types of impeller mixers are used for liquid mixing:
i) Paddle agitators
ii) Turbine agitators
iii) Propeller agitators
ii) Turbine agitators: A turbine mixer has four or more blades attached to the same shaft,
which is usually located centrally in the mixing vessel. The blades are smaller than
paddles and rotate at higher speeds, in the range 30–500 rpm. Simple vertical blades as
shown in Fig. (a) Promote rotational and radial flow. Some vertical flow develops when
the radial currents are deflected from the vessel walls. Swirling and vortexing are
minimized with the use of baffles. Liquid circulation is generally more vigorous than that
produced by paddles and shear and turbulence is high near the impeller itself. Pitched
blades as shown in Fig. (b) Increase vertical flow. Curved blades as shown in Fig. (c) are
used when less shear is desirable, e.g. when mixing friable solids. Vaned or shrouded
discs as shown in Fig. (d) Control the suction and discharge pattern of the impeller and
are often used when mixing gases into liquids. Turbine mixers are used for low and
moderate viscosity liquids, up to 60 Ns/ m2, for preparing solutions and incorporating
gases into liquids.
iii) Propeller Mixer: This type of mixer consists of a relatively small impeller, similar in
design to a marine propeller, which rotates at high speed, up to several thousand rpm. It
develops strong longitudinal and rotational flow patterns. If mounted on a vertical shaft
and located centrally in the mixing vessel, baffling is essential shown in Fig. (a & b).
Alternatively, the shaft may be located off centre in the vessel and/or at an angle to the
vertical shown in Fig. (c). When mixing low viscosity liquids, up to 2 Ns/ m2, the
currents developed by propeller agitators can travel throughout large vessels. In such
cases the shaft may enter through the side wall of the tank shown in Fig. (d). Special
propeller designs are available which promote shear, for emulsion premixing. Others
have serrated edges for cutting through fibrous solids.
Four main types of mixers are used for High Viscosity Liquids:
i) Pan mixers
ii) Horizontal trough mixers (Kneaders , Dispersers, Masticators)
iii) Continuous Mixers for Paste like Materials
iv) Static Inline Mixers
i) Pan mixers: These are two general types. In the stationary pan mixer fig (a) the mixing
elements move in a planetary path visiting all parts of the stationary mixing pan.
Elements are used singly or in pairs and usually designed to provide only a small
clearance between each other and the pan walls. In the rotating pan type the mixing
vessel is mounted on a rotating turntable fig (b). The mixing elements also rotate but in
one position and are located near the pan wall. Mixing elements vary in design
depending on the duty. Pan are removable either by raising or tilting the elements or by
lowering the pan support.
iii) Static Inline mixers: When viscous liquids are pumped over specially shaped stationary
mixing elements located in pipes, mixing may occur. The liquids are split and made to
flow in various different directions, depending on the design of the mixing elements.
Many different configurations are available. The energy required to pump the materials
through these mixing elements is usually less than that required to drive.
C) Mixers for Dry Solids: In the mixing of particulate solid materials the probability of
getting an orderly arrangement of particles is virtually zero. In practical systems the best
mix attainable is that in which there is a random distribution of the ingredients.
Solid mixing is generally regarded as arising from one or more of three basic
mechanisms. These are as follows
i) Convection: The transfer of masses or groups of particles from one location
to another.
ii) Diffusion: The transfer of individual particles from one location to another
arising from the distribution of particles over a freshly developed surface.
iii) Shear: The setting up of slipping planes within the mass also resulting
mixing of groups of particles.
The movement of particles during a mixing operation can also result in segregation of the
particles arising from difference in their properties. Thus in any mixing operation mixing and de-
mixing occur concurrently and the intimacy of the resulting mix depends on the predominance of
the of the former mechanism over the latter. The properties of the ingredients that most influence
their mixing are particle size, shape and density. Other properties are also important including
surface and flow characteristics, moisture content and tendency to cluster.
The importance of segregation on the degree of homogeneity achieved in solids mixing cannot
be over emphasized. Any tendency for segregation to occur must be recognized when selecting
solids mixing equipment. Segregation in a mixture of dry solids is readily detected by use of
heap test.
i) Tumbler Mixers: These operate by tumbling the mass of solids inside a revolving
vessel. These vessels take various forms as shown in fig. Such mixers may be fitted
with baffles or stays to improve their performance and some have separately driven
internal rotating devices to help break up cluster. These shells rotate at speeds up to
100 rpm and their working capacity is normally 50-60% volume of its vessel. They
are constructed from a wide variety of materials including stainless steel and are fitted
with ports or valves for filling and emptying. Tumbler mixers are best suited to the
gentle blending of powders with similar physical characteristics. Segregation can be a
problem if particles vary particularly in size and shape.
iii) Vertical screw mixers: A rotating vertical screw located in a cylindrical or cone-
shaped vessel is another device used for mixing solids. The screw may be fixed
iv) Fluidised bed mixers: Fluidised beds may use for mixing solids and are quite
effective for particles with similar settling characteristics. Also of course the solid
particles must have good fluidizing characteristics.
Mixing of Gases and Liquids: Gases may be mixed with low viscosity liquids using impeller
agitators in mixing vessels. Turbine agitators are generally used for this purpose. In unbaffled
vessels, vortexing can draw gas into the liquid. However, the gas may not be well distributed
throughout the liquid. It is more usual to use baffled vessels with relatively high-speed turbine
impellers. Impellers with six, 12 and even 18 blades have been used. Pitched blades and vaned
discs are particularly suited to this duty. Some special designs of vaned discs, featuring concave
rather than flat blades, have been used for this purpose. Gas may be introduced into liquids using
some designs of static inline mixers. More heavy duty equipment, such as pan and Z-blade
mixers, may be used to introduce gas into more viscous materials. For example whisk-like
elements in pan mixers may be used to whip creams. Other types of elements, such as forks,
hooks and gates, are used to introduce air into doughs and batters. Dynamic, inline systems, such
a scraped surface heat exchangers may be used to heat or cool viscous materials while at the
same time introducing gas to aerate them, such as in the manufacture of ice cream,
A) Low Viscosity Liquids: Examples of applications for impeller mixers include: preparing
brines and syrups, preparing liquid sugar mixtures for sweet manufacture, making up fruit
squashes, blending oils in the manufacture of margarines and spreads, premixing
emulsion ingredients.
