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Chemical Engineering Research and Design


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Laboratory cake ltration testing using constant rate


F.M. Mahdi, R.G. Holdich
Department of Chemical Engineering, Loughborough University, Loughborough LE11 3TU, UK

a b s t r a c t
A precipitated calcium carbonate with Sauter mean diameter of 7.5 m was ltered under conditions of constant rate
and constant pressure in a comparative laboratory investigation. The specic cake resistance to ltration was found
to vary between 1 109 and 1 1011 m kg1 , depending on the applied pressure, and the corresponding lter cake
volume concentrations were between 0.42 and 0.54 (v/v). The calculated specic resistance, from the particle size
distribution data and the KozenyCarman equation is one order of magnitude lower than that measured, even though
the solids were extremely robustly characterised. Practical lter testing rather than design based on size distributions
is known to be essential. However, the conventional approach is to use constant pressure laboratory tests, the results
presented here demonstrate that constant rate ltration is a more reliable method for data acquisition, especially
when determining the lter medium resistance, and readily available laboratory equipment is adequate for use.
2012 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
Keywords: Vacuum ltration; Calcium carbonate; Resistance; Cake compressibility

1.

Introduction

1.1.

Filtration

Cake ltration is a widely practised and mature technology


for both the recovery of solids and for ensuring the clarity of the ltrate (Svarovsky, 2000), either of which (or both)
can be the desired product. It is acknowledged to be considerably more economical than thermal dewatering for the
removal of liquid from the retained lter cake, and there have
been many developments for industrial equipment to maximise the mechanical dewatering effect (Earle and Earle, 1983).
In most cases laboratory testing of a material is performed
using conditions of constant pressure; normally using laboratory vacuum ltration, or an overpressure of compressed
gas in constant pressure ltration (Holdich, 2002). However
most industrial ltrations, apart from rotary vacuum drum
and disc lters, are performed under initial conditions closer
to constant rate: often a positive displacement pump is used
to feed a pressure lter and the rate of ltration will remain
constant until a signicant back pressure is established. There
are some signicant advantages in operating at low pressures
at the start of the ltration cycle, the ne particles present
are less likely to penetrate the lter medium and cause blinding. In the case of constant pressure ltration the entire and

ultimate pressure drop is over the lter medium from the


start of the ltration cycle, before signicant cake is formed,
and this can lead to serious blockage of the lter medium,
or compression of the initial cake layers. It can also lead to
non-conventional ltration conditions and lter cake nonuniformities (Stickland et al., 2005; Iritani, 2003).
For laboratory testing of moderately and highly compressible lter cakes the compression-permeability (CP) cell was
recommended for use in the 1960s, but it was later shown that
the pressure distribution within the cell is highly non-uniform
and it has only limited use today (Mattsson et al., 2011; Iritani,
2003). Furthermore, it is not possible to test the inuence of
solid concentration on the ltration performance using a CP
cell as concentrations need to be sufciently high for compression to be effective. The solids concentration can have a
signicant inuence on the measured cake resistance and the
lter medium resistance. When ltering low concentrations
the ability of ne particles to migrate into the lter medium is
greater and during the initial stages of ltration the medium
resistance will rapidly increase to what is assumed to be a constant value, but often orders of magnitude greater than the
medium resistance in the absence of solids (Kotlyarov, 1976).
In most laboratory studies the objective is to determine
the lter cake permeability, or specic cake resistance to ltration, and how it varies with ltration pressure as well

Corresponding author. Tel.: +44 1509 222519; fax: +44 1509 223923.
E-mail address: R.G.Holdich@Lboro.ac.uk (R.G. Holdich).
Received 9 August 2012; Received in revised form 10 October 2012; Accepted 19 November 2012
0263-8762/$ see front matter 2012 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.cherd.2012.11.012
Please cite this article in press as: Mahdi, F.M., Holdich, R.G., Laboratory cake ltration testing using constant rate. Chem. Eng. Res. Des. (2012),
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Nomenclature
A
C
c

cross sectional area (m)


