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Chinese Journal of Chemical Engineering, 19(5) 792798 (2011)

A Study on Enhancement of Filtration Process with Filter Aids


Diatomaceous Earth and Wood Pulp Cellulose
DU Lihong ()1,2,*, CHEN Xu ()1, LI Wenping ()3 and ZHU Qixin ()1
1
2
3

Chemical Industry Academy, Tianjin University, Tianjin 300072, China


Shanghai Research Institute of Chemical Industry, Shanghai 200062, China
Agrilectric Research Company, Lake Charles, USA

Abstract In this paper, a study to enhance the filtration for solid/liquid materials difficult to be filtered, such as
highly viscous, highly compactible or gel like materials, is presented. Filter aids diatomaceous earth and wood pulp
cellulose are used to enhance the filtration by improving filter cake structure and properties in the filtration of a
biological health product and a highly viscous chemical fiber polymer melt product. The property of solid/liquid
systems, filtration at different flow rates, specific cake resistance, cake wetness, filtration rate, filtrate turbidity for
filter aid selection and evaluation, and operation optimization are investigated. The results are successfully applied
to industrial process, and can be used as a reference for similar filtration applications.
Keywords filter aid, specific cake resistance, cake compressibility coefficient, diatomaceous earth, wood pulp
cellulose

INTRODUCTION

Filtration and separation operations are widely


used in chemical, petrochemical, pharmaceutical industries, and other areas such as health and biological
products, drink and wine, and new material manufacture. Some solid/liquid systems in these applications
are highly viscous, colloidal, stable, deformable or highly
compactible and very difficult to be filtered with the
formation of little cake or highly resistant cake. For
such materials, some approaches, such as addition of
filter aid, are needed to enhance the filtration and improve the efficiency of filtration operation [1, 2].
Filter aids are normally particulate or fiber materials. They can be used as a precoat or bodyfeed or
their combination. With a precoat, filter aid forms a
dense yet porous and highly permeable cake layer on
the filter medium to protect it from clogging, improving the separation efficiency. In bodyfeed applications,
filter aid is mixed with the solid/liquid suspension to
increase cake porosity, decrease cake compactibility
and therefore improve the filtration and flow rate. Filter
aid enables the cake filtration to be used for various
suspensions with wider particle size distribution, larger
solid concentration range and different solid particles,
such as gel like and highly compactible particles [3-6].
Effects of filter aid to assist cake filtration can be
evaluated by porosity, specific cake resistance, and
cake compressibility coefficient of precoat or filter
cake with the addition of filter aid. This paper focuses
on the filtration of biological health product and
highly viscous chemical fiber polymer melt with the
assistance of diatomaceous earth and wood pulp fiber.
Results on cake porosity, specific cake resistance and
cake compressibility coefficient and corresponding
filtration properties are presented.

2
2.1

THEORY
Darcys theory

Based on Poiseuille equation for viscous flow


through capillaries, Darcy [2, 3, 7] established Darcys
law that correlates flow rate with pressure drop as the
liquid flows through a porous bed, or filtrate flows
through a filter cake:
p
dV
= KP c
(1)
q=
Adt
L
where Kp is the cake permeability, determined by cake
structure, size and shape of particulates.
To replace the cake permeability with average
specific cake resistance av and cake thickness with
volume of cake per unit area c, Eq. (1) can be written as
1 pc
q=
(2)

av c

The differentiation of Eqs. (1) and (2) gives


K dpL
1 dpL
q=
=
dx d

(3)

in which K is the permeability of cake dx, and is


specific cake resistance of cake d. The integration of
Eq. (3) needs the relationships for K vs. pL and vs.
pL. Since K and are directly related to ps rather than
pL, the force balance or stress analysis for the cake
must be first conducted.
2.2 Stress analysis and empirical constitutive
equation

Figure 1 shows a simplified cake structure with

Received 2011-06-02, accepted 2011-07-04.