B) Viscous Materials: Examples of applications for pan mixers and kneaders include:
dough and batter mixing in bread, cake and biscuit making, blending of butters,
margarines and cooking fats, preparation of processed cheeses and cheese spreads,
manufacture of meat and fish pastes.
Filtration
Introduction: Solid-liquid filtration, hereinafter called filtration may be defined as that unit
operation in which the insoluble solid component of a solid-liquid suspension is separated from
the liquid component by passing in latter through a porous membranes or septum which retains
the solid particles on its upstream surface or within its structure or both. The solid-liquid
suspension is known as the feed slurry or prefilter. The liquid component that passes through the
membranes is called the filtrate and the membrane itself is referred to as the filter medium. The
separated solids are known as the filter cake once they form a detectable layer covering the
upstream surface of the medium.
The equipment in which filtration washing and drying is carried out kwon as filter.
The flow of filtrate may be brought about by means of gravity alone by the application of a
pressure greater than atmospheric upstream of the medium is known as Pressure filtration.
The application for filtration in the food industry are divided into three categories:
1. Cake filtration: Embraces all those application wherein slurries containing appreciable
amounts of insoluble solids i.e. more than one or two percent by weight are separated into
their solid and liquid components. Either the liquid or solid component or both may be
valuable. In such operations a cake is formed on the upstream surface of the medium and
the process is known as cake filtration.
2. Clarification: It involves removing small quantities of insoluble solid from a valuable
liquid is known as clarification. here the object usually is to produce a clear liquid and the
solids are generally unwanted In such filtration a cake may build up on the medium or
alternatively where the amount of solids is very small they may become enmeshed within
the structure of the medium.
3. Microfiltration: It involves the removal of very fine particles of order of 1 µm or less is
known as microfiltration. It is generally directed at removing microorganism from liquid
foods.
Theory of Filtration:
In the initial stages of filtration the first particles of solid to encounter the filter medium
become enmeshed in it reducing its open surface area and increasing the resistance it offers to
the flow of filtrate. As filtration proceeds a layer of solids builds up on the upstream face of the
medium and this layer or cake increases in thickness with time. Once formed this cake in fact
becomes the primary filtering medium. Filtrate passing through a filter encounters three types of
resistance (a) That offered by the channels and ports of the filter itself (b) That offered by the
filter medium (c) That offered by the filter cake.
Filter cake resistance: Many slurries contain non-rigid deformable solid particles or
agglomerates of particles. The resistance to flow in cakes formed from such solids depends on
the pressure drop and also varies throughout the depth of the cake being highest near the filter
medium such cake is known as compressible.
Washing cake: In most filter cake washing is carried out by substituting wash liquid for the
feed slurry when filtration is complete. Thus the wash liquid follows the same paths through the
cake as the filtrate. In such an operation if the physical properties of the wash liquid notably
viscosity are the same as the filtrate the rate of washing will be approximately equal to the final
rate of flow of filtrate. Since washing is usually carried out at constant pressure the rate of
washing remain approximately constant.
Filter media: The main function of the filter medium is to promote the formation of a cake of
solids and to support it once formed. The medium should offer the minimum resistance to flow
consistent with the rapid formation of a filter cake. It must be strong enough to support the cake
and retain its strength under the extreme conditions occurring during the operation. Its surface
characteristics should be such as to facilitate cake removal. The medium must be non-toxic and
chemically compatible with the material being filtered. It must not be too expensive.
Filter media may ne rigid of flexible rigid media may be loose such as sand and/or gravel,
diatomaceous earths or charcoal. Such loose media are seldom used alone food applications.
Fixed rigid media are also used. These include porous carbon, porcelain fused alumina,
perforated metal plates, rigid wire meshes or edge media. Such rigid media are available in the
form of plates, discs, tubes and other shapes.
Filter aids: When the solids to be filtered off are very finely divided or are of a slimy highly
compressible character the filter medium tends to block quickly and only short runs are
possible. In such circumstances materials are known filter aids are often used. These usually
consist of comparatively large inert, non-compressible solid particles of different shapes. They
may applied by mixing with the feed slurry or they may be suspended in a clear liquid often
some filtrate from a previous run which is then passed through the filter so that a precoating of
the filter aid builds up on the medium. The filter aid forms a rigid lattice structure on the
medium and provides numerous channels through which the filtrate can flow thus slowing up
the plugging of the medium and prolonging the filtration cycle.
Filtration Equipment:
I. Pressure filters
a) Vertical plate pressure filters (filter presses)/ Plate and frame filter press
b) Horizontal plate filters
c) Shell and leaf pressure filters
d) Shell and tube pressure filters
e) Edge pressure filters
II. Vacuum filters
a) Continuous rotary drum vacuum filters
b) Rotary vacuum disc filters
III. Centrifugal filters
a) Batch centrifugal filters
b) Batch centrifugal filters
I. Pressure filters: In pressure filters a superatmospheric pressure is maintained
upstream of the medium to induce the flow of filtrate through the system. This
upstream pressure is achieved by pumping the feed slurry throughout filtration or the
pressure may be gradually increased so as to maintain a constant flow rate of filtrate.
Various combinations of these two basic methods may also be used.
The maximum pressure used in pressure filters is usually of the order of 25 – 75 psig
(276 – 621 kN/m2) but some filters operate at much higher pressures.
a) Vertical plate pressure filters (filter presses)/ Plate and frame filter press: A
vertical drainage place supporting a filter medium is the basic filtering element in
a vertical plate press. A commonly used design is the plate and frame press. In
this type of filter grooved plates covered on both sides with filter medium
alternate with frames in a rack as shown in fig (a).
The assembly of plates and frames can e squeezed tightly together by a screw
hydraulic or pneumatic mechanism to form a liquid tight unit. The filter medium
also acts as a gasket preventing leakage between the plates and frames. Both
plates and frames are provided with openings at one corner and when the press is
closed theses openings from a channel through which the feed slurry is
introduced. In addition the hollow centre of each frame is connected by a
auxiliary channel to this feed channel as shown in fig (b).
The feed slurry enters the frames and the cake builds up in the hollow centre of
the frames. The filtrate passes through the medium and on the grooved surfaces
of the filter plates from where it is removed via an outlet channel in each plate.
Filtration is continued until the flow of filtrate drops below a practical level or the
pressure reaches an unacceptably high level due to the cake packing tightly in the
frames. After filtration washing of the cake may be carried out by replacing the
flow of feed slurry with wash liquid. However more effective washing is obtained
by the use of special wash plates as shown in fig. (b) These are arranged in the
press so that every second’s plate is wash. During filtration these wash plates act
as filter plates. During washing the outlets from the wash plates are closed and
the wash liquid introduced on to their surfaces through a special inlet channel.