solid concentration by volume fraction
dry mass of solids per unit ltrate volume
(kg m3 )
L
bed height (m)
m and n coefcients of the solid/liquid system
Pc
cake pressure (Pa)
medium resistance (m1 )
Rm
s
solid concentration of the slurry by mass
time (s)
t
V
volume of ltrate (m3 )
xsv
Sauter mean diameter (m)
Greek letters

specic cake resistance (m kg1 )


average specic cake resistance (m kg1 )
av
P
pressure drop (Pa)
pressure drop over the cake (Pa)
Pc
liquid viscosity (Pa s)


liquid density (kg m3 )
s
solid density (kg m3 )

as information on the lter medium resistance, after it has


stabilised. There have been studies comparing data from
constant pressure and constant rate ltrations over a number of years (Tiller, 1953; Tarabara et al., 2002). Generally,
the agreement between these two approaches is good, and
predictable, provided that the solids under investigation are
predominantly incompressible. Other studies have shown that
specic resistance by the two techniques can be quite different
(Rushton and Matsis, 1994). It has been proposed that a homogeneous constant growth rate of cake using constant rate
provides better packing structure of particles that is independent of cake thickness (Greil et al., 1992). Virezub et al. (1977)
found that constant rate provides more ltrate than constant
pressure ltration in less time. These latter studies raise a
question on the ability of the usually employed laboratory
constant pressure ltration tests to determine the ltration
parameters; specic resistance and lter medium resistance,
when used to predict the performance of, or design, industrial
ltration equipment operating under conditions of constant
rate. In the laboratory constant pressure is used because it
is not easy to provide constant rate ltration test conditions,
using readily available laboratory equipment.
Under constant rate the principal variables correlated are
pressure with ltrate volume, or ltration time which is proportional to the pressure. In the initial stages of ltration, the
lter medium has no cake and the measured pressure is due
to the resistance of the medium with initial deposit for a given
ow rate. Pressure then rises, depending on the slurry concentration and other parameters in the system (Chi, 2006; Rushton
et al., 2000; Greil et al., 1992; Shpanov, 1973; Tiller and Cooper,
1960; Tiller, 1955). It is usual to dene an average cake concentration and average specic resistance, both of which may be a
function of the applied pressure over the cake, at any instance
in time.
Increasing the applied pressure increases the cake density by reducing the spaces between particles. In general,
pressure has greater effect on soft and occulated materials,
which provide highly compressible lter cakes (Wakeman and

Tarleton, 2005; Nicholas, 1998). The equation used to correlate


average specic resistance and pressure is
av = 0 (1 n)Pnc

(1)

where av is the average specic resistance of the cake, Pc is


the pressure drop across the cake, 0 is the specic resistance
of the cake under a pressure drop of 1 bar and n is a constant
for the material, called its compressibility. This expression for
av can be inserted into the ltration equations and values for
0 and n can be determined experimentally by performing a
series of constant pressure ltrations at different pressures.

1.2.

Filtration conditions and benets

According to a number of research workers including Greil


et al. (1992), Tiller and Cooper (1960) and Tiller (1955, 1953)
the advantages and disadvantages of constant pressure and
constant rate ltration are:

1.2.1.

Constant pressure ltration

Advantages
A huge number of experimental studies.
Since liquid ow in the cake is additive, the ow rate necessarily increases as the liquid approaches the medium
compressing the lter cake.
Simplicity of obtaining the data.
Disadvantages
Calculations and results have to be treated with caution;
there is often a lack of consistency, especially when different
personnel perform the tests.
At the start there may be experimental difculties, such as
establishing a constant pressure over the lter cake, due to
a period of medium blocking.
There is not enough time to study the initial ltration period

1.2.2.

