The document defines filtration and clarification processes. It describes the basic components and process of filtration using a filter press. Key points include:
- Filtration separates solids from liquids using a porous medium, while clarification is used for very low solid concentrations below 1.0% w/v.
- A filter press uses alternating plates and frames with a filter medium to separate solids. Slurry enters the frames under pressure and the filtrate exits through outlets on the plates.
- Factors like particle properties, liquid properties, temperature, pressure difference, and filter media properties influence the filtration rate according to equations like Poiseuille's, Darcy's, and Kozeny-Carman
2. Definition
Filtration: It may be define as a process of separation
of solids from a fluid by passing the same through a
porous medium that retains the solids but allows the
fluid to pass through.
Clarification: When solid are present in very low
concentration, i.e., not exceeding 1.0% w/v, the
process of its separation from liquid is called
clarification.
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3. Suspension to be filteredSlurry
Filter
medium
Filter
cake
Filtrate
Porous medium used to
retain solid
Accumulated solids on the
filter
Clear liquid passing through
the filter
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4. Process of filtration
Pores of filter medium are smaller than size of particles to be separate.
Filter medium (filter paper) is placed on a support (mesh)
Slurry is placed over the filter medium
So solids are trapped on the surface of the filter medium
Gravity is acting over the liquid medium
Due to pressure difference across the filter, fluid flows through the filter medium
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5. Applications of filtration
Production of sterile products:
HEPA filters or laminar air bench
Membrane filters.
Production of bulk drugs
Production of liquid dosage
Effluents and waste water treatment
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6. Mechanism of filtration
The mechanism whereby particles are retained by a filter is
significant only in initial stages of filtration.
Straining
Impingement
Entanglement
Attractive forces
• Similar to sieving, i.e., particles of larger size can’t
pass through smaller pore size of filter medium.
• Solids having the momentum move along the path of
streaming flow and strike (impinge) the filter medium. Thus
the solids are retained on the filter medium.
• Particles become entwined (entangled) in the masses of
fibres (of cloths with fine hairy surface or porous felt) due
to smaller size of particles than the pore size. Thus solids
are retained within filter medium.
• Solids are retained on the filter medium as a result of
attractive force between particles and filter medium, as in
case of electrostatic filtration.
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7. Surface filtration
The size of particles retained is
slightly higher than the mean pore
size of medium.
Mechanical strength of filter
medium is less, unless it is made
of stainless steel.
It has low capacity.
The size of particles retained is
more predictable.
Equipment is expensive
because
ancillary equipment such as edge
clamps is required.
Ex. Cellulose membrane filter.
Depth filtration
The size of particles retained is
much smaller than the mean pore
size of medium.
Mechanical strength of filter
medium is high.
It has high capacity.
The size of particles retained is
less predictable.
Equipment is cheaper because
ancillary equipment is not
required.
Ex. Ceramic filters and sintered
filters.
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8. Theories of filtration
The flow of liquid through a filter follows the basic rules that govern the
flow of any liquid through the medium offering resistance.
The rate of flow may be expressed as-
Rate = driving force / resistance
The rate of filtration may be expressed as volume (litres) per unit
time (dv/dt).
Driving force = pressure upstream – pressure downstream
Resistance is not constant.
It increases with an increase in the deposition of solids on the filter
medium.
Therefore filtration is not a steady state.
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9. The rate of flow will be greatest at the beginning of filtration process,
since the resistance is minimum.
After forming of filter cake, its surface acts as filter medium and solids
continuously deposit adding to thickness of the cake.
Powder or granule bed visualized as a bundle of capillaries
Upstream pressure, P1
Surface area
Downstream
pressure, P2
Viscosity
Flow rate:
m3 / unit time
Length (L)
Resistance to movement=
{pressure upstream- pressure downstream}/ length of capillaries
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10. Poiseullie’s Equation
Poiseullie considered that filtration is similar to the streamline
flow of liquid under pressure through capillaries.
Poiseullie’s Equation is-
Where, V = rate of flow, m3/s (l/s)
ΔP= Pressure difference across the filter, Pa
r = radius of capillary in the filter bed, m
L = thickness of filter cake (capillary length), m
𝝶 = viscosity of filtrate
If the cake is composed of bulky mass of particles and the liquid
flows through the interstice, then flow of liquids through these
may be expressed by this equation.
V =
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11. Darcy’s Equation
Poiseullie's law assumes that the capillaries found in the filter
are highly irregular and non-uniform.
Therefore, if the length of capillary is taken as the thickness of bed,
a correction factor for radius is applied so that the rate is closely
approximated and simplified.