* To whom correspondence should be addressed. E-mail: 1186394191@qq.com

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Chin. J. Chem. Eng., Vol. 19, No. 5, October 2011

the parameters by stepped pressure test and data fitting,


with which a large amount of testing data is required
to conduct the data analysis [11-13].
Based on Darys Law, Ruth [3] developed a cake
resistance model, which combines filtration flow rate,
cake resistance and other filtration data. The Ruth
cake resistance model can be used to determine cake
resistance and cake compressibility parameters by
constant pressure cake filtration test [14, 15].
2.3

Figure 1 Diagram of a cake with spatial x and material


coordinates [8-10]

spatial x and material coordinates. It is assumed that


the particles are in point contact and liquid pressure is
uniform over the cross sectional area in the cake.
Based on the force balance, the effective pressure ps,
caused by accumulative friction Fs as ps = Fs/A, is
balanced with hydraulic pressure pL on dx. We have
dps + dpL = 0.
To integrate Eq. (2), K and must be functions
of ps. Replacing ps with pL in Eq. (3) based on the
stress analysis, we have
K dps
1 dps
q=
=
(4)
dx
d
K and as functions of ps and cake solid content ratio
(solidosity) s as a function of ps are given [11-13] as
following empirical constitutive equations.

s = s0 (1 + ps / pa )

= 0 (1 + ps / pa )

K = K 0 (1 + ps / pa )
1/

1/

The Ruth cake resistance model

2.3.1 K and av
Based on the Ruth cake resistance model [2, 4],
for constant pressure filtration, we have
dv
p
=
dt
v cg vm cg
av
+

1 m cg 1 m cg

p 1 m cg

1/ n

s
K

p
= =1+ s
(6)

p
a
s0
0
0
in which , and n are cake compressibility coefficients. They are used to evaluate the variations of s,
and K as ps changes. Parameters so, 0, and K0 are
initial cake layer solidosity, specific cake resistance,
and permeability as ps equals zero, respectively.
The relationship of , n and can be given by
/5 = n/4 =
(7)
With Eqs. (6) and (7) and the boundary conditions, if s0, 0, K0, , , and n are known, Eq. (4) can
be integrated to give filtrate flow rate and average
liquid or solid content in the cake at certain time and
operation pressure [1, 6, 7]. The above parameters are
normally determined by measuring specific cake resistance and cake porosity or solidosity vs. pressure
based on compression-permeability cell tests. The test
is rather complicated and results vary with testing cell,
friction, and testing method and procedure. Tiller and
Li developed a simplified testing method to measure

(8)

cg av (v + vm )

If the filter medium resistance can be neglected, we


have vm = 0.
Integrating Eq. (1) and taking reciprocal of the
integrate yields
t cg av ( v + 2vm ) 1
=
= ( v + 2vm )
v
K
2p 1 m cg

(9)

in which K is called Ruth constant pressure filtration


coefficient,
K=

(5)

2p 1 m cg

(10)

cg av

From Eq. (10), we have

av =

2p 1 m cg

cg K

(11)

In a constant pressure cake filtration, with known slurry


concentration cg, filtrate viscosity and density ,
constant cake pressure p, measured wet and dry cake
ratio m, and volume of filtrate per unit area v (m3m2)
vs. time, K can be determined by plotting t/v vs. v, and
the average specific cake resistance av is obtained.
2.3.2 Determination of cake compressibility coefficient n
Based on experimental data, the specific cake resistance for most compactible filter cakes is exponentially related with filtration pressure by

av = 0 (p)n

(12)

Equation (12) can be transformed to

lg av = lg 0 + n lg p

(13)

Based on Eq. (13), n can be determined by plotting lgav

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Chin. J. Chem. Eng., Vol. 19, No. 5, October 2011

vs. lgp. The average specific cake resistance is determined from Eqs. (9) and (11) with the data from the
constant pressure filtration. At least five constant pressure tests are need to provide sufficient av and p data.
Porosity, average specific resistance, and compressibility coefficient of filter cakes and their effects
to filtration performance with the addition of filter
aids will be investigated. Filter aids involved in the
study are diatomaceous earth (DE) and wood pulp
fiber, which are hard and rigid particles and a soft
material, respectively.
3
FILTRATION WITH DIATOMACEOUS
EARTH FOR BIOLOGICAL HEALTH PRODUCT

Three types of DE filter aids, 1#, 2# and 3#, are


used in the study. Fig. 2 shows the particle size distribution.

cake resistance increases as pressure drop increases.