Constant rate ltration

Advantages
Upper and lower limits on the variation of solids pressure
in the lter cake can easily be obtained.
Industry use is widespread (apart from vacuum lters).
Constant growth rate of the cake is induced with reports of
homogeneous particle incorporation into the growing cake
surface.
The particle packing structure is expected to be independent of cake thickness so that uniform compacts are
formed.
.
Disadvantages
The applied pressure has to be continuously increased with
cake thickness.
In case of investigating gas deliquoring under pressure then
this test rig would need to be modied.
It is common in data analysis to assume that there is no
effect of sedimentation during cake formation. Hence, the
cake resistance and permeability are calculated using equations based on Darcys law for liquid ow through a cake from

Please cite this article in press as: Mahdi, F.M., Holdich, R.G., Laboratory cake ltration testing using constant rate. Chem. Eng. Res. Des. (2012),
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Fig. 1 Scanning electron microscope (SEM) image of calcium carbonate.


graphical plots of time over ltrate volume plotted against ltrate volume (constant pressure) or ltration pressure plotted
against ltrate volume, or time (constant rate). In general, during most ltration tests there are three regions during a test
run, which are: cake formation, transition and ow through
the already formed cake region (Couper et al., 2010; Li et al.,
2005; Wakeman and Tarleton, 2005).

1.3.

Basic analysis

As ltration proceeds, a porous cake of solid particles accumulates on a porous lter medium; its ltration rate can be
found from
rate of ltration =

driving force
resistance

By applying Darcys law the ow rate will be


Q=

constants in Eq. (5) can then be found from the intercept and
slope of a linear plot of P against V, noting that dV/dt is a constant, by denition. In the case of compressible cake ltration
equation (5) is still valid, at any increment in time, and the
intercept can be used to determine the lter medium resistance, but the relation will deviate from linearity as specic
resistance changes with the applied pressure over the lter
cake.

dV
AP
=
R
dt

(2)

where Q is the volumetric rate of ow, and the pressure drop


across the lter is
P =

 R   dV 
A

dt

(3)

where R is the total resistance that is formed of the lter


medium (Rm ) and the lter cake.
Addition of the lter cake and medium pressure drops
provides the well-known linear equation for the analysis of
constant pressure ltration:
Rm
av c
t
=
V+
A p
V
2A2 P

(4)

where t is the ltration time, V is the ltrate volume,  is the


liquid viscosity, A is the cross section ltration area, c is the
dry mass of solids per unit ltrate volume, Rm and av , are
ltration constants that may be evaluated from the intercept
and slope of the t/V vs. V plot, respectively.
The equation for constant rate ltration is
P =

Rm dV
av c
dV
+
(V)
dt
A dt
A2

(5)

Eq. (5) should be linear, provided that the average specic


resistance and dry cake mass per unit volume of ltrate
are constant; i.e. for incompressible ltration. The ltration

2.

Materials and methodology

2.1.

Material

Suspensions of aqueous calcium carbonate (CaCO3 Fordacal30 manufactured by MINELCO) at different solid concentrations: 9%, 11%, 13%, 15%, 17%, 19% and 21% by volume,
were prepared. In order to avoid too dilute feed suspension,
where sedimentation may inuence the ltration results, 9%
(v/v) was the lowest initial suspension concentration used.
Each suspension was prepared by dispersing the dry powder
in reverse osmosis water to avoid the ionic variation found
with tap water usage. The natural pH of the suspension was
8 and this was constant for all the tests. A Sauter mean
diameter of 7.5 m was measured using a Horiba LA-920-wet
Laser dynamic scattering device. Scanning electron microscope (SEM) images of the calcium carbonate powder show
a rhomboidal shape, indicating that the material is mainly
calcite, see Fig. 1. The values of the D10 , D50 and D90 particle diameters, measured by the Horiba at a variety of different
recirculation pump speeds, are shown in Fig. 2.

2.2.

Methodology

Constant rate ltration tests were performed in a clear acrylic


cell with an inner diameter of 60 mm and total volume of
424 mL as represented in Fig. 3, using a laboratory pump to
suck the ltrate through the lter medium and depositing
cake. To ensure a clear ltrate in all tests and promote cake
ltration, a metal microporous membrane, with 10 m slots,
manufactured by Micropore Technologies Ltd. (Hatton, Derbyshire, UK) was used as the lter medium. This 10 m rated
membrane had a nominal thickness of 0.06 mm and a measured hydraulic permeability of 1.2 1013 m2 , when clean,
tested by a series of water ow tests at different pressures. At
the base of the cell, within the ltrate line, a pressure transducer (HCX Series Honeywell S&C) was used to monitor the

