FILTRATION

 Removal of solid particles from a fluid by passing the fluid through a filtering
medium, or septum.

MECHANSIMS OF FILTRATION

(a) Clarifiers

* Also known as “deep-bed filters”.

* The particles of solid are trapped inside the filter medium.
* A typical cartridge filter:

(b) Cake filters

* The filter medium is relatively thin, compared with that of a clarifying filter.
* After the initial period, the cake of solids does the filtration, not the septum.
* A visible cake of appreciable thickness builds up on the surface and must be
periodically removed.
EQUIPMENT FOR CONVENTIONAL FILTRATION

(1) Plate and Frame Filter Press:

* The most common type, but less common for bioseparations.

* Used where a relatively dry cake discharge is desired.
* Cake removal: open the whole assembly
 Should not be used where there are toxic fumes or biohazards.

(2) Horizontal Plate Filter:

* Filtration occurs from the top of each plate.

* Cake removal: removed with a sluicing nozzle or discharged by rapidly
rotating the leaves.

(3) Vertical Leaf Filter and Candle Type Vertical Tank Filter:
 * Have a relatively high filtration area per volume.
 Require only a small floor area.
* Filter cake is formed on the external surface of the tubes.
* The tubes are cleaned by backwashing.

(4) Rotary Vacuum Filter:

* Rotate at a low speed during the operation.

* Pressure inside the drum is a partial vacuum.
 Liquid is sucked through the filter cloth and solids are retained on the
surface of the drum.
* Three chief steps of the filtration cycle:
(1) Cake formation
(2) Cake washing to remove either valuable or unwanted solutes
(3) Cake discharge
* Being automated.
 Have a lower labor cost.
* The workhorse of bioseparations.
* Common for large-scale operations whenever the solids are difficult to filter.
PRETREATMENT OF FILTRATION

“Filtration is a straightforward procedure for well-defined crystals.”

* Fermentation beers and other biological solutions are notoriously hard to filter,
because of: (1) high, non-newtonian viscosity, and (2) highly compressible filter
cakes.

 Conventional filtration is often too slow to be practical.

 The filtration requires pretreatment: heating, coagulation and

flocculation, or adsorption on filter aid.

A. Heating

* To improve the feed’s handling characteristics. (Thinking of filtering a dilution

solution of egg white.)

* The simplest pretreatment (and the least expensive).

* Chief constraint: thermal stability of the product.

B. Coagulation and Flocculation

* Through the addition of electrolytes.

* Types of coagulants:
(1) Simple electrolytes (such as ferric chloride, alum, or acids and bases)
(2) Synthetic polyelectrolytes

* Action of simple electrolytes: reduce the electrostatic repulsion existing between

colloidal particles.

* Action of synthetic polyelectrolytes:

(1) Reduce electrostatic repulsion
(2) Adsorb on adjacent particles

* Commercially available polyelectrolytes (can be anionic, cationic, or nonionic):

polyacrylamides, polyethylenimines, and polyamine derivatives.
C. Adsorption on Filter Aids
* Why filter-aid filtration?
 Two major problems can be reduced:
(1) High compressibility of the accumulated biomass
(2) Penetration of small particles into the filter medium
 Lengthen the filtration cycle; improve the quality of the filtered liquor.

* How does the filter-aid help?

(1) Give porosity to the filter cake.
Solids to be filtered Porosity
Hard spheres of the same size  0.45
General cases 0.20.3
Compressible solids 0
Diatomaceous silica  0.9
(2) Create a very large surface to trap the gelatinous precipitate.
 Allow much more filtrate to be obtained before eventually clogging up.
* How to use filter-aid?
(1) Precoat—a thin layer (0.1 to 0.2 lb/ft2) of filter aid is deposited on the filter
medium prior to introducing the filter feed to the system
 - Protect the filter medium from fouling.
- Provide a finer matrix to exclude particles from the filtrate.
(2) Body feed—add the filter aid to the filter feed

* The use of filter-aid is mainly for removing small amounts of unwanted particulate
material.
 It cannot deal with large quantities of precipitate successfully.

* Types of filter-aid (the most effective):

(1) Diatomaceous earths such as Celite (consisting mainly of SiO2)
(2) Perlites (volcanic rock processed to yield an expanded form)
 Note: some products like the aminoglycoside antibiotics may
irreversibly bind to diatomaceous earth.
GENERAL THEORY FOR FILTRATION

Darcy’s law—relate the flow rate through a porous bed of solids to the pressure drop
causing that flow.
kP
v

where v = velocity of the liquid
P = pressure drop across the bed of thickness  (P/  = pressure gradient)
 = viscosity of the liquid
k = permeability of the bed, a proportionality constant (dimension: L2)

* Like Ohm’s law,  /k is the resistance of filtration.