The flow path for both filtration and washing when wash plates are used is shown
in fig. (c). the cake is removed manually after opening the press.
c) Shell and leaf pressure filter: These filters have a filter leaf as the basic filter
element. A filter leaf consists of a wire mesh screen or grooved detaining plate
over which the filter medium is stretched. The leaf may be suspended from the
top or supported from the bottom or centre. The supporting member is usually
hollow and forms an outlet channel for the filtrate as shown in fig.
In horizontal shell and leaf filters the filter leaves are mounted vertically in a
horizontal pressure tight vessel. The feed slurry is introduced under pressure into
the shell and the cake builds up on the outer surfaces of the leaves. The filtrate
passes through the medium and drains from the inner structure of the leaves into
the outlet channel provided. Leaves may be rectangular or circular in shape and
may be stationary as shown in fig. (a, b) or rotating slowly about a horizontal axis
as shown in fig. (c). the rotation of the leaves at 1-2 rpm promotes uniform cake
build up. Filtration is continued until the cake thickness reaches a predetermined
value, and then washing is carried out either by replacing the slurry with wash
liquid or alternatively by sluicing down the cake using water jets, re-slurring and
re-filtering it. Cake removal is achieved either by withdrawing the leaves from
the shell and cleaning them manually or by sluicing down cake with the bottom
half of the open.
Shell and leaf filters are flexible and can be economic in the use of labour,
especially where cake discharge from the closed shell is possible. They have a
higher capital cost than plate filters. Pressure used do not normally exceed about
60 psig (0.52 MN/m2 ) but units can work at 250 psig (1.85 MN/m2)
d) Shell and tube pressure filters: These filters incorporate cylindrical tube,
instead of a leaf as the basic filter element. The tubes are usually suspended
vertically from the filtrate take always in vertical pressure vessels. Tubes may be
made of perforated and metal wire mesh, plastics or porous stone. Their features
are similar to shell and leaf filters but they usually have smaller capacities and are
almost always used with a precoating of filter aid.
e) Edge pressure filters: A stack of closely spaced rings or discs often known as a
filter pile forms the basic feature of an edge filter. The discs are mounted one
above the other on a fluted rod and held in position between a boss and nut as
shown in fig. The edges of the discs are separated by gaps of the order of 0.001 –
0.01” (25.4 – 254 µm) by means of projections on the rings. The required number
of these filter piles may be fixed in a head plate and enclosed in a pressure vessel.
In operation a precoat of filter aid is built up at the edges of the discs. The feed is
introduced under pressure into the shell and the cake builds up over the precoat.
Filters pass through the precoat through the spaces between the discs and out via
the grooves in the supporting rod. Premixing of filter aid with the slurry is usually
practiced in addition to precoating. Cake is removed when filtration and washing
are complete by back blowing and/or back flushing through the filtrate outlet and
removing the sludge formed through a bottom outlet.
partly submerged in an open tank of slurry. Filter medium covers the entire drum
surface and is supported by perforated plates grids or wire meshes to provide
drainage space between the medium and the floor of each shallow compartment.
The drum rotates at speeds of the order of 0.1 – 2 rpm. Consider one compartment
on the drum surface e.g. the shaded one shown in fig. As the drum rotates and this
compartment becomes submerged in the slurry a vacuum is drawn on it by means
of the automatic rotary valve. Filtrate flows through the medium and out through
the drain pipe from the compartment and is directed to the filtrate receiver by
means of the valve. A layer of cake builds up on the outer surface of the medium.
As the compartment emerges from the slurry the cake is sucked free of filtrate. As
it proceeds further on its cycle the draining from the compartment are diverted to
another receiver by means of sprays. As the compartment passes from beneath the
sprays the cake is sucked free of washings. Further on its cycle the compartment
is disconnected from its vacuum source and compressed air is introduced beneath
the filter medium for a short period loosing the cake from the surface of the
medium. This is again controlled by the automatic rotary valve. The cake is
removed by means of a scraper knife. Then as the compartment becomes
submerged in the slurry again vacuum is reapplied and new cycle commences.
Thus each compartment behaves as an individual filter operating in a sequence
which results in the continuous delivery of filtrate and discharge of cake.
III. Centrifugal filtration: This term describes the separation of solids from a liquid by
filtration when the flow of filtrate is induced by centrifugal means. The general
principle of the centrifugal filter is shown in fig. The slurry is fed into a rotating bowl
with a perforated wall which is lined with a suitable filter medium. The solids are
thrown to the bowl wall and form a filter cake through which the filtrate passes under
the influence of centrifugal force then through the filter medium and perforated
basket wall. In the latter both the centrifugal force and the filtering area increase with
increase in radius. Centrifugal force acts on the filtrate passing through the cake and
on the cake itself supplementing the hydraulic head.
Centrifugal filtrations are of two types:
hydrogenating fats and oils are recovered by filtration. Since hydrogenated fats have
relatively high melting points, heated plate filters may be used.
2. Sugar Refining: The juice produced by extraction from sugar cane or sugar beet contains
insoluble impurities. The juice is treated with lime to form a flocculent precipitate which
settles to the bottom of the vessel. The supernatant liquid is filtered to produce a clear
juice for further processing. Plate-and-frame presses, shell-and-leaf and rotary drum
vacuum filters are used. The settled ‘mud’ is also filtered to recover more juice. Plate-
and-frame presses or rotary drum vacuum filters are used for this duty. Filtration is also
used at a later stage in the refining process to further clarify sugar juice. In the production
of granulated sugar, purified sugar juice is concentrated up to 50–60% solids content by
vacuum evaporation and seeded with finely ground sugar crystals to initiate
crystallization. When the crystals have grown to the appropriate size, they are separated
from the juice in batch or continuous centrifugal filters.
3. Beer Production: During maturation of beer, a deposit of yeast and trub forms on the
bottom of the maturation tank. Beer may be recovered from this by filtration using plate-
and- frame presses, shell-and-leaf or rotary drum vacuum filters. The beer is clarified by
treatment with isinglass finings, centrifugation or filtration. If filtration is used, the beer is
first chilled and then filtered through plate-and-frame, horizontal plate or edge filters. In
the case of plate filters, the filter medium consists of sheets of cellulose, aluminum oxide
or zirconium oxide fibers, with added kieselguhr. Insoluble polyvinyl pyrrolidone may
also be incorporated into the medium to absorb phenolic materials associated with beer
haze. Edge filters are precoated with filter aid and more filter aid is usually added to the
beer prior to filtration. Yeasts and bacteria may also be removed from beer by filtration.
