Filtration Report.
Filtration Report.
Filtration Report.
OBJECTIVE:
• To study the theory of filtration
• To determine the average cake resistance for the given slurry and the resistance of the
filter medium used in the filtration process.
• To determine the time for filtration and hence the performance of the equipment based on
the volume of the filtrate collected.
THEORETICAL STUDY:
INTRODUCTION:
The separation of particles is done on the basis of the state of the particles to be
separated. There are a group of separation techniques where the separation is accomplished by
the differences in the mechanical- physical forces in the system and not the molecular/ chemical
forces. These mechanical- physical forces act on the particles, liquids, or the mixtures of
particles and the liquids and not necessarily on the individual molecules.
Filtration is the removal of solid particles from a fluid by passing the fluid through a
filtering medium, or septum, on which the solids are deposited. Filtration is the most common
application of the flow of fluids through packed beds. It is analogous to the filtration carried out
using a filter paper on a funnel or using a Buckner funnel in a laboratory. The objective is to
separate the solid from the fluid in which it is present. The separation is carried out by forcing
the fluid through the porous membrane. The solid particles are trapped within the pores of the
membrane and a build up as a layer is seen on the surface of the membrane.
Industrial filtrations range from simple straining to highly complex separations. The fluid
may be a liquid or a gas; the valuable stream from the filter may be the fluid, or the solids or
both. Sometimes it is neither, as when waste solids may be separated from the waste liquid prior
to disposal. In industrial filtrations, the solid content ranges from a trace to a very high
percentage. Often the feed is subjected to a pretreatment process to increase the filtration rate,
as by heating recrystallizing, or by adding filter aids.
1
CLASSIFICATIONS:
Industrial Filters:
The classification of different equipments according to the different driving forces
are listed below
• Pressure filters
Plate and frame filter press
Leaf filter
Sparkler filter
Candle filter
Line, Cartridge filter
• Vacuum filters
Nutsche filter
Rotary Drum filters
• Centrifugal filters
Top driven centrifuge
Bottom driven centrifuge
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Mechanisms of filtration:
• Cake filters separate relatively large amounts of solids as a cake or crystals or sludge.
Often they include provisions for washing the cake and removing some of the liquids
form the solids before discharge.
• Clarifying filters remove small amounts of solids to produce a clean gas or sparkling
clear liquids, like beverages. The solid particles are trapped in the filter medium as
shown. Clarifying filters differ from screens in that the pores in the filter medium are
much larger in diameter than the particles to be removed.
• In a Cross-flow filter the feed suspension flows under pressure at a very high velocity
across the filter medium. A thin layer of solids may form on the surface of the medium
but the high liquid velocity keeps the layer from building up. The filter medium may be
ceramic, metal or a polymer membrane with pores small enough to exclude most of the
suspended particles. Some liquid passes as a clear filtrate and leaves behind a suspension
of solids.
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CAKE FILTRATION:
In cake filtration, the filter cloth often acts as no more than a substrate
for building up the first thin layers of the filter cake, which itself then acts a filter to trap more
and more particles of smaller and smaller size. The first particles form bridges over the pores of
the medium. After this, smaller particles pass through the filter cloth, leading to a turbid liquid
(filtrate). As soon as the first layer of the particles has accumulated on the filter medium, this
cake will then act as the actual filter medium. The first solid particles enter the pores of the
medium and are immobilized, but soon others begin to collect on the septum surface. After the
brief initial period, a cake of apparent thickness builds up on the surface and must be
periodically removed. Naturally, the pressure drop through the filter cake increases and flow
decreases as the filter cake gets thicker. If the slurry contains too many fines, all pores of the
cloth may become blocked.
DERIVATION:
For laminar flow, in a packed bed of particles, the Carman-Kozeny relation has been
shown to apply to filtration. It is given by,
…1
4
where, ∆pc -> Pressure drop across the cake in N/m2 (lbf/ft2)
ν -> Open tube velocity in m/s (ft/s)
D -> Diameter in m (ft)
L -> Length in m (ft)
µ -> Viscosity in Pa.s or kg/m.s (lbm/ft.s)
k1 -> constant = 4.17 for random particles of definite size and shape
ε -> Void fraction or porosity of cake
S0 -> Specific surface area of particle in m2 per volume of solid particle
The linear velocity depends on cross sectional are according to the relation,
…2
…3
5
where, α -> Specific cake resistance in m/kg (ft/lbm), given by
where,
The volume of the filtrate V can be related to W, the kg of accumulated dry cake solids, as
Specific cake resistance is a function of void fraction ε and S0. It is also a function of pressure as
pressure can affect ε. By conducting various experiments at various pressure drops, the variation
of α with ∆p can be calculated.