Strictly speaking, Darcy’s law holds only when

vd
5
 (1   )
where d is the particle size of the filter cake,  is the liquid density, and  is the void
fraction in the cake.
* Biological separations almost always obey this inequality.

For a batch filtration,

1 dV 1 dV kP
v  
A dt A dt 
where V is the total volume of filtrate, A is the filter area, and t is the time.

Two contributions to the filtration resistance:


 R M  RC
k
where RM is the resistance of the filter medium (constant), and RC is the resistance of
the cake (varies with V).

The basic differential equation for filtration at constant pressure drop can thus
be obtained as:
1 dV P

A dt  ( R M  RC )
Incompressible Cakes

For incompressible cake,

V 
RC   0  
 A
where  = specific cake resistance, cm/g
 0 = mass of cake solids per volume of filtrate

1 dV P 1 dV P
   (I.C.: t = 0, V = 0)
A dt  ( R M  RC ) A dt [ 0 (V / A)  R M ]

Integration:
At  0  V  R M V 
    K   B
V 2P  A  P  A

0 R M
where K  and B 
2P P

Plot   versus   , slope = K.

At V
V   A
Known ,  0 , P.   can be determined.

Often, the medium resistance RM is insignificant, B = 0.

 0  V 
2

t  
2P  A 
[Example] A suspension containing 225 g of carbonyl iron powder, Grade E, per
liter of a solution of 0.01 N NaOH is to be filtered, using a leaf filter. Estimate the
size (area) of the filter needed to obtain 100 lb of dry cake in 1 h of filtration at a
constant pressure drop of 20 psi. The cake is incompressible. The specific cake
resistance is 1011 ft/lb. The resistance of the medium is taken as 0.1 in1.

At  0  V  R M
Solution:   
V 2P  A  P
mass of cake solid 225 g  28.32 L   lb 
0        14.0 lb/ft 3
volume of filtrate L  ft 3
  453.6 g 
100 lb
V  volume of filtrate  3
 7.1 ft 3
14.0 lb/ft
t = filtration time = 1 h
 2.116  10 3 lb f /ft 2   lb - ft   (3600) 2 s 2 
P  20 psi    32 . 2 2 2  = 1.2  1012 lb/ft-h2
 14.7 psi  lb f - s   h 
 = specific cake resistance = 1011 ft/lb
RM = resistance of the medium = 0.1 in1 = 1.2 ft1
 = viscosity of the liquid = 1 cp = 2.42 lb/ft-h (assumed)


A(1) (2.42)(1011 )(14.0) 7.1 (2.42)(1.2)

  
7.1 2(1.2  1012 ) A 1.2  1012

A2  1.7  1011A  71.2 = 0

A = 8.4 ft2
#
[Example] Streptomyces Filtration from an Erythromycin Broth. Using a test
filter, we find the following data for a broth containing the antibiotic erythromycin (紅
黴素) and added filter aid:

Filtration Time (s) Volume of Filtrate (L)

5 0.040
10 0.055
20 0.080
30 0.095
The filter leaf has a total area of 0.1 ft2 and the filtrate has a viscosity of 1.1 cp. The
pressure drop is 20 in. of mercury and the feed contains 0.015 kg dry cake per liter.
Determine the specific cake resistance  and the medium resistance RM.

At  0  V  R M
Solution:   
V 2P  A  P
Known data of V versus t.
 30.48 2 cm 2 
A = 0.1 ft2  2
2
 = 92.9 cm = 0.00929 m
2

 ft 
 0.01 g/cm - s 
 = 1.1 cp   = 0.011 g/cm-s
 1 cp 
1.01  10 6 dyne/cm 2   g - cm 
P = 20 in Hg    2 
= 6.77  105 g/cm-s2
 29.92 in Hg   dyne - s 
 0 = 0.015 kg/L = 0.015 g/cm
3

At V  0 R M
 Plot versus , slope = and intercept = .
V A 2P P

Intercept = 0  RM = 0
s - m4 s
Slope = 0.29 2
= 29
L cm 2
0.011    0.015
 29 
2  6.77  10 5
  = 2.34  1011 cm/g
[Example] We have filtered a slurry of sitosterol at constant pressure through a
filtration medium consisting of a screen support mounted across the end of a Pyrex
pipe. We find that the resistance of the filtration medium is negligible. We also
find the following data in a laboratory test:

Weight of crystals 62 g Cake depth 12.5 cm

Pressure of filtration 15 psi Cake volume 253.3 cm3
Filter diameter 5.08 cm Filtration time 163 min

On the basis of this laboratory test, predict the number of frames (30 in  30 in  1 in
thick) needed for a plate-and-frame press. Estimate the time required for filtering a
63 kg batch of steroid. In these calculations, assume that the feed pump will deliver
10 psi and that the filtrate from the press must be raised against the equivalent of 15 ft
head.

Solution:
62 g
Cake density  3
 0.245 g/cm 3
253.3 cm
63  10 3 g
Cake volume of 63 kg steroid =  2.57  105 cm 3
0.245 g/cm 3
2.57  105 cm 3  in 
3

Number of frames needed =  17.4

30  30  1 in 3  2.54 cm 
 18 frames are needed.
For incompressible cake with a negligible filter medium resistance,
 0  V   1   0V 
2 2

t   or t   
2 P  A  2 P  0  A 
2
 
  62 g 
In the laboratory test: 163 min   
2 (15 psi)  0   2 
(5.08 cm)
 4 
 min - psi - cm 4
  261
2 0 g2

In the large-scale operation:

2
 2.54 cm 
A  18  2  (30  30) in 
2
  2.09  105 cm 2
 in 
 14.7 psi 
P  10 psi  15 ft head    3.5 psi
 33.9 ft head (water) 
 1   0V 
2 2
1  63,000 
t    261     6.8 min
2  0 P  A  3.5  2.09  105 
#
Compressible Cakes

“Almost all cakes formed of biological materials are compressible. As

these cakes compress, filtration rates drop.”

To estimate the effects of compressibility, we assume that the cake resistance 

is a function of the pressure drop.
   ' (P) s
where ’ = a constant related largely to the size and shape of the particles forming the
cake
s = the cake compressibility

log   log  ' s log P

 Plot log versus logP, slope = s, intercept = log’.

 For a rigid, incompressible cake, s = 0.

 For a highly compressible cake, s  1.

 In practice, s ranges from 0.10.8.

 When values of s are high, one should consider pretreating the feed with filter
aids.
[Example] Filtration of Beer Containing Protease. We have a suspension of
Bacillus subtilis fermented to produce the enzyme protease. To separate the
biomass, we have added 1.3 times the biomass of a Celatom filter aid, yielding a beer
containing 3.6 wt% solid, with a viscosity of 6.6 cp. With a Buchner funnel 5 cm in
diameter attached to an aspirator, we have found that we can filter 100 cm3 of this
beer in 24 min. However, previous studies with this type of beer have had a
compressible cake with s equal to 2/3.
We now need to filter 3000 L of this material in a pilot plant’s plate-and-frame
press. This press has 15 frames, each of area 3520 cm2. The spacing between
these frames can be made large, so that we can filter all the beer in one single run.
The resistance of the filter medium is much smaller than the filter cake, and the total
pressure drop that can be used is 65 psi. How long will it take to filter this beer at
50 psi?

Solution:
 0  V 
2

Negligible RM  t  
2P  A 

 '  0  V 
2

Compressible cake,    ' (P) s

 t  
2P 1 s  A 
Laboratory test:

P = 14.7 psi (a Buchner funnel attached to an aspirator), A= (5 cm) 2 ,
4
3
V = 100 cm , t = 24 min, s = 2/3
2
 
 '  0  100 cm 3 
 24 min     ’0 = 4.53 min psi1/3 cm2
  (5 cm) 2 
1/ 3
2(14.7 psi)
 4 

Pilot-plant operation:
V = 3000 L = 3  106 cm3
A = 15  2  3520 cm2 (Filtration occurs on both sides of the frame.)
2
 '  0  V  4.53  3  106 
2

t      = 496 min = 8.3 h

2P1 s  A 2(50)1 / 3  15  2  3520 
#
ANALYSIS OF CONTINUOUS ROTARY VACUUM FILTERS

There are three stages involved in the

operation:
(1) cake formation,
(2) cake washing, and
(3) cake discharge (not affecting the
filter size and the cycle time).