This can be explained by the compaction of rigid DE
particles as pressure increases during the tests. As the
DE particles are rigid, the cake compaction may reach
a maximum, where the effect of pressure on cake resistance is little. However, even for rigid particles
such as DE, the specific cake resistance increases with
pressure drop within certain pressure range. It is wise
to always seek optimum operating pressure.
3.2 Compressibility coefficient of diatomaceous
earth cake

Cake compressibility n of three DE filter aids


determined by plotting lgav vs. lgp based on Eq. (13)
and constant pressure filtration data is shown in Table 1.
The coefficient for the three DE filter aids based on
Eq. (7) is also listed in the table. The filtration pressure drop in the tests ranges from 0.015 to 0.09 MPa.
Table 1

Figure 2

Particle size distribution of three DE filter aids

Figure 3 Average specific cake resistance vs. pressure


drop of 2# filter aid

Filter Aid

1#

0.13

0.16

2#

0.04

0.05

3#

0.15

0.19

Based on the classification [8, 13, 16] of cake


compressibility as shown in Table 2, the filter cakes
from the three types of DE fall into the nearly incompressible category.
Table 2

3.1 Average specific resistance of filter aids and


effect of pressure

Pressure drop provides driving force in filtration.


It is a common understanding that filtration flow rate
increases with pressure drop, which is often accompanied by increase of filtration resistance.
Figure 3 shows the variation of specific cake resistance of 2# DE filter aid against pressure. The specific

Compression coefficient of filter aids

Classification of filter cake compactibility

incompressible

n=0

=0

moderately compactible

n0.5-0.6

0.6-0.8

highly compactible

n0.7-0.8

0.9-1.0

super-compactible

n>1

>1.0

3.3

Filtration of biological health product

3.3.1 Sample property


The material involved is a health product enzyme
solution. It has a viscosity of 3103 Pas, soft and floc
like solid particles with mass concentration of 1.69%.
The particle size distribution of the solids is shown in
Fig. 4, in which the x axis is particle size (m), and
the y axis is the cumulative volume (%) of particles
and the differential coefficient volume (%) of particles.
The medium particle size d50 is 7.11 m.
3.3.2 Selection of filter aid
The objective of the process is to remove the
solid particles and obtain clear filtrate product. The
soft and floc like solid particles in the enzyme solution
are difficult to be separated by centrifugation, pressure
or vacuum filtration due to the formation of highly

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Chin. J. Chem. Eng., Vol. 19, No. 5, October 2011

dense and resistant cake. The filtration such material


can be improved by bodyfeed addition of inert, rigid,
low resistant filter aid.
Figure 4 shows that the particle size is more
concentrated in the ranges of 0.5-70 m and 70-500
m. Comparing the particle size distribution with that
of the three DE filter aids, one can see that 1# DE
filter aid is in the first range and 3# DE is in a wider
range including the two ranges. Thus DE filter aids 1#
and 3# are selected to assist filtration of the enzyme
solution.

Figure 4

Table 4
Pressure
drop/MPa
0.06

Filtration of enzyme solution with DE 3# under


different pressure drop
Total
Wet and dry
Specific cake
filtration cake mass
resistance/mkg1
time/s
ratio
780
315

1.87

3.6510

114

0.14

255

1.83

4.051011

224

0.2

146

1.82

4.421011

359

11

Particle size in enzyme solution

Constant pressure filtration tests were carried out


with 500 ml enzyme solution under 0.07 MPa pressure
drop. A dosage of 2% (by mass) of DE filter aid 1# or
3# was added to the enzyme solution. Results are
shown in Table 3. Filter aid 3# yields a lower cake
resistance, shorter filtration time, larger amount of
filtrate, and a better wet and dry cake ratio than filter
aid 1#, though filter aid 1# also provides a good filtrate
quality. The filtrate quality from 3# meets the process
specification, which is selected as filter aid for filtration of the enzyme solution.