4. Wine Making: Wine is filtered at different stages of production: after racking, after
decolorizing and finally just before bottling. Plate-and-frame presses, shell-and-leaf
filters, edge filters and precoated rotary drum vacuum filters have been used. Filter media
are mainly sheets made of cellulose incorporating filter aid material (mainly
diatomaceous earth) which is bound into the cellulose sheets with bitumen. With edge
and precoated drum filters, loose filter aid material is used.
There are many other applications for filtration in the food industry, including the
filtration of starch and gluten suspensions and the clarification of brines, sugar syrups,
fruit juices, yeast and meat extracts.
CENTRIFUGATION
Introduction
Mechanical separations are divided into four groups- sedimentation, centrifugal separation,
filtration and sieving. (In sedimentation, two immiscible liquids or a liquid and solid, are
separated by allowing them to come to equilibrium under the action of gravity, the heavier
material falling with respect to the lighter. This may be a slow process and it is often speeded
up by applying centrifugal forces to increase the rate of sedimentation; this is called
centrifugal separation. Filtration is the separation of solids from liquids, by causing the
mixture to flow through fine pores which are small enough to allow the liquid to pass.
Classification of solid particles is often done by sieving.
In mechanical separation studied, the forces considered are gravity, combinations of gravity
with other forces, centrifugal forces, pressure forces in which the fluid is forced away from
the particles, and finally total restraint of solid particles where normally the fluid is of little
consequence. The velocities of particles moving in fluid are important for several of these
separations. Particles in a liquid, under a constant force, for example the force of gravity,
accelerate for a time and thereafter move at uniform velocity. This maximum velocity which
they reach is called their terminal velocity. The terminal velocity depends upon the size,
density and shape of particles, and upon properties of fluid.
Sedimentation uses gravitational forces to separate particulate material from fluid streams.
The particles are usually solid, but they can be small liquid droplets and the fluids can be
either liquid or gas. Sedimentation is very often used in food processing industry for
separation of dirt and debris from incoming raw material, crystal from their mother liquors
and dust or product particles from air streams.
Centrifugation:
The separation by sedimentation of two immiscible liquids or of a liquid and solid depends
on the effects of gravity on components. Some time separation is very slow because the
specific gravities of the components may not be very different because of forces holding the
components in association.
The applications of centrifugation are discussed under four heading.
1) Separation of immiscible liquids
2) Centrifugal clarification
3) Desludging
4) Centrifugal filtration.
Other applications for centrifugal equipment are separation of gas-solid systems (Cyclone
separator), separation of Vapour-liquid systems (entrainment separator).
Thus the magnitude of centrifugal force depends on the radius of rotation, the speed of
rotation and the mass of the body or, for a unit volume of material, the density of the
material. If two immiscible liquids A and B with densities ρA and ρB respectively are placed in
the cylindrical bowl which rotates about a central axis, the more dense liquid A will tend to
move towards the walls of bowl and form an angular ring near its inner surface as shown in
figure. The less dense liquid B will be displaced towards the centre of rotation and form an
inner annular ring as shown in figure. If provision made for introduction the liquid feed
continuously to the bowl and for tapping off from the liquid layers separately, separation of
liquid can achieved. The feed is usually introduced to the bottom of the bowl by a centrally
located pipe and the liquids removed from each layer by a weir system.
The dense liquid flows out over a circular weir of radius R A and the lighter liquid over one
radius RB. If we assume that the liquid rotates bowl speed, that is, that slippage and friction
are negligible, and then the drop in pressure, arising from centrifugal force, between R i and
RA must equal the pressure drop between Ri and RB. If this was not so interface would not be
stable at radius Ri.
B) Centrifugal Clarification:
This is the term used here to describe the removal of small quantities, a few percent or
loss, of insoluble solids from a liquid by centrifugal means. If a liquid containing solids
with a greater density than liquid is fed to rotating cylindrical bowl, the solids will move
towards the bowl wall. If an outlet is provided for the liquid near the centre of rotation,
e.g. if the outer exit (radius RA) in the bowl shown in figure is closed off, then those
particles of solids which reach the bowl wall will remain in the bowl. Those particles
which do not reach the bowl wall will be carried out in the liquid. The fraction remaining
in the bowl and the fraction passing out in a liquid will be controlled by the rate of feed
i.e. the dwell time in bowl.
C) Desludging:
This term is used here to describe the removal of solids from liquid by centrifugal
means when the quantity of solids present exceeds that which can be handled by a
simple clarifiers (that is, when solids content is greater than 5% or 6% by weight of
feed). In such systems provision is made for removal of solids from the centrifuge
bowl during its operation. The general theory is discussed in centrifugal clarification
is applicable, but errors occurs due to solids movement system altering the conditions
on which the formulae are based and more complex expressions need to be used.
from the top with a guide provided for the base. The feed is introduced through a
stationary pipe to the bottom of the bowl and quickly accelerated to bowl speed by means
of vanes or baffles. The two liquids are removed from the annular layers formed through
a circular weir system as shown in fig. and discharge into stationary covers. Bowl
dimensions range from 3 to 6’ (7.6 to 15.2 cm) diameter and up to 5” (1.5 m) high. A
typical unit 4’diameter and 30’ high would rotate at 15000 rpm and laboratory models
rotate up to 50000 rpm.
b) Disc bowl centrifuge: In this type of centrifuge a relatively shallow, wide, cylindrical
bowl rotates at moderate speed in a stationary casing. The bowl is usually bottom driven.
The feed is normally introduced to the bottom of the bowl through a centrally located
feed pipe from above. The bowl contains a number of closely spaced metal cones called
discs which rotate with the bowl and are located one above the other with the fixed
clearance between them as shown in fig. (a). The discs have one or more sets of matching
holes which form channels through which the feed material flows as shown in fig. (b).
Under the influence of centrifugal force the dense phase travelling towards the bowl wall
streams down the undersides of the discs while light phase displaced towards the centre
flows over the upper faces of the discs as shown in fig (c). The liquids are thus divided
into thin layers and the distance any drop of one liquid must travel to get caught up in
and removed in the appropriate outgoing stream is very small. The separation efficiency
of disc bowl centrifuge is much better than rotating at a similar speed.