Cake Formation
For compressible cake and negligible medium resistance,
2
 '  0  V   '  0  V f 
2

t   or t f   
2 P 1 s  A  2P 1 s  A 

where tf = cake formation time

Vf = volume of filtrate collected during the period of tf
A = filtration area (submerged area of filter)
2
 '  0  V f 
Let tf = tc and A = AT  t c   
2P 1 s  AT 

where tc = cycle time
AT = total filter area
 = fraction of the drum submerged

Cake Washing
Two factors involved in the stage of cake washing:
(1) The fraction of soluble material remained after the wash
 Governing the volume of wash liquid required.
(2) The rate of wash liquid passes through the cake
 Controlling the fraction of cycle time for cake washing.
An empirical equation for the fraction of soluble material remained:
r  (1   ) n

where r = ratio of soluble material remained after the wash to that originally
present in the cake
n = volume of wash liquid divided by the volume of retained liquid
 = washing efficiency of the cake
The wash liquid contains no additional solids.
 (1) The cake thickness is constant.
 The flow of wash liquid is constant.
(2) Wash rate = filtration rate at the end of cake formation
1 dVw Vw
Wash rate  
A dt At w

where Vw = volume of wash water required, and tw = time required for washing.
1 dV
Filtration rate at the end of cake formation =
A dt t t f

1/ 2
 '  0  V  V  2( P )1 s t 
2

t   or  
2P1 s  A  A   '  0 
1/ 2
1 dV d V   ( P )1 s 
Wash rate      
A dt t t f dt  A  t  t f  2  '  0 t f 
1/ 2
V  ( P )1 s 
 w  
At w  2  '  0 t f 

A useful expression:
1/ 2 1/ 2
Vw  ( P )1 s  Vf  2( P )1 s 
  ,  
At w  2  '  0 t f  At f   '  0 t f 

V  2  '  0 t f  V f   '  0 t f 
1/ 2 1/ 2

 tw  w  and t f 
A  ( P )1 s  A  2( P )1 s 

tw V V V
  2 w  2 w r  2nf
tf Vf Vr V f

where Vr = volume of liquid retained, and f = ratio of the volume of retained liquid to
the volume of filtrate.
[Example] It is desired to filter a cell broth at a rate of 2000 L/h on a rotary vacuum
filter at a vacuum pressure of 70 kPa. The cycle time for the drum is 60 s, and the
cake formation time is 15 s. The broth to be filtered has a viscosity of 2.0 cp and a
cake solid per volume of filtrate of 10 g/L. From laboratory tests, the specific cake
resistance has been determined to be 9  1010 cm/g. Determine the area of the filter
that is required.

Solution:
 0V f2
2
 0  V f 
For incompressible cake, t f    or A 2 
2  P  A  2t f P
g
  2 cp  0.02
cm - s
cm
  9  1010
g
g g
 0  10  10  10  3
L cm 3
 cm 3   h 
V f   2000  10 3   (15 s)    8333 cm 3
 h   3600 s 

N  kg - m  1000 g   m  g
P  70 kPa  70  10 3 2  2      7.0  105
m  N - s   kg  100 cm  cm - s 2

 0V f2(0.02)(9  1010 )(10  10 3 )(8333) 2

A 
2
  5.95  10 7 cm 4
2t f  P 2(15)(7.0  10 )5

 A = 7715 cm2 = 0.7715 m2

tc 60
AT  A   0.7715   3.09 m 2
tf 15
#
[Example] We want to filter 15,000 L/h of a beer containing erythromycin using a
rotary vacuum filter originally purchased for another product. Our filter has a cycle
time of 50 s and an area of 37.2 m2. It operates under a vacuum of 20 in Hg. The
pretreated broth forms an incompressible cake with the resistance:
 0
 29 s/cm 2
2P
We want to wash the cake until only 1% of the retained solubles is left, and we expect
that the washing efficiency will be 70% and that 1% of the filtrate is retained. (a)
Calculate the filtration time per cycle. (b) Find the washing time.
Solution:
2
 0  V f 
(a) For incompressible cake, t f  t c   
2P  AT 

 h 
V f  (15,000 L/h)  (50   s)    208 L  208  103 cm 3
 3600 s 
tc = 50 s
AT = 37.2 m2 = 37.2  104 cm2
0
 29 s/cm 2
2P
2
0  V f   208  103 
 tf     29   9.1 s
4 
2P  AT     37.2  10 

tw
(b)  2nf and r  (1   ) n
tf

Fraction of retained solubles, r = 0.01

Washing efficiency,  = 0.7
Fraction of filtrate retained, f = 0.01
r = 0.01 = (1  0.7)n  n = 3.82
tw = 2nf  tf = 2  3.82  0.01  9.1 = 0.7 s
#

Application of Rotary Vacuum Filter

 It is commonly used to recover yeast and mycelia.