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Fig. 2 Variation of the particle diameters (D10 , D50 and D90 ) over time for six different pump speeds (P.Sp.) 1, 3, 6, 9, 12 and
15 rpm during analysis by laser diffraction.
vacuum. A vacuum gauge (WIKA Instruments Ltd.) was also
connected to the system in order to validate and check the
sensor reading. The ltrate was pumped out using a peristaltic pump (Watson Marlow 401U/D1) and collected in a
vessel placed on an electronic balance (OHAUS SPU601). The
weight of the ltrate and pressure drop in the system, as a
function of time, were recorded using a PC within Labview
software. For the tests three different ltrate pump settings
were used (10, 30 and 50%) of full-scale, which gave rise to

three different ltration rates and cake forming pressure proles.


The same suspension was used many times, to avoid any
variability in the feed material. The loss in the reused suspension was monitored between ltrations and found to be
very low (approx. 1% between runs). The dead volume below
the microporous membrane and within the lter tubes was
lled with ltrate from a ltration of similar CaCO3 before
starting an experiment, in order to avoid missing ltration

Fig. 3 Schematic diagram of constant rate vacuum ltration equipment.


Please cite this article in press as: Mahdi, F.M., Holdich, R.G., Laboratory cake ltration testing using constant rate. Chem. Eng. Res. Des. (2012),
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Table 1 Measured cake heights and determined cake concentrations with 95% condence limits on height
measurements.
In. concentration (v/v)

Pump speed (rpm)

Cake height (mm)

Cake concentration (v/v)

Errora % ()

9%

5
10
30

20.12
19.31
18.28

0.475
0.494
0.522

4.46
4.45
4.90

11%

5
10
30

24.36
21.21
19.85

0.479
0.550
0.588

2.76
3.17
3.40

13%

5
10
30

31.35
27.76
26.61

0.440
0.497
0.518

4.48
5.06
5.30

15%

5
10
30

36.38
32.33
30.34

0.438
0.492
0.525

2.05
2.30
2.40

17%

5
10
30

44.22
35.48
34.72

0.408
0.508
0.520

2.19
2.74
2.80

19%

5
10
30

45.02
39.30
37.86

0.448
0.513
0.533

1.17
1.34
1.40

21%

5
10
30

51.81
44.68
42.09

0.430
0.499
0.528

1.95
2.27
2.40

95% condence that the concentration is the one provided plus or minus two times the standard deviation based on the cake height
measurement variability.

data at the very early stages of the experiment due to lling


this dead volume. Before each series of tests, the suspension
was prepared and left at room temperature (20 2 C) for at
least 24 h, with periodic mixing. This ensured that the system
had reached ionic equilibrium and avoided thermal gradients.
To validate the calculations of the nal cake concentrations
a vernier-scale measuring calliper was used; measuring over
ve different positions of cake height per test and using the
average cake height for a mass balance to give the cake concentration. Measuring was done from the top of the cell to
the lter medium before starting the experiment and to the
cake surface at the end. The cake height was, therefore, the
difference between these two. It was possible to clean the
membrane after each run and reuse it.
For comparison with the constant rate ltration data, tests
were also performed in a similar ltration cell under conditions of constant pressure. The same material was ltered,
using the same lter medium as before. The vacuum was
applied by a vacuum pump and the vacuum receiver was
positioned on a scale balance in order to measure the mass
of ltrate recovered with respect to ltration time. A needle
valve was used to bleed air into the vacuum receiver, to enable
different amounts of vacuum across the lter to be achieved.

3.

Results and discussion

3.1.

Cluster formation analysis

3.1.1.

SEM image

From Fig. 1 it is uncertain if particles are loosely agglomerated


together, forming clusters, or if the particles are composed of
fused together crystals. Fine particles may be dragged through
the cake by the shear eld into the lower regions of the lter
cake and, likely to, be deposited at the lter medium. Another
aspect that was considered is the ability of the particles to

form clusters that may compress with a variable pressure


applied, this has been shown to have a major inuence on
the analysis and modelling of ltration and sedimentation
process (Di Giovanni et al., 2012). Hence, a particle characterisation study was performed investigating the possibility of
clustering.