If α is independent of -∆p, then the sludge is incompressible. Usually, α increases with –∆p,
since most cakes are somewhat compressible.
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An empirical equation is often used as,
where αo and s are empirical constants. The compressibility constant s is zero, for incompressible
cakes. Usually, it varies between 0.1 and 0.8 .
For constant pressure, constant α, and incompressible cake, V and t are the only variables.
Integrating to obtain the time of filtration in t s,
Dividing by V,
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Constant Rate Conditions:
These conditions are attained if the slurry is fed to the filter by a positive
displacement pump. Here, the flow rate of the slurry through the filter medium is kept a
constant.
where,
where Kv is in N/m5 ,
C is in N/m2.
Assuming that the cake is incompressible, Kv and C are constants characteristic of the
slurry, cake, rate of the filtrate collected.
A plot of pressure –∆p Vs V, the total volume of the filtrate collected, gives a straight line for a
constant rate dV/dt. The slope of the line is Kv and the intercept is C.
The pressure increases as the cake thickness increases and as the volume of the filtrate collected
increases.
The equations can also be rearranged in terms of –∆p and time ‘t’ as variables. At any moment
during the filtration, the total volume V is related to the rate and total time t as,
For a case when the specific cake resistance is not a constant, but varies as
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CENTRIFUGAL SEPARATION PROCESS:
Sometimes gravity settling may be too slow because of the closeness of the densities of
the particles and the fluid, or because of forces holding the particles together as in the case of
emulsions. In such cases, centrifugal separation is employed.
Here, a cylindrical bowl is shown rotating with a slurry feed of solid particles and liquid being
admitted at the centre. The feed enters and is immediately thrown outward to the walls of the
container, as in section (b). The liquid and solids are now acted upon by the vertical gravitational
force and the horizontal centrifugal force. The centrifugal force is usually so large that the force
of gravity may be neglected. The liquid layer then assumes the equilibrium position with the
surface almost vertical. The particles settle horizontally outward and press against the vertical
bowl wall.
In section (c) two liquids having different densities are being separated by the centrifuge. The
more dense fluid will occupy the outer periphery, since the centrifugal force is greater on the
more dense fluid.
9
Equations for Centrifugal forces:
In circular motion, the acceleration from the centrifugal force is
and
Substituting
Hence, the force developed is r ω2/g times gravity force. This is expressed as equivalent to so
many g forces.
10
Equations for rates of settling in centrifuges:
General equation for settling:
If a centrifuge is used for sedimentation (removal of particles by settling), a particle of a
given size can be removed from the liquid in the bow if sufficient residence time of the particle
in the bowl is available for the particle to reach the wall. For a particle moving radially at its
terminal setting velocity, the diameter of the smallest particle removed can be calculated.
At the end of the residence time of the particle in fluid, the particle is at a distance rb m from the
axis of rotation. If rb < r2, then the particle leaves the bowl with the fluid. If rb = r2 , it is deposited
on the wall of the bowl and effectively removed from the liquid.
For settling in the stokes’ law range, the terminal settling velocity at a radius r is obtained by,
If hindered settling occurs, the RHS of the above equation is multiplied by the factor (ε2Ψp).
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Since,
The residence time tr is equat to the volume of liquid V m3 in th bowl divided by the feed
volumetric flow rate q in m3/s. The volume V is given by,
Particles having diameters smaller than that calculated, will not reach the wall of the bowl and
will go out with the exit liquid. Larger particles will reach the wall and be removed from the
liquid.
The critical diameter Dpc is be
defined as the diameter of a
particle that reaches ½ the
distance between r1 and r2. This
particle moves a distance of half
the liquid layer or (r2-r1)/2 during
the time this particle is in the
centrifuge.
The integration is then between r =
(r1+r2)/2 at t = 0 and r = r2 at t = tr.
Then we obtain,
At this flow rate qc, particles with a diagram greater than Dpc will predominantly settle to the
wall and most smaller particles will remain in the liquid.
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Sigma values and scale-up of centrifuges:
Σ is physical characteristic of the centrifuge and not of the fluid- particle syste, being separated.