Bowl diameter range from 8 to 40’ (20 -102 cm) and the spacing between the discs is of
the order of 0.02 – 0.05’ (0.5-1.3 mm). A 12’diameter bowl rotating at 6400 rpm
develops a force equivalent to 7000 times.
2. Centrifugal clarifiers: Both tubular and disc bowl centrifuge may be used for clarifying
small quantities of solids from liquids. If the dense phase outlets are closed off and the
liquid is removed through the central outlet then most of the solid particles with diameter
greater than the cut point diameter will remain as a deposit on the bowl wall. The solids
capacity of tubular bowl machines is seldom more than 2-4.5 kg and for economical
operation the solids content of the feed should normally not exceed about 1% by weight.
Disc bowl machine have solids capacities in the range 2-20 kg.
a. Solid bowl clarifier: Where large volumes of liquid containing small quantities of
solid (1-2%) with good settling characteristics need to be clarified simple large
diameter 24-42’(60-108 cm) cylindrical bowls without discs may be used as shown
in fig. These are operated on a batch principle and when a cake of solids of the
maximum thickness is formed the feed is cut off excess liquid removed with a
skimmer pipe and the solids cut out with knife or plough and dropped through an
opening in the bowl floor.
b. Cylinder bowl (Multi chamber) centrifuge: This machine is shown in fig. The
bowl is divided into a number of annular chambers and the liquid follows a
circuitous path to the bowl wall and exit port. The coarsest particles are removed in
the inner chamber and the finest in the outer. Again the centrifuge is operated on a
batch principle and is suitable for handling feed with about 1% or less of solids.
c. Nozzle discharge (self cleaning) centrifuge: This centrifuge is of the disc bowl type
but the bowl shown in fig. is biconical in shape. A number of holes of the order 3-4
mm diameter are spaced around the bowl at its largest diameter. The solids removed
from liquid are continuously discharged in the form of thick slurry into an outer
casing. Feeds contacting up to 25% solids can be handle in this type of clarifier.
one or two revolutions per minute faster than the latter. The solids are carried to one end
of the bowl by the conveyor and discharged while the liquid leaves through adjustable
ports at the other end. Such machine can handle feeds with up to 50% solids and wide
range of particle size.
c. Reciprocating conveyor (push type) centrifuge: Single stage push type centrifuge
machine shown in fig. The feed enters the rotating basket through rotating funnel
which accelerates it gently to bowl speed. A layer of solids 2.5 – 7.6 cm thick forms
on the bowl wall and this layer is moved towards the open end of the basket by a
reciprocating pusher a few inches at a time. On each return stroke of the pusher the
feed funnel which reciprocates also delivers feed to the freshly exposed basket wall.
The cake may be washed as shown and is finally spun off the open lip of the basket
into the stationary casing. Basket diameters are of the order of 0.3 – 1.2 m.
d. Screen conveyor centrifuge: It is perforated bowl is used through which the filtrate
escapes. Other types employ rotating about a vertical axis as shown in fig.
the gums after these treatments. In the case of acid-degumming, the degummed oil may
be washed with hot water and the washings removed by centrifugation. The next step in
oil refining is neutralisation. The free fatty acids, phosphatides and some of the
pigments are treated with caustic soda to form soap stock which is then separated from
the oil by centrifugation, using nozzle or self-opening centrifuges. The oil is then
washed with hot water and the washings removed by centrifugation.
3. Beer Production: Centrifugation may be used as an alternative to filtration at various
stages in the production of beer. Nozzle discharge centrifuges may be used for
clarifying rough beer from fermenting vessels and racking tanks. Self-opening
centrifuges may be used for wort and beer clarification. Centrifuges used for the
treatment of beer may be hermetically sealed to prevent the loss of carbon dioxide and
the take-up of oxygen by the beer. Self-opening centrifuges may also be used for the
recovery of beer from fermenters and tank bottoms. Decanting centrifuges maybe used
for clarifying worts and beers containing relatively high contents of yeast or trub. They
may also be used as an alternative to self-opening machines to recover beer from
fermenters and tank bottoms.
4. Wine Making: Centrifugation may be used instead of or in combination with filtration
at various stages in the production of wine. Nozzle or self-opening centrifuges are
generally used. Applications include: the clarification of must after pressing, provided
that the solids content is relatively low, the clarification of wine during fermentation to
stabilise it by gradual elimination of yeast, the clarification of new wines after
fermentation and before filtration, the clarification of new red wines before filling into
barrels and the facilitation of tartrate precipitation for the removal of tartrate crystals.
5. Fruit Juice Processing: Centrifugation may be used for a variety of tasks in fruit juice
processing. Self opening centrifuges are used to remove pulp and control the level of
pulp remaining in pineapple and citrus juices. Centrifuged apple juice is cloudy but free
from visible pulp particles. Tubular bowl centrifuges were originally used to clarify
apple juice but more recently nozzle and self-opening machine are used. The use of
hermetically sealed centrifuges prevents excessive aeration of the juice. In the
production of oils from citrus fruits centrifugation is applied in two stages. The product
from the extractor contains an emulsion of 0.5–3.0% oil. This is concentrated up to 50–
70% oil in a nozzle or self-opening centrifuge. The concentrated emulsion is then
separated in a second centrifuge to produce the citrus oil.
Separations by the use of membranes are becoming increasingly important in the process
industries. In this relatively new separation process, the membrane acts as a semipermeable
barrier and separation occurs by the membrane controlling the rate of the movement of various
molecules between two liquid phases, two gas phases, or a liquid and a gas phase. The two fluid
phases are usually miscible and the membrane barrier prevents actual, ordinary hydrodynamic
flow. A classification of the main types of membrane separation follows:
1. Gas diffusion in porous solid: In this type a gas phase is present on both sides of the
membrane, which is a microporous solid. The rates of molecular diffusion of the various gas
molecules depend on the pore sizes and the molecular weights.
2. Liquid permeation or dialysis: In this case, the small solites in one liquid phase diffuse
readily because of concentration differences through a porous membrane to the second liquid (or
vapour) phase. Passage of large molecules through the membrane is more difficult. This
membrane process has been applied in chemical processing separations such as separation of
H2SO4 from nickel and copper sulfates in aqueous solutions, food processing separations such as
separation of kidneys. In electrodialysis, separation of ions occurs by imposing an imposing an
emf difference across the membrane.