3.1.2.

Results analysis and cluster formation

The variation of the D10 , D50 and D90 particle diameters over
time for six different values of shear elds created by increasing the laser diffraction equipment pump speed from 1 to 15,
is shown in Fig. 2. This work done with and without sonication and the results were the same for both cases. The lack
of variation of these particle diameters shows that there was
no signicant aggregation of the calcium carbonate particles
suggesting that particle clustering is not a problem with this
material under the prevailing conditions. The water used during these tests was collected ltrate.

3.2.

Cake concentration and uniformity

Cake concentration was determined using the knowledge of


the starting volume concentration and volume of slurry ltered, together with the measured lter cake heights and the
lter area, by a material balance. The standard deviation of
the height measurements was calculated and a test of signicance based on 95% condence was applied: i.e. the expected
error on the calculated cake concentrations are plus, or minus,
two times the standard deviation around the mean value. The
measured heights, calculated cake concentrations and error,
based on 95% condence are shown in Table 1. The results
show that the expected error decreased rapidly from approx.
5% with an initial slurry concentration of 9% (v/v) to less than
1.5% when using 19% (v/v) feed suspension, a consequence of a
more homogeneous bed structure being formed. It is assumed

Please cite this article in press as: Mahdi, F.M., Holdich, R.G., Laboratory cake ltration testing using constant rate. Chem. Eng. Res. Des. (2012),
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Fig. 4 Effect of pressure on cake concentration with initial concentrations 921 (% v/v); number in the gure indicates
pump speed 5, 10 and 30 [errors bars provide 95% condence interval].
that the cake is of uniform, or average, concentration throughout its height and is discussed further later.
The uncertainty bars around the mean values in Fig. 4 represent two times the standard deviation around the mean
concentration value, based on the ve height measurements
used to calculate that concentration. Hence, the condence
level in the cake concentration is again 95% within the range
illustrated by the bars. Fig. 4 shows three different trends,
which depend on pump speed and initial suspension concentration. Pump speed determines the ltration ow rate and,
consequently, the pressure drop in the lter cake, which has
the expected power-law type of relation with the cake concentration. The cake volume concentration was used to calculate
the dry cake mass per unit volume of ltrate (Holdich, 2002),
using Eq. (6).

c=

1
(1 s)/(s) (1 C)/(Cs )

Finally on the subject of using the experimental technique


for the analysis of industrially relevant ltration testing using
a sample taken from a process stream, if conrmation of the
cake uniformity by height measurement is not required, the
simplest equation for dry cake mass per ltrate volume at the
end of the ltration comes from the knowledge of the mass of
slurry ltered (M) and the ltrate volume (VF ):
c=

sM
VF

(7)

It is proposed that Eq. (7) would be used for most industrial


slurries due to its simplicity and ability to be applied when
ltering mixtures, where densities are less likely to be known.

3.3.
Specic resistance by constant rate and constant
pressure testing
(6)

where C is the cake concentration by volume fraction, s is the


mass fraction of solids in the slurry, s is the density of solids
and  is the liquid density.
One aspect of the reported work is to assess the applicability of the experimental technique to an industrially relevant
ltration testing study. In such a case, it is likely that a slurry
sample can be taken from a process stream, and the solids
concentration by mass could be determined (by drying). However, obtaining a representative sample of the lter cake is
more difcult and it is time-consuming to weigh and dry the
entire cake. The measurement of the cake height at the end
of the experiment is a much more rapid method for determination of the dry cake mass per unit ltrate volume, and it
can be used to check the uniformity of the cake concentration by comparison with the height predicted from a volume
balance: i.e. cake volume = original volume ltrate volume.
Using the knowledge of the lter area enables the cake height
to be predicted and compared with the measured height. If
the measured height is signicantly higher than the predicted
value, then the lter cake is not uniform. In the tests reported
here the measured and predicted heights agreed to approximately 2%, suggesting that a uniform cake concentration can
be assumed.