The factors influencing the rate of filtration has been incorporated
into an equation by Darcy, which is:
Where, K = permeability coefficient of cake, m2
A = surface area of porous bed (filter medium), m2
Other terms are same as previous equation
K depends on characteristics of cake, such as porosity, specific
surface area and compressibility.
V =
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12. Permeability may be defined quantitatively as the flow rate of a
liquid of unit viscosity across a unit area of cake having unit
thickness under a pressure gradient of unity.
This equation is valid for liquids flowing through sand, glass
beds and various porous media.
This model is applied to filter beds or cakes and other types of
depth filter.
This equation is further modified by including characteristics of K
by Kozeny-Carman.
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Kozeny-Carman (K-C) equation
Kozeny-Carman equation is widely used for filtration.
V =
Where,
𝝴 = porosity of cake (bed)
S = specific surface area of particles comprising the cake m2 / m3
K = Kozeny constant (usually taken as 5)
Other terms are same as previous equations
Limitations:
It does not consider the fact that depth of granular bed is lesser
than the actual path traversed by the fluid.
The actual path is not same through out the bed, but it is sinuous
or tortuous.
14. Factors influencing filtration
Properties of solid
• Particle shape
• Particle size
• Particle charge
• Density
• Particle size
distribution
• Rigidity or
compressibility
of solid under
pressure
• Tendency of
particle to
flocculate or
adhere
together
• Density
• Viscosity
• corrosiveness
Properties of liquids
Properties of solid
in slurry
• Rate of
formation of
filter cake
especially in
early stage of
filtration
Objectives
• Whether the
solid or liquid
or both are to
be collected
Temperature
• Temperature
of suspension
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Surface area of filter medium
Rate of
filtration
Inversely proportional to specific surface of filter bed
(According to K-C equation)
Directly proportional to surface area of filter medium
(According to Darcy’s equation)
Rate can be increased either using large filter or connecting a number
of small units in parallel.
Filter press works on principle of connecting units in parallel.
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Pressure drop across the filter medium
According to K-C equation the rate of filtration is proportional to the
overall pressure drop across both the filter medium and filter cake.
The pressure drop can be achieved in a number of ways:
• A pressure difference could be obtained by maintaining a head of slurry above the filter
medium.
• The pressure developed will depend on the density of the slurry
Gravity
• The pressure below the filter medium may be reduced below atmospheric pressure by
connecting the filtrate receiver to a vacuum pump and creating a pressure difference
across the filter.
Vacuum
(Reducing pressure)
• The simplest method being to pump the slurry into the filter under pressure.
• The gravitational force could be replaced by centrifugal force in particle separation
Pressure
Centrifugal
force
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Filter Media
The surface upon which solids are deposited in a filter is called the
“Filter medium”
Properties of ideal filter medium:
It should-
1) be capable of delivering a clear filtrate at a suitable production rate.
2) have sufficient mechanical strength.
3) be inert.
4) retain the solids without plugging at the start of filtration.
5) Not absorb dissolve material.
6) Sterile filtration imposes a special requirement since the pore size
must not exceed the dimension of bacteria or spores.
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Material used as filter media
Woven material
• Made up of wool, silk, metal or synthetic fibres (rayon, nylon etc.).
• These include a- wire screening and b- fabrics of cotton, wool, nylon.
• Wire screening e.g. stainless steel is durable, resistance to plugging and easily
cleaned.
• Cotton is a common filter ,however, Nylon is superior for pharmaceutical use,
since it is unaffected by mould, fungus or bacteria and has negligible absorption
properties .
• The choice of fibre depends on chemical
Perforated sheet metal
• Stainless steel plates have pores which act as channels as in case of meta filters.
Bed of granular solid built up on supporting medium
• In some processes, a bed of graded solids may be formed to reduce resistance of flow.
• Ex. Of granular solids are gravel, sand, asbestos, paper pulp and keiselgur.
• Choice of solids depends on size of solids in process.
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Prefabricated porous solid units
• Used for its convenience and effectiveness.
• Sintered glass, sintered metal, earthenware and porous
plastics are used for fabrication.
Membrane filter media
• These are cartridge units and are economical and available in pore
size of 100 μm to even less than 0.2 μm.
• Can be either surface cartridges or depth type cartridges.
• Surface cartridges
• These are corrugated and resin treated papers and used in hydraulic
lines.
• Ceramic cartridges and porcelain filter candles are examples.
• Can be reuse after cleaning.
• Depth type cartridges:
• Made up of cotton, asbestos or cellulose.
• These are disposable items, since cleaning is not feasible.
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Filter Aids
The objective of filter aid is to prevent the medium from becoming blocked and
to form an open, porous cake, hence, reducing the resistance to flow of the
filtrate.
Filter aid forms a surface deposit which screens out the solids and also
prevents the plugging of supporting filter medium.