For a special case of settling of a thin layer,
The value of Σ is really the area in m2 of a gravitational settler that will have the same
sedimentation characteristics as the centrifuge for the same feed rate. To scale up from a
laboratory test of q1 and Σ1 to q2 ( for νi 1 = νi 2 ),
This scale-up procedure is dependable for similar type and geometry centrifuges and if the
centrifugal forces are within a factor of 2 from each other. If different configurations are used,
efficiency factors E should be used where q1/Σ1E1 = q2Σ2E2 . These efficiencies are determined
experimentally and values for different types of centrifuges are available.
The theory of constant pressure filtration can be modified and used where the centrifugal force
causes the flow instead of the impressed pressure difference. The equation will be derived for the
case where a cake has already been deposited. The inside radius of the basket is r2, ri is the inner
radius of the face of the cake, and r1 is the inner radius of the liquid surface. We will assume that
the cake is nearly incompressible so that an average value of α can be used for the cake. Also the
flow is laminar. If we assume a thin cake in a large-diameter centrifuge, then the area A for flow
is approximately constant. The velocity of the liquid is,
13
where q is the filtrate flow rate in m3/s and v is the velocity.
For the case where the flow area A varies considerably with the radius, the following has been
derived
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FILTER MEDIUM:
It is defined as a material that is permeable to one or more components of a
mixture, solution or suspension, and is impermeable to remaining components. Its principal role
is to cause a clear separation of particulates from the fluid with minimum consumption of
energy.
3. Metal sheets
Perforated
Woven wire
5. Plastic sheets
Woven monofilaments
Fibrillated film
Porous sheets
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6. Membranes
Polymeric
Ceramic
Metal
7. Cartridges
Sheet fabrications
Bonded beds
Yarn wound
FILTER AIDS:
Filter aids should have low bulk density to minimize settling and aid
good distribution on the filter-medium surface.
They should be porous and capable of forming a porous cake
to minimize flow resistance.
They must be chemically inert to the filtrate.
Examples:
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LAB – SCALE EXPERIMENT: (CONSTANT PRESSURE PROCESS)
OBJECTIVE:
• To determine the average cake resistance for the given slurry and the resistance of the
filter medium used in the constant pressure filtration process.
• To determine the rating of the equipment, given the volume of the filtrate to be collected.
APPARATUS REQUIRED:
Sample to be filtered, pressure filtration set- up – Buchner funnel, filter medium of appropriate
pore size, purified water for cleaning purposes
THEORY:
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From the derivation of the Pressure drop through the filter cake,
This equation is in the form of a straight line, y = mx + c, where Kp is the slope of the straight
line and B is the intercept of the line in the y - axis.
A plot of t/V vs V thus, gives a straight line, from which the values of Kp and B can be
calculated. Substitution of these values in the above expressions gives the values of α and Rm.
ASSUMPTIONS MADE:
• There is negligible solid motion, that is, the solid phase velocity is considered zero.
• There is a constant and time invariant wet to dry cake mass ratio in the slurry, that is, the
concentration of the solids in the slurry is a constant.
• Absolute vacuum conditions are assumed through the entire filtration process
• Rm is a constant throughout the filtration process
• The properties of the newly formed cake layer (concentration and specific resistance) are
similar to the average filter cake properties.
EXPERIMENTAL PROCEDURE:
1) Settling Test:
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2) Cake Permeability Test:
• Filter the slurry sample through a Buchner funnel with vacuum to obtain a filter cake
about 2" thick.
• Measure the rate at which the clear ML is filtered through the cake.
• If the liquors filter at a rate of 1 gpm/ft2 of filter area or greater, then it is a good
candidate for centrifugation or other large-scale filtration. If the liquor filtration rate
is less than 0.5 gpm/ft2, it means that the slurry contains too many fines, or that the
product is amorphous (noncrystalline) in nature and too easily compressed to allow
liquid to drain through. Again, a change in crystallization conditions may be required.
• Determine the solid concentration in the slurry sample before carrying the filtration
tests.
• Pour the sample into the funnel and apply vacuum to the container
• Measure the volume of filtrate collected at various time intervals. The intervals may
be increased progressively to compensate for the drop in the filtrate flow rate.
• Remove the cake from the filter and dry it and weigh it. This can also be used for the
calculation of the concentration of the dry solids in the sample.
• The plot of time and filtrate data gives the desired parameters characteristic of the
slurry.
PRECAUTIONS:
The cake should not crack at any point. The filtration should be stopped if a crack is
observed in the filter cake.
Do not allow the cake to completely drain before adding more slurry.
The slurry should be kept as homogeneous as possible during the test.
The initial tests should be performed to check the amount of fines in the slurry.
The concentration of the solids in the slurry should be calculated initially before the
experiment.