The two linear equations represented by Eqs. (5) and (4) represent the conventional method of analysis for determining
specic resistance from constant rate and constant pressure
ltrations respectively. Examples of the results from these
tests are shown in Figs. 5 and 6 respectively. In Fig. 5 three
different starting concentrations are illustrated: 11%, 15% and
21% (v/v). There is a very slight intercept above the origin on
the pressure axis, indicating a small but nite lter medium
resistance, in accordance with Eq. (5). It is relatively easy to
determine the intercept from the cut-away graph and linearity of these data plots is good, after about 10 mL of ltrate and
up to about 120 mL, after which the ltration is substantially
completed. For comparison, Fig. 6 shows a typical set of data
achieved using the constant pressure ltration equipment, at
a constant feed concentration of 11% (v/v), and three different constant applied pressures: 0.2, 0.4 and 0.6 bar. Again the
linearity is good, but as is typical of constant pressure ltration the intercept values are highly scattered and the trend
with pressure (for a constant value of Rm ) is not as would be
expected from Eq. (4). It did not help to plot the initial data
on an expanded scale, as it was very randomly scattered, as is
often the case in constant pressure ltration.
Both sets of data, together with a number of other tests,
were used to determine the relation between specic resistance and pressure. The log plot for the constant rate tests is

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Fig. 5 Measured ltration pressure during ltration at three starting concentrations: 11%, 15% and 21% (v/v) with 10 rpm
pump speed.
shown in Fig. 7, where the specic resistance and pressure values plotted were determined by the end point of the constant
rate ltration data: i.e. the last recorded values for specic
resistance with pressure using the rearranged form of Eq. (5):

av =

A
cV

 PA  dt 


dV

Rm


(8)

The end point of the ltration was deemed to be the most


appropriate part of the ltration for this analysis, to ensure
that the conditions within the lter cake had stabilised adequately; most specically, the lter cake concentration or dry
cake mass per unit volume of ltrate (Rushton et al., 2000).
Table 2 shows data comparing the ltration scale up constants
obtained by using the two ltration techniques: constant rate
and constant pressure. It is noticeable that the data does
appear to be very similar, as would be expected for a material of moderate compressibility. Also included in Table 2 is
the data for the cake concentration as a function of pressure,
obtained from the data illustrated in Fig. 4.

When ltering compressible materials the dry cake mass


per unit volume of ltrate will vary with pressure, as concentration does, see Eq. (6). However, it is usual for the variation of
concentration with pressure to be much less than the variation
of specic resistance with pressure (Holdich, 2002). Nevertheless, concentration will vary during a constant rate ltration
during the early stages, as the pressure applied rises from zero
to its ultimate value. It is informative to investigate this further, by solving Eq. (8) for all times during the ltration and
comparing the values of specic resistance, as a function of
pressure, with the average values obtained at the end of all
the ltrations; at known values of pressure and ow rate. Fig. 7
provides all the data used to determine the specic resistance
scale up constants, which were provided in Table 2. In all cases
the specic resistance was determined from the last ltration
data point: i.e. values of pressure and ow rate. As would be
expected, a low pump speed provides a low pressure resulting in a lower specic resistance. A best t line was used on
the logarithmic data to provide the values for the scale-up
constants, as indicated by Eq. (1).

Fig. 6 Constant pressure ltration of calcite at 11% (v/v) starting concentration and three total applied pressures for
analysis by parabolic rate law.
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Fig. 7 Effect of pressure on cake ltration resistance, initial concentrations from 9 to 21 (% v/v); numbers in the gure
indicate pump speeds 5, 10 and 30 rpm.

Table 2 Comparison of constant rate and constant


pressure ltration techniques for the determination of
coefcients in the constitutive equations for scale-up
constants.
Technique
a

Constant rate
Constant pressureb
a
b

0 (m kg1 )

Co (v/v)

6.78 10
5.53 109

0.19
0.18

0.25

0.08

Initial concentration 921% (v/v) applied pressure range 880 kPa.


Initial concentration 13% (v/v), applied pressure range 3060 kPa.