 Filtration of bacterial fermentation broth will usually require a precoat of filter
aid.
 The separation of cell debris is performed by adding filter aid to the feed liquor.
CENTRIFUGAL FILTRATION

 * A combination of a centrifuge and a filter.

* Accumulated solids can be washed.
Hydrostatic Equilibrium in a Centrifugal Field
In a rotating centrifuge, a layer of liquid is thrown outward from the axis of
rotation and is held against the wall of the bowl by centrifugal force.

Consider a volume element of thickness dr at a radius r,

dF  r 2 dm

where dF = centrifugal force, dm = mass of liquid in the element, and  = angular

velocity.
dm   (2rh)dr

where  = density of the liquid, and h = height of the ring.

dF
 dF  2h 2 r 2 dr and  dP    2 rdr
2rh
1
Integration  P1  P2  P   2 (r22  r12 )
2

Principles of Centrifugal Filtration

R1 = radius of the surface of feed solution

Rc = radius of the cake’s interface
 k P P 1
Darcy’s law: v or  v
  k
1 P
Set   0    0 v
k 
For centrifugal filtration, the pressure drop varies with the radius, thus
dP
   0 v (Note: v varies with r.)
dr
Q
The total volumetric flow rate, Q = (2rh)v; or v 
2rh
dP  Q 
   0  
dr  2rh 
 Q  R0
Integration   P   0   ln
 2h  Rc
* Note: Rc is a function of time, and so is Q; however, Q is not a function of r.
The pressure drop (P) is due to the centrifugal force on the liquid.
1
 P   2 ( R02  R12 )
2
h 2 ( R02  R12 )
 Q
 0 ln( R0 / Rc )

Mass balance for the solids:  0V   C  ( R02  Rc2 )h (where c = cake density)
dV  c h dR  2h ( R02  R12 )
Q  (2 Rc ) c 
dt 0 dt  0 ln( R0 / Rc )
dRc  2 ( R02  R12 ) 1
  
dt 2  c  Rc ln( R0 / Rc )

I. C.: t = 0, Rc = R0

The integrated expression is complex, and can be approximated as:

 c Rc2  R 
2
R 
t  0   1  2 ln 0 
2  2 ( R02  R12 )  Rc   Rc 


 This is the desired result to find the time needed for obtaining a
cake of thickness (R0  Rc).

 0  V 
2

* Recalling that for a flat cake, t   

2P  A 
[Example] We can filter 250 cm3 of a slurry, containing 0.016 g progesterone (黃體
3 2
激素) per cm , in 32 min. Our filter has a surface area of 8.3 cm , a pressure drop of
1 atm, and a filter medium of negligible resistance. The solids in the cake have a
density of 1.09 g/cm3, and the slurry density is that of water.

We want to use this experiment to estimate the time to filter 1,600 liters of this
slurry through a centrifugal filter. The filter has a basket of 51 cm radius and 45 cm
height. It rotates at 530 rpm. When it is spinning, the liquid and cake together are
5.5 cm thick. How long will this filtration take?

Solution:
 0  V 
2

In the laboratory test, t   

2P  A 
t = 32 min = 1920 s
0 = 0.016 g/cm3
1.01  106 dyne/cm 2   g - cm/s 2  g
P  1 atm      1.01  10 6
 atm   dyne  cm - s 2

V = 250 cm3
A = 8.3 cm2
 (0.016 )  250 
2

 1920      = 2.67  108 s1

2(1.01  10 )  8.3 
6

 c Rc2  R 
2
R 
Using centrifugal filtration, t   0   1  2 ln 0 
2  ( R0  R1 )  Rc
2 2 2
  Rc 

 = 2.67  108 s1
c = 1.09 g/cm3
 = 1.0 g/cm3
 = 530 rpm = 55.47 s1
R0 = 51 cm
R1 = 51  5.5 = 45.5 cm
Mass balance for solids:  0V   c ( R02  Rc2 )h
 (0.016)(1,600  103) = (1.09)[(51)2  Rc2](45)  Rc = 49.3 cm
( 2.67  108 )(1.09)( 49.3) 2  51   51 
2

t 2    1  2 ln   466 s

2(1.0)(55.47) (51  45.5 )  49.3 
2 2
 49.3 