3. Gas permeation in a membrane: The membrane in this process is usually a polymer such as
rubber, polyamide, and so on, and is not a porous solid. The solute gas first dissolves in the
membrane and then diffuses in the solid to the other gas phase. Examples of membrane
separations are helium being separated from natural gas and nitrogen from air. Separation of gas
mixture occurs because each type of molecule diffuses at a different rate through the membrane.
4. Reverse Osmosis: A membrane, which impedes the passage of a low molecular weight solute,
is placed between a solute- solvent solution and a pure solvent. The solvent diffuses into the
solution by osmosis. In reverse osmosis, a reverse pressure difference is imposed which cause
the flow of solvent to reverse, as in the desalination of seawater. This process is also used to
separate other low- molecular- weight solutes, such as salts, sugars, and simple acids from a
solvent (usually water).
Prof. Palve Sandip Balvant, K. K. Wagh College of Food Technology, Nashik.
Theory Notes of Unit Operations in Food Processing I (FE 237)
5. Ultra filtration membrane process: In this process, pressure is used to obtain a separation of
molecules by means of a semipermeable polymeric membrane (M2). The membrane
discriminates on the basis of molecular- weight solutes such as proteins, polymers, colloidal
materials such as minerals and so on. The osmotic pressure is always negligible because of the
high molecular weights.
6. Gel permeation chromatography: The porous gel retards diffusion of the high-molecular-
weight solutes. The driving force is concentration. This process is quite useful in analyzing
complex chemical solutions and in the purification of very specialized and/or valuable
components.
Important requirements for a membrane suitable for food processing purpose include:
(1) The membrane must be capable of giving the degree of separation required, at high
rates of flow and over extended periods of operation.
(2) Membranes must be capable of withstanding effective cleaning and disinfection to
the requirements necessary for satisfactory hygienic operation.
(3) Membranes should have a long ‘in-place’ life under the operating conditions
experienced.
Example: In dairy operations, for example, deposits of proteinaceous matter which tend to build
up on membrane surfaces can quickly lead to an unacceptable fall in permeation rates. For this
reason cleaning programmes assume major importance in the membrane separations other than
for the avoidance of microbiological contamination.
Membrane Flow: It should be realised that although ultra filtration and reverse osmosis are
frequently regarded as extensions of filtration to molecular size ranges, any analogy to flow
through conventional filter beds must be regarded with caution. This simple approach does not
adequately describe the flow across either UF or RO membranes.
(a) Capillary flow model: In this simple model, solute is rejected by filtering or sieving
action as a liquid flow through a micro porous structure which prevents the passage of
larger molecules. The model considers flow to occur through pores in an otherwise
impermeable layer. A laminar flow regime is established so the Hagan-Poiseuille
equation can be applied to determine the ‘flux’ (volumetric floe rate per unit area of
membrane surface) across the membrane.
(b) Solution-diffusion model: A second model for the transport of the material across a
membrane postulates the dissolution of the molecular species being transported, in the
material of the membrane, followed by molecular diffusion across the barrier. Since
both the solubility’s and rates of diffusion of the various molecular species present
will be different for different components, the solution-diffusion model appears to
explain in the selectivity of a reverse osmosis membrane to various components in
solution.
Structure of membranes: Asymmetric and ultra micro porous. They consist of an ultrathin skin
of dense polymer some 0.5-1.5 µm thick, supported on a relatively thick but micro porous
polymer structure. The laminate of dense film and porous support is made in a single casting
process and has a total thickness of 0.1-0.2mm.
Cellulose esters were the first polymers to be successfully employed in low pressure membrane
separation processes and they can be constructed with various porosities according to need.
Disadvantages:
a. Cellulose acetate is subject to hydrolysis in both acidic and mildly alkaline conditions.
Hydrolysis is the minimum in the pH 4.5-5.0.
b. They are unable to withstand elevated temperatures, upper limits being in the range 40-60
0
C according to the type of material.
c. Cellulose acetate membranes are also subject to microbial and enzymatic attack.
For ultrafiltration other materials can be used. These include polyvinyl chloride, polyacrylonitrile
and nylons. Some newer materials-aromatic polyamides and polyimide are able to withstand
elevated temperatures under corrosive conditions.
Advantages:
1. They have high resistance to collapse or consolidation under applied pressures,
resistance to change in properties at higher temperatures.
2. Possess good mechanical strengths and abrasion resistance and withstand acidic, alkaline
and oxidative conditions.
Only two materials have found extensive use in commercial reverse osmosis applications-
cellulose acetate and polyamide, a modified form of nylon.
Basic features: Though at first sight a variety of system appeared to find use in UF and RO
processes basically they are very similar. Dilute feed from storage vessel is fed under pump
pressure, via a manifold, to the appropriate number of membrane modules necessary to give a
surface area for separation at required rate. Permeate passing through the membrane is taken off.
In food processing application the desired stream is usually the enriched concentrate (retenate)
stream. ‘Once-through’ system as shown in fig (a) or ‘recirculating system’ as shown in fig (b)
may be used in the letter concentrate is recycled for further concentration. A heat exchanger is
often included in the system to permit any desired temperature control, e.g. to avoid temperature
at which microbial growth is rapid. For RO application high pressure pump are needed. This can
be positive displacement pumps or multistage centrifugal pumps.
In the operation of these units the aim is to achieve the desired degree of separation (‘rejection
‘of undesired components) at the required production level. Maximum flux rate at the working
pressure thus minimizing the area of membrane surface required are highly desirable.
Ultra-filtration is used in many different processes at the present time. Some of these are
separation of oil-water emulsion, concentration of latex particles, processing of blood and plasma,
fractionation or separation of proteins, recovery of whey proteins in cheese manufacturing,
removal of bacteria and other particles to sterilize wine, and clarification of fruit juices.
Membranes for Ultrafiltration are in general similar to those for reverse osmosis and are
commonly asymmetric and more porous. Membranes are made from aromatic polyamides,
cellulose acetate, cellulose nitrate, polycarbonate, polyimides, polysulfone, and so forth .
Prof. Palve Sandip Balvant, K. K. Wagh College of Food Technology, Nashik.
Theory Notes of Unit Operations in Food Processing I (FE 237)
The equipment for ultrafiltration is similar to that used for reverse osmosis and gas separation
processes. The tubular type unit is less prone to fouling and more easily cleaned than any of the
other three types; however, this type is relatively costly.