In Fig. 8 the specic resistance at each time interval is calculated, according to Eq. (8), and this is compared to the specic
resistance calculated using Eq. (1), where the cake forming
pressure is used. In order to determine the cake forming pressure the lter medium resistance was assumed to be constant
and equal to the value determined from Fig. 5. This gave a
value of 1.43 109 m1 . The agreement between the values of
specic resistance calculated by Eqs. (1) and (8) is very good.
Clearly, as an experimental technique it would be possible to

use the constant rate ltration equipment to determine values


for specic resistance as a function of pressure, provided the
dry cake mass per unit volume of ltrate is recalculated at each
time increment, as it was using Eq. (6) and then Eq. (8). Just one
experiment would provide the data for specic resistance as a
function of pressure over a wide range of pressures, but a few
experiments are required to determine the cake concentration functionality with pressure as illustrated in Fig. 4 (which
provides a constitutive equation for the analysis used in Eq.
(8)). In Fig. 8, an additional comparison is provided by specic resistance calculated using the KozenyCarman equation
for permeability and hence specic resistance. The resulting
equation is:
av =

36KC
3

2 
(1 C) xsv
s

(9)

where K is the Kozeny constant, a value of 5 was used as is con2 is the Sauter mean diameter of
ventionally assumed, and xsv
the particles. It is fairly common for the text book value of the
Kozeny constant to provide values of permeability, and hence

Fig. 8 The effect of pressure during constant rate ltration test on the specic cake resistance during ltration of the 21%
(v/v) feed solids at 10 rpm pump speed and theoretical resistance by KozenyCarman.
Please cite this article in press as: Mahdi, F.M., Holdich, R.G., Laboratory cake ltration testing using constant rate. Chem. Eng. Res. Des. (2012),
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Fig. 9 The percentage of total ltration resistance due to the lter medium as a function of total applied ltration pressure
and time.
specic resistance, that are an order of magnitude lower resistance (higher permeability) than are measured. It is notable
that this occurs even here when using very stable and well
characterised solids, as evidenced by the data illustrated in
Fig. 2. Hence, there is a signicant need for laboratory testing when designing ltration systems and the constant rate
system, described here, provides a convenient and thorough
technique for such analysis. By changing the Kozeny constant
to a value of 33 it was found possible to match the specic
resistance data illustrated in Fig. 8, but the text book value of
5 is signicantly in error.
The conventional technique for laboratory testing is a constant pressure ltration. Supercially, this has the attraction
of providing a xed and known pressure drop so that a limited
number of experiments, typically four, may provide values of
specic resistance and cake concentration as a function of
pressure; to provide the data for Eq. (1) and its concentration equivalent equation. However, the results are often very
scattered and one reason for this is due to the lack of constant pressure conditions. Even if the total applied pressure
remains constant, the pressure drop over the lter cake will
vary during an experiment and hence so will the pressures
that should be used in Eq. (1); where cake forming and not
total pressure should be used. At the start of the constant
pressure ltration the total pressure drop is over the lter
medium and zero pressure is over the lter cake. During the
initial stages the proportion of the pressure drop over the cake
rises from zero to a nite amount. After a short while it is usually assumed that the total pressure drop is now acting over
the cake but between the start of the ltration, and the end, the
pressure forming the cake will be changing. Hence, even during constant pressure ltration the cake forming pressure is
varying. The point of varying resistance over the lter medium
is illustrated for the constant rate ltration data investigated
here in Fig. 9. At the start the percentage of the total pressure drop due to the lter medium is 100%, but this quickly
drops down to a negligible amount. The inset graph shows
that this is a period during which the applied pressure rises to
30 mbar, equal to 200 s. Hence, over the rst 200 s the cake concentration would be expected to be changing rapidly. During
constant pressure ltration this stabilisation period is likely