The rate at which the slurry is added into the funnel should not be altered too much so
a smooth graph can be obtained.
If the filtration pressure is increased too quickly, the filtration rate will increase too
fast. This should be avoided.
The selection of the filter medium should be done with the knowledge of the
suspension characteristics of the slurry.
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GRAPHS AND CALCULATIONS:
COMPOUND 2
COMPOUND-2
0.540
0.510
0.480
0.450
0.420
0.390
0.360
0.330
0.300
t/V
0.270
0.240
0.210
0.180
0.150
0.120
0.090
0.060
0.030
0.000
50 100 150 200 250 300 350 400 450 500 550 600 650 700 750 775
Volum e
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where
µ -> Viscosity in Pa.s or kg/m.s = 1 centi Poise = 1 * 10-3 Pa.sec
A -> filter area in m2 = ( 3.14) r2 = 0. 0095 m2
∆pc -> Pressure drop across the cake in N/m2 = 95.99 kPa
Cs -> kg solids /m3 of filtrate
Cs = 7.86 % w / w
Assume 100 kg of slurry
7.86 kg of solid corresponds to 100 kg of slurry
7.86 kg of solid corresponds to 92.14 kg of ML
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COMPOUND 4
Total time 111 secs
TIME t (sec) VOLUME V (Ml) t/V
7 100 0.070
10 200 0.050
14 250 0.056
19 300 0.063
22 400 0.055
26 450 0.058
28 500 0.056
34 550 0.062
36 600 0.060
46 700 0.066
55 800 0.069
70 850 0.082
COMPOUND-4
0.090
0.080
0.070
0.060
0.050
t/V
0.040
0.030
0.020
0.010
0.000
100 250 400 Volume 500 600 800
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where
µ -> Viscosity in Pa.s or kg/m.s = 1 centi Poise = 10-3 Pa.sec
A -> filter area in m2 = ( 3.14) r2 = 0. 0095 m2
∆pc -> Pressure drop across the cake in N/m2 = 95.99 kPa
Cs -> kg solids /m3 of filtrate
Cs = 10 % w / w
Assume 100 kg of slurry
10 kg of solid corresponds to 100 kg of slurry
10 kg of solid corresponds to 90 kg of ML
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COMPUOND 5
COMPOUND -5
0.120
0.100
0.080
t/V
0.060
0.040
0.020
0.000
100 200 350 450 V 550 650 750
Kp = 2.074 * 10 -4 B = 0.040
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where
µ -> Viscosity in Pa.s or kg/m.s = 0.6 centi Poise = .6 * 10-3 Pa.sec
A -> filter area in m2 = ( 3.14) r2 = 0.0095 m2
∆pc -> Pressure drop across the cake in N/m2 = 95.99k Pa
Cs -> kg solids /m3 of filtrate
Cs = 11.60 % w / w
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COMPOUND 6
VOLUME V
TIME t (sec) (Ml) t/V
7 100 0.070
10 250 0.040
13 300 0.043
17 400 0.043
20 450 0.044
24 500 0.048
27 550 0.049
31 600 0.052
35 650 0.054
41 700 0.059
46 750 0.061
51 800 0.064
61 850 0.072
70 900 0.078
80 950 0.084
103 1000 0.103
COMPOUND-6
0.110
0.100
0.090
0.080
0.070
0.060
t/V
0.050
0.040
0.030
0.020
0.010
0.000
100 250 300 400 450 500 550 600 650 700 750 800 850 900 950 1000
V
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where
µ -> Viscosity in Pa.s or kg/m.s = 0.37 cPoise = 0.37 * 10-3 Pa.sec
A -> filter area in m2 = ( 3.14) r2 = 0. 0095 m2
∆pc -> Pressure drop across the cake in N/m2 = 95.99 kPa
Cs -> kg solids /m3 of filtrate
Cs = 9.25 % w / w
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COMPOUND 7 [2 FILTER
CLOTHS]
VOLUME V
TIME t (sec) (Ml) t/V
10 100 0.100
14 200 0.070
18 250 0.072
25 300 0.083
34 350 0.097
80 600 0.133
86 650 0.132
90 700 0.129
108 750 0.144
117 800 0.146
150 825 0.182
COMPOUND-7
0.200
0.180
0.160
0.140
0.120
t /V
0.100
0.080
0.060
0.040
0.020
0.000
100 200 250 300 350 600 650 700 750 800 825
V
Kp = 3.5 * 10 -4 B = 0.03
where
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µ -> Viscosity in Pa.s or kg/m.s = 1 centi Poise = 1 * 10-3 Pa.sec
A -> filter area in m2 = ( 3.14) r2 = 0. 0095 m2
∆pc -> Pressure drop across the cake in N/ m2 = 95.99 kPa
Cs -> kg solids /m3 of filtrate
Cs = 1.55 % w / w
α = 49.35 m/kg
Rm = 4.559 * 104 m-1
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COMPOUND 8 [2 FILTER