Characteristics of filter aids:
Chemically inert and free from impurities.
Low specific gravity, so remain suspended in liquids.
Porous rather than dense, so that pervious cake can be formed.
Recoverable.
Disadvantages:
Remove the coloured substances by absorbing them.
Sometimes active principles such as alkaloids are absorbed on filter aid.
Rarely, filters are source of contamination such as soluble iron salts, which
can provoke degradation of sensitive ingredient.
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Handling of filter aids
Filter aids may be used in either or both two ways:
1) Pre- coating technique: by forming a pre-coat over the filter medium by
filtering a suspension of the filter aid .
2) Body- mix technique: A small proportion of the filter aid (0.1- 0.5 %) is
added to the slurry to be filtered. This slurry is re-circulated through the filter
until a clear filtrate is obtained, filtration then proceeds to completion.
Different flow rates can be achieved depending on grade of aid-
1. Low flow rate: fine grade filter aids- mainly used for clarity
2. Fast flow rate: coarse grade filter aids- acceptable filtrate.
Examples of filter aids
Diatomite (Keiselgur) , obtained from natural siliceous deposits.
Perlite , it is an aluminium silicate. Cellulose, Asbestos, charcoal, talc,
bentonite , fullers earth etc.
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Based on operation of filtration
Discharge and filtrate
are separated steadily
and uninterrupted
Discharge of filtered solid is
intermittent.
Filtrate is removed continuously.
Operation should be stopped to
collect solid.
Continuous filtration
Discontinuous
filtration
Filters
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Based on nature of filtration
Feed of suspension
flows under
pressure at fairly
high velocity across
the filter medium
Remove small
amounts of solids
Remove large
amount of solid
Cross- flow filtersClarifying filtersCake filters
Filters
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Plate and frame filter press
Principle:
Mechanism is surface filtration.
The slurry enters the frame by pressure and flows through filter
medium.
The filtrate is collected on the plates and send to outlet.
A number of frames and plates are used so that surface area
increases and consequently large volumes of slurry can be processed
simultaneously with or without washing.
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Construction
The Filter press is made of two types of units, plate and frames.
Usually made of aluminium alloy.
Sometimes, these are also lacquered for protection against
corrosive chemicals and made suitable for steam sterilization.
Frame
It contains a open space inside wherein the slurry reservoir is
maintained for filtration and an inlet to receive the slurry.
It is indicated by two dots in description.
Slurry inlet
Handle to rest on rod
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Frames of different thickness are available.
It is selected based on the thickness of cake formed during filtration.
Optimum thickness of frame should be chosen.
Plate
The plate has a studded or grooved surface to support the filter cloth
and an outlet.
It is indicated by one dot in description.
Through channel
Filtrate outlet
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Plate supports the filter medium, receiving the filtrate and outlet.
The filter medium usually cloth is interposed between plate and frame.
Plate, filter medium, frame, filter medium and plate are arranged in
sequence and clamed to a supporting structure.
It is normally described by dots as 1.2.1.2.1 so on.
A number of plates and frames are employed so that the filtration area
is as large as necessary.
Number of filtration units are operated in parallel.
Channels for slurry inlet and filtrate outlet can be arranged by fitting
eyes to the plates and frames, these join together to form a channel.
In some types only one inlet channel is formed, while each plate is
having individual outlets controlled by valves.
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Working
Working can be divided into two steps-
1. Filtration operation
2. Washing of cake (if desirable)
Filtration operation
Frame- marked by 2 dots
Plate – marked by 1 dot
Plate and frame filter press, principle of filtration operation
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Slurry enters the frame from the feed channel and passes through the filter medium on the
surface of the plate
The solid forms a filter cake and remain in the frame
As filtration proceeds, the resistance of the cake increases and filtration rate decrease
The filtrate drains between the projections of the surface of the plate and escape from the
outlet
Thus two filter cakes are formed , which meet eventually in the centre of the frame
The thickness of the cake is half of the frame thickness, because on each side of frame
filtration occurs
At a certain point process is stopped and press is emptied and cycle is
restarted
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Washing operation
When washing of cake is also required modified plate and frame
filter is used.
For this purpose an additional channel is included called as washing
plate and are identified by 3 dots.
In the half of the washing plate, there is a connection from wash water
cannel to the surface of plate.
The sequence of arrangement of plates and frames can be
represented by dots as 1.2.3.2.1.2.3.2.1 so on (between 1 and
1, 2.3.2 must be arranged.
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Procedure for washing the press
Step-1
Step-3
Step-2
Step-4
Step-5
• Filtration proceeds in the ordinary way until the frames are filled with cake.
• To wash the filter cake, the outlets of washing plates are closed.
• Wash water is pumped in the washing channel.