to be faster, as the applied pressure is normally much higher,


but there would also be a higher pressure driving the ne particles into the ltration medium. This will lead to a greater
ltration medium resistance than when operating under the
more mild pressures at the start of the ltration that constant
rate uses.
To summarise, the constant rate laboratory equipment for
analysis of ltration performance is best used as follows. A
slurry sample to be tested is taken and weighed (M) and a
separate small sample is weighed, dried and weighed again
to provide a value for s. After ltration the dry cake mass
per unit volume of ltrate for the entire ltration can be
determined from Eq. (7). The average cake concentration by
volume fraction can be determined from a rearranged form of
Eq. (6). At least three different cake forming pressure ranges
(pump speeds) should be used, to obtain data similar to that
illustrated in Fig. 4 and suitable for determining the cake concentration constants with pressure as provided in Table 2. The
initial stages of the ltration are important for the determination of Rm , as illustrated in Fig. 5. This is then assumed to
remain constant during ltration, allowing the pressure drop
over the lter medium to be calculated and hence the cake
forming pressure. The average dry cake mass per unit volume
of ltrate at any instance in time can be determined from Eq.
(6), using the cake volume fraction calculated for the pressure
drop over the cake only. The specic cake resistance, at the
cake forming pressure, can be calculated using Eq. (8), where
the total pressure difference is used in this equation. It is then
possible to use Eq. (1) to correlate specic resistance with cake
forming pressure.

4.

Conclusions

The acquisition of design data for cake ltration is normally


obtained from laboratory investigations performed under
conditions of constant pressure ltration. However, most nonvacuum industrial ltrations are under conditions that are
closer to constant rate, where the pressure drop over the lter
cake will be varying signicantly and the cake concentration
will also vary with time. Constant rate laboratory ltration
testing is not normally conducted as the laboratory equipment

Please cite this article in press as: Mahdi, F.M., Holdich, R.G., Laboratory cake ltration testing using constant rate. Chem. Eng. Res. Des. (2012),
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is not so prevalent. However, it is possible to induce ltration by means of a simple laboratory peristaltic pump and to
very precisely monitor the mass of ltrate with time using
a balance. Using this procedure reliable data points at the
start of the ltration can be determined, providing a reliable value for the lter medium resistance. The robustness
of this data is superior to what is normally obtained from the
alternative constant pressure ltration data. Even in the case
of constant total pressure ltrations, the pressure difference
going to form the lter cake will vary; as the proportion of
the total pressure over the lter medium varies from 100%
at the start of the ltration to a much lower value towards
the end of the ltration. The actual pressure forming the cake
can only be calculated knowing the lter medium resistance,
which is notoriously difcult to achieve when using a constant pressure ltration with small samples of slurry and lter
areas.
Once it has been reliably established, the medium resistance can be assumed to remain constant during the ltration
and the values of ltration rate at any instance in time will
provide the pressure drop over the lter medium from Darcys
law. Hence, by deduction from the total pressure drop the
value of pressure over the lter cake can be calculated at any
instance in time. Likewise, it is possible to deduce the average
specic resistance to ltration at any instance and this can be
plotted against the prevailing cake forming pressure. Hence,
a constant rate ltration provides much more detailed information than the alternative constant pressure ltration, for
the purposes of ltration analyses. Mass balancing tests, such
as measurement of the formed cake height, and its variability
over a number of different locations, can also be used to check
on the reliability of the information obtained.
The range over which the pressure may be varied is, of
course, limited by the vapourisation of the liquid. This is not a
signicant problem when ltering water based suspensions
at normal temperatures encountered in the laboratory, but
ashing is a known problem with vacuum ltration systems
when conducting constant pressure ltration tests using a
vacuum pump, and even vacuum ltration equipment. However, it is worth noting that the most noticeable variation of
specic resistance with pressure is found within the lower
pressure range; as pressure increases, the change in resistance
becomes less pronounced as would be expected of a power
law equation such as that shown in Eq. (1). Hence, the most
relevant region to investigate is the lower pressure one.

Acknowledgements
The author FMM is grateful to the Libyan Ministry of Higher
Education and Sirte University, Libya for sponsoring this work.

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Please cite this article in press as: Mahdi, F.M., Holdich, R.G., Laboratory cake ltration testing using constant rate. Chem. Eng. Res. Des. (2012),
http://dx.doi.org/10.1016/j.cherd.2012.11.012

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