(a) Flat sheet membranes: These are used in assemblies similar in construction to
plate and frame filter presses, the membrane being stretched across a series of
perforated baffles supported on a grooved plate. The liquid flows at low velocity
(0.5m/s) through narrow channels (0.3-0.5 mm) and is only in contact with the
membrane for a distance of about 150 mm. This type of construction is being used
in the dairy field, e.g. whey concentration.
(b) Tubular membranes: Here the membrane is cast onto the inside of a porous
support tube and they are widely used. A complete module consists of the tubular
membrane carried inside other jacket (rather like a simple pipe heat exchanger).
The liquid being treated is pumped through the inner porous tube, in a number of
designs, at a velocity sufficiently high to promote turbulent flow.
(c) Spiral-wound flat sheet membranes: This is a variation of the flat sheet
membranes and is frequently used in a reverse osmosis where, as seen, higher
pressures are required. Two flat sheets of membrane sandwiching a porous support
medium are wrapped, with a plastic spacer, around a central tube. The tube
connects with porous material along one edge of the sandwich. The spiral-wound
roll is contained inside a cylindrical metal tube. Liquid, under pressure in the pipe,
flows into the space created by the plastic spacer and across the membrane
surfaces. Permeate, after passing the membrane, is removed from the system via
the porous support and the central tube.
(d) Hollow fibre membranes: One of the most widely used membrane systems in
reverse osmosis applications is that based on the use of hollow-fibre membranes of
an asymmetric polyamide marketed. The use of very narrow bore hollow fibres
(the bore is about 40µm and overall diameter 80µm) allows a very large membrane
surface to be packed into a small volume. The fibres are wrapped around a porous
feed tube so as to fill the annular space between this tube and outer cylinder.
Permeate (usually water) flows from the feed tube, through the outer wall of the
fibres, to leave via the hollow centre of the fibres which themselves connect to a
common outlet. Concentrate, containing the rejected dissolve solids, having failed
to pass the membrane flows to a common concentrate outlet.
Ultrafiltration units operate at about 5-100 psi pressure drop, compared to 400-2000 for reverse
osmosis. For low-pressure drops of 5-10 psi and dilute solutions of up to 1 wt %.
Types of membranes for reverse osmosis: One of the more important membranes for reverse-
osmosis desalination and many other reverse-osmosis process is the cellulose acetate membrane.
The asymmetric membrane is made as composite film in which a thin dense layer about 0.1 - 10
µm thick of extremely fine pores is supported upon a much thicker (50 – 125 µm) layer of
microporous sponge with little resistance to permeation. The thin dense layer has the ability to
block the passage of quite small solute molecules.
Limitation: It can only used in aqueous solutions and that it must be used below about 60 0C.
Another important membrane useful for seawater, wastewater, nickel-plating rinse solution and
other solutes is the synthetic aromatic polyamide membrane “Permasep” made in the form of
very fine hollow fibers. When used industrially this type membrane withstands continued
operation at pH value of 10 to 11.
When liquid flows through the tortuous micro pores in a membrane, energy is expended in
overcoming the resistance to flow. This energy loss manifests itself as a drop in pressure exactly
as in flow through pipelines. Pressure must be applied to the liquid on upstream side of the
membrane if flow is to occur. With smaller pore sizes (tighter membrane) higher applied
pressures will be required to maintain a particular flow rate. For a particular membrane,
increasing the applied pressure, at least initially, results in larger ‘flux’ value. In the case of
permeable membranes a second pressure component, not experienced in conventional filtration,
arises. This is osmotic pressure.
In reverse osmosis application of considerably higher pressure of some 5-7.5MN/m2 (50-75 atm)
are required to effect separations.
1. Basic models for membrane processes: There are two basic types of mass- transport
mechanisms which can take place in membranes. In the first basic type, using tight
membranes, which are capable of retaining solutes of about 10 A in size or less, diffusion –
type transport mainly occurs. Both the solute and the solvent migrate by molecular or
Fickian diffusion in the polymer, driven by concentration gradients set up in the membrane
by the applied pressure difference. In the the second basic type, using loose, microporous
membranes which retain particles larger than 10 A, a sieve-type mechanism occurs, where
the solvent moves through the micropores in essentially viscous flow and the solute
molecules small enough to pass through the pores are carried by convection with the solvent.
In many commercial units, operating pressures in reverse osmosis range from about 1035 up to
10350 kPa (150 up to 1500 psi). As the feed pressure is increased, solvent or water flow through
the membrane increases and the solute flow remains approximately constant, giving lower solute
concentration in the product solution.
At a constant applied pressure, increasing the feed solute concentration increases the product
solute concentration. This is caused by the increase in the feed osmotic pressure, since as more
solvent is extracted from the feed solution (as water recovery increases), the solute concentration
become higher and the water flux decreases. Also, the amount of solute present in the product
solution increases because of the higher feed concentration.
If a reverse-osmosis unit has a large membrane area (as in commercial unit), and the path
between the feed inlet and outlet is long, the outlet is long, the outlet feed concentration can be
considerably higher than the inlet feed c1 .then the salt flux will be greater at the outlet feed as
compared to the inlet. Many manufacturers use the feed solute or salt concentration average
between inlet and outlet to calculate the solute or salt rejection R in equation.
incurs greater energy costs and requires special pumps. Therefore, the main applications of RO
are for concentrating liquids, recovering solids and treatment of water.
1. Milk Processing: RO can be used for concentrating full cream milk up to a factor of 2–3
times. Flux rates for skimmed milk are only marginally higher than those for full cream
milk. The product concentration attainable is nowhere near as high as that for
evaporation, due to increasing osmotic pressure and fouling, due mainly to the increase in
calcium phosphate, which precipitates out in the pores of the membrane. Therefore, most
of the commercial applications have been for increasing the capacity of evaporation
plant. Other possible applications that have been investigated and discussed include: (a)
the concentration of milk on the farm for reducing transportation costs, (b) for yoghurt
production at a concentration factor of about 1.5, to avoid the addition of skimmed milk
powder, (c) for ice cream making, also to reduce the use of expensive skimmed milk
powder, (d) for cheese making to increase the capacity of the cheese vats and (e) for
recovering rinse water. Cheese whey can also be concentrated, to reduce transportation
costs or prior to drying.