• The water enters through the inlets on the surface of washing plate.
• Water passes through the filter cloth and enters frame which contains the cake.
• Then water washes the cake, passes through the filter cloth and enters the plate down
the surface.
• Finally washed water escapes through the outlet of that plate.
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Uses:
Filtration of viscous liquid can also be done by incorporating
heating/cooling coils in the press
Advantages
Construction of filter press is very simple and a variety of
materials can be used.
I. Cast iron – for handling common substances.
II. Bronze - for smaller units.
III. Stainless steel – contamination can be avoided.
IV. Hard rubber and plastic- used where metals must be avoided.
V. Wood- for lightness though it must be kept wet.
Provide large filtration area in relatively small floor space. The capacity
being variable according to thickness of frames and number used.
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Sturdy construction permits the use of considerable
pressure
difference. (2000 Kilopascals normally used)
Efficient washing of cake is possible.
Operation and maintenance is easy.
It produce dry cake in form of slab.
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Disadvantages
It is a batch filter, so it is a time consuming.
The filter press is an expensive filter, the emptying time, the labour
involved, and the wear and tear on the cloths resulting in
high costs.
Operation is critical, as the frames should be full, otherwise washing is
inefficient and the cake is difficult to remove.
The filter press is used for slurries containing less about 5 % solids
In view of the high labour costs , it is most suitable for expensive
materials e.g. the removal of precipitated proteins from insulin liquors.
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Metafilter
Principle:
Mechanism is surface filtration.
In this, metal rings contain semicircular projections, which are arranged
as a nest to form channels on the edges.
This channel offers resistance (strainer) to the flow of solids (coarse
particles).
The clear liquid is collected into receiver from the top.
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Construction
Metafilter consists of a series of metal rings.
These are threaded so that a channel is formed on the edges.
It contains a grooved drainage column on which a series of metal
rings are packed.
These rings are usually made up of stainless steel and have
dimensions of about 15.0 mm internal diameter and 22.0 mm external
diameter.
Each metal ring has a number of semicircular projections (0.8 mm in
thickness) on one side of surface.
The projections are arranged as a nest to form channels on the
edges.
These rings are tightened on the drainage column with a nut.
Metafilters are also known as edge filters.
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Working
Filters are
placed in a
vessel
Slurry is pumped
under pressure or
occasionally by
Applying reduced
pressure to the
outlet side
Slurry passes
through the
channels
formed on
the edges
between the
rings
The clear liquid
rises up and
collected from
the outlet into
receiver
For separation of fine particles, a bed of suitable materials
such kieselguhr is first built up.
The pack of rings serves essentially as a base on which the
true filter medium is supported.
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Uses
Metafilters can be used for-
Clarification of syrups
Filtration of injection solutions
Clarification of insulin liquors
Filtration of viscous liquids can be achieved by applying
pressure.
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Advantages
Can be used under high pressures, without any danger of bursting the
filter medium.
Running cost are low, as separate filter medium is not used.
Can be constructed from a material that can provide excellent
resistance to corrosion and avoid contamination of sensitive
products.
It is extremely versatile filter because fine as well as large both type of
particles can be separated.
Removal of cake can be carried out by simply back- flushing with
water.
Change over from one batch to another or one product to another is
easy.
Sterile products can be handled.
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The candle filter
• Construction:
These are ceramic filters and are
made of porcelain or Kieselguhr. Kiesel-
guhr filters are usually softer than the
porcelain variety. These are cylindrical
candles with an opening which is
connected to vacuum pump for reducing
the pressure under it, during the
filtration process. The candles are
available in a range of different pore size
which is designed by a number.
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• Working:
The candle is placed in the solution to be filtered. When
vacuum is applied, the liquid will pass through the thick wall of the
candle and gets collected inside the candle from where it is
removed.
• The filter candle gets blocked with continuous use. This can be
cleaned by scratching the external surface with a nail brush and
passing water through it in the reverse direction.
• Uses:
These candles are used for sterilization of solutions.
It has the tendency to absorb materials from aqueous solutions.
Therefore, it is not used commonly.
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Sintered filters
• Construction: These are made of borosilicate glass.
Borosilicate glass is finely powdered, sieved and particle of desired
size are separated. It is then packed into a disc mould and heated to
a temperature at which adhesion takes place between the particles.
The disc is then fused to a funnel of suitable shape and size.
• Working: The sintered glass filters are available in
different pore size. Hence the funnel with a sintered filter is
numbered according to the pore size. The filtration is carried
out under reduced pressure. These funnel are used for
bacterial filtration.
• Uses: Sintered filters are also available in stainless steel
which has a greater mechanical strength. However these are
very much liable to attack by the solutions passing through
them.