CLOTHS]
VOLUME V
TIME t (sec) (Ml) t/V
13 100 0.130
20 150 0.133
24 200 0.120
31 250 0.124
40 300 0.133
52 350 0.149
62 400 0.155
68 450 0.151
75 500 0.150
88 550 0.160
95 600 0.158
110 650 0.169
118 675 0.175
125 700 0.179
150 750 0.200
COMPOUND-8
0.220
0.200
0.180
0.160
0.140
0.120
t/V
0.100
0.080
0.060
0.040
0.020
0.000
100 200 300 400 V 500 600 675 750
Kp = 2.16 * 10 -4 B = 0.105
30
where
µ -> Viscosity in Pa.s or kg/m.s = 1 centi Poise = 1 * 10-3 Pa.sec
A -> filter area in m2 = ( 3.14) r2 = 0. 0095 m2
∆pc -> Pressure drop across the cake in N/ m2 = 95.99 kPa
Cs -> kg solids /m3 of filtrate
Cs = 11.21 % w / w
Cs = 240 kg / 3.68 m3 of ML
= 113.636 kg/ m3 of ML
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COMPOUND 9 [2 FILTER
CLOTHS]
VOLUME V
TIME t (sec) (Ml) t/V
9 100 0.090
12 150 0.080
16 200 0.080
22 250 0.088
27 300 0.090
31 350 0.089
36 400 0.090
40 450 0.089
47 500 0.094
52 550 0.095
59 600 0.098
68 650 0.105
79 700 0.113
87 750 0.116
93 775 0.120
97 800 0.121
105 825 0.127
113 850 0.133
122 875 0.139
146 900 0.162
COMPOUND-9
0.180
0.160
0.140
0.120
0.100
t/V
0.080
0.060
0.040
0.020
0.000
100 200 300 400 500 600 700 775 825 875
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From the graph,
Kp = 2.84 * 10 -4 B = 0.0090
where
µ -> Viscosity in Pa.s or kg/m.s = 0.6 centi Poise = 0.6 * 10-3 Pa.sec
A -> filter area in m2 = ( 3.14) r2 = 0. 0095 m2
∆pc -> Pressure drop across the cake in N/ m2 = 95.99 kPa
Cs -> kg solids /m3 of filtrate
Cs = 6.35 % w / w
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CONCLUSIONS:
o Filtration was studied theoretically and on a lab scale.
o Using the available equipment (Buchner funnel set- up), the resistance of the filter medium
and the specific cake resistance of different cakes were calculated.
o It was observed that as the cake thickness increases, the pressure difference across the cake
also increases. Thus, the resistance to the fluid flow by the cake also increases.
o A graph was plotted between t/V Vs Volume of the filtrate collected over the filter medium.
The slope and the intercept of this graph gave values characteristic of the slurry.
o The conclusions of the experiments conducted are applicable to Pressure filtration
equipments such as Sparkler, Line, Candle, Cartridge filters and Vacuum filters such as
Nutsche filters and ANFDs.
o Scaling up of a centrifuge requires Pilot plant centrifuge devices for conducting lab- scale
experiments. It requires the application of other equations determined by scale up factors
after the calculation of the specific cake resistance and resistance of the filter medium.
• Theoretically, specific cake resistance values must lie in the range of 109 to 1012 and the
resistance of the medium should lie in the range of 104
• The DEVIATIONS in the values calculated from the graphs might be because
The Pressure assumed in the experimental conditions might not have been
absolute vacuum.
The concentration of the sample was assumed to be the same as the batch
concentration. This might not have been correct.
The graphical calculation of the slope and the intercept of the graph plotted
might not have been precise.
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ACKNOWLEDGEMENTS
I thank the H.R. Department for their timely assistance. I thank Mr.Jacob Jayakumar for his
help with the transportation, without which things wouldn’t have been so easy. I also thank
Mr.Jai Ganesh for the assistance at the canteen.
Lastly, I thank Orchid Chemicals & Pharmaceuticals for this wonderful opportunity provided
to young, aspiring students to increase their aptitude and enrich their knowledge by working in
the company for a brief period of time and providing them with the required exposure to be
successful individuals.
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