2. Other Foods: Reverse osmosis has found application in the processing of fruit and
vegetable juices, sometimes in combination with ultrafiltration and microfiltration. The
osmotic pressure of juices is considerably higher than that of milk. It is advantageous to
minimise thermal reactions, such as browning, and to reduce loss of volatiles. From a
practical viewpoint, the flux rate and rejection of volatiles is important. RO modules can
cope with single strength clear or cloudy juices and also fruit pulp. RO can be used to
produce a final product, as in the case of tomato paste and fruit purees, or to partially
concentrate, prior to evaporation. RO is a well established process for concentrating
tomato juice from about 4.50 Brix, to 8–120 Brix. Other fruit juices which have been
successfully concentrated are apple, pear, peach and apricot. Where juices have been
clarified, osmotic pressure limits the extent of concentration and up to 250 Brix can be
achieved. Unclarified juices may be susceptible to fouling.
Usually the pressure drop used across the membranes varies from 1 psi to 50 psi. Types of
membranes are extremely varied and can be ceramics, polymers.
1. Dead end microfiltration flow model: In many laboratory batch filtrations, the batch
process is run in dead-end flow, with the membrane replacing the conventional filter
paper. The particles build up with time as a cake and the clarified permeate is forced
through the membrane, as shown in fig.(a).
2. Cross filtration microfiltration flow model: In the cross-flow model shown in fig.(b),
the operation is similar to that for reverse osmosis and ultrafiltration in that the flow of bulk
solution is parallel to the membrane surface and not through it. The permeate flow through
the membrane carries particles to the surface, where they form a thin layer. A relatively high
flow rate tangential to the surface sweeps the deposited particles towards the filter exit
leaving a relatively thin deposited cake layer. This thin cake layer is similar to the gel layer
formed in ultrafiltartion.
Ion Exchange:
General Principles
Ion exchange can be used for separations of many types of molecules, such as metal ions,
proteins, amino acids or sugars. The technology is utilised in many sensitive analytical
chromatography and laboratory separation procedures, frequently on a very small scale.
However, industrial-scale production operations, such as demineralization or protein recovery,
are possible. Ion exchange is the selective removal of a single, or group of, charged species from
one liquid phase followed by transfer to a second liquid phase by means of a solid ion exchange
material. This involves the process of adsorption – the transfer of specific solute(s) from a feed
solution on to a solid ion exchanger. The mechanism of adsorption is electrostatic involving
opposite charges on the solute(s) and the ion exchanger. After washing off the feed solution, the
solute (s) is desorbed back into solution in a much purified form.
Ion exchangers can be used to retain simple ionised species such as metal ions, but may also be
used in the separation of polyelectrolytes, such as proteins, which carry both positive and
negative charges, as long as the overall charge on the polyelectrolyte is opposite to the fixed
charges on the ion exchanger. This overall charge depends on the isoelectric point (IEP) of the
polyelectrolyte and the pH of the solution. At pH values lower than the IEP, the net overall
charge will be positive and vice versa.
To maintain electrical neutrality, these fixed ions must be balanced by an equal number of
mobile ions of the opposite charge, i.e. anions, held by electrostatic forces. These mobile ions
can move into and out of the porous molecular framework of the solid matrix and may be
exchanged stoichiometrically with other dissolved ions of the same charge and are termed
counterions. Therefore, if an anion exchanger, as shown in fig. is in equilibrium with a solution
of NaCl, the internal phase contains some Na+ ions, although the concentration is less than in the
external phase because the internal concentration of Cl– ions is much larger. When an ion
exchanger is contacted with an ionised solution, equilibration between the two phases rapidly
occurs.
In the adsorption stage, a negatively charged solute molecule (e.g. a protein, P–) is attracted to a
charged site on the ion exchanger (R+), displacing a counterion (X–):
R+ X– + P–→ R+ P–+ X–
In the desorption stage, the anion is displaced from the ion-exchanger by a competing salt ion (S–) and
hence is eluted:
R+ P–+ S–→ R+ S– + P–
Ion exchangers are further classified, in terms of how their charges vary with changes in pH, into
weak and strong exchangers. Strong ion exchangers are ionised over a wide range of pH and
have a constant capacity within the range, whereas weak exchangers are only ionised over a
limited pH range, e.g. weak cation exchangers may lose their charge below pH 6 and weak anion
exchangers above pH 9.
rate of counterions into and out of the matrix, the degree of swelling and the durability of the
material.
Ion exchange processes can be used to remove specific metals or anions from drinking
water and food fluids, which has potential application for detoxification or radioactive
decontamination. Procedures have been described for the retention of lead, barium,
radium, aluminium, uranium, arsenic and nitrates from drinking water.
2. Decolourisation: Sugar liquors from either cane or beet contain colourants such as
caramels, melanoidins, melanins or polyphenols combined with iron. Many of these are
formed during the earlier refining stages and it is necessary to remove them in the
production of a marketable white sugar. The use of ion exchangers just before the
crystallisation stage results in a significant improvement in product quality. It is
necessary to use materials with an open, porous structure to allow the large colourant
molecules access to the adsorption sites. Colour reduction of fermentation products such
as wine uses a strongly basic anion exchanger to remove colouring matter, followed by a
strong cation exchanger to restore the pH.
3. Protein Purification: High purity protein isolates can be produced in a single step from
dilute solutions containing other contaminating materials by ion exchange. The
amphoteric nature of protein molecules permits the use of either anion or cation
exchangers, depending on the pH of the environment. Elution takes place either by
altering the pH or increasing the ionic strength. The eluate can be a single bulk, or a
series of fractions produced by stepwise or linear gradients, although fractionation may
be too complex for large-scale industrial production. Separation of a single protein may
take place on the basis that it has a higher affinity to the charged sites on the ion
exchanger compared to other contaminating species, including other proteins present in
the feed. Typically whey contains 0.6–0.8% protein which is both highly nutritious and
displays excellent physical properties, yet the vast majority of this is wasted or under-
utilised. Anion exchange materials can produce high purity functional protein from
cheese whey, using a stirred tank reactor into which the whey is introduced at low pH.
Following rinsing of non adsorbed material, the protein fraction is eluted at high pH and
further purified by ultrafiltration, so that the final protein content is approximately 97%
(dry weight). The use of ion exchange to recover or separate the caseins in milk is not
carried out commercially, although it has been shown to be feasible. This system has also
been demonstrated for recovery of food proteins from waste streams resulting from the
processing of soya, fish, vegetables and gelatin production, plus abattoir waste streams.
Such protein fractions could be used as functional proteins in the food industry or for
animal feeds.