Total
Filter
filtration
aid
time/s

112

0.07

Figure 5

Table 3

1.87

Turbidity
/NTU

Results with different DE filter aids [17]


Total
amount of
filtrate/m3

Wet and
Specific cake
Turbidity
dry cake
resistance
/NTU
mass ratio
/mkg1

1#

532

4.3104

2.02

101

4.641011

3#

315

4.4104

1.87

114

1.821011

3.3.3 Filtration process optimization


Experiments to optimize filtration pressure and
filter aid dosage were conducted with 5104 m3 enzyme solution and filter aid 3# at different dosages and
different filtration pressure drop varying from 0.06
MPa (vacuum) to 0.2 MPa (pressure) for each test.
The results under different pressures are shown in Table 4 and the results with different filter aid dosages
are shown in Fig. 5.
Table 4 shows that within the testing pressure
range, for either vacuum filtration or pressure filtration, increase of pressure drop yields a faster filtration,
drier cake, but a higher specific cake resistance. In the
vacuum filtration, the total filtration time decreases

Filtration time vs. dosage (by mass)

significantly as pressure drop increases, while the


change of total filtration time is not so significant in
pressure filtration as pressure varies. The filtrate turbidity increases as pressure drop increases, which is
due to the bleeding of small particles at higher filtration pressure, especially during the initial bridging
period. Factors such as total filtration time or filtrate
flow rate, filtrate turbidity, and operation cost should
be considered to select an optimized filtration pressure.
Figure 5 shows the variation of total filtration
time at different filter aid dosages. When the dosage is
less than 2.5% , the total filtration time decreases as
dosage increases. When the dosage is higher than
2.5%, the filtration time is unfavorable. Excess addition of filter aid yields the formation of thick cake and
therefore high total cake resistance. An optimum filter
aid dosage needs to be determined based on filtration
tests and experience.
Based on the above experiments and analysis, it
can be concluded that DE filter aid 3# can assist the filtration of the chondroitin hydrolystates enzyme solution.
Evaluation on the specific cake resistance, total filtration time, and filtrate turbidity indicates that vacuum
filtration under 0.07 MPa and a dosage of 2.5% filter
aid 3# will yield a good filtration result, which has
been successfully applied to industrial production [18].
4 WOOD PULP FIBER PRECOAT FILTRATION FOR HIGHLY VISCOUS FLUID

Chemical fiber polymer melt contains gel like


materials and is highly viscous. The gel materials clog

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Chin. J. Chem. Eng., Vol. 19, No. 5, October 2011

the filter medium, and form a highly compactible and


highly resistant filter cake. A bypass flow may occur
in such highly resistant or impermeable cake, greatly
reducing the filtration efficiency. To improve the cake
structure and filtration, a wood pulp fiber material
with certain flexibility is selected to assist bridging
and precoat the filter medium, to prevent pore clogging in filter medium, increase cake porosity and improve cake filtration, and at the same time increase the
removal of small particles and rejection efficiency of
gel like material [14, 16, 19].
4.1

Morphology of wood pulp fiber

The wood pulp fiber in this study has a diameter


of 5-10 m and length of 800-1000 m. Its SEM
(scanning electron microscope) microscopy image is
shown in Fig. 6.

Figure 7 t/v vs. v linear plots of wood pulp fiber filter aid

Table 5 Specific cake resistance at varying wood pulp


fiber mass concentration and operating pressure
Pressure/MPa

Figure 6

SEM microscopy structure of wood pulp fiber

4.2 Operating pressure, wood pulp fiber concentration and specific cake resistance

Specific cake resistance109/mkg1


0.50%

0.75%

1.00%

1.25%

1.50%

0.10

2.299

1.499

1.038

0.869

0.719

0.15

2.710

1.555

1.207

1.087

0.855

0.20

2.917

1.886

1.407

1.190

1.044

0.25

3.058

1.898

1.486

1.312

1.101

0.30

3.233

2.310

1.625

1.384

1.151

In constant pressure filtration, the t/v vs. v is linear as shown in Fig. 7. The slop of straight line gives
the Ruth constant pressure filtration coefficient [Eq.
(10)]. Substituting K, p, and m to Eq. (11) , the specific cake resistance can be calculated.
Based on the experimental data, the specific cake
resistance at varying wood pulp fiber mass concentration (%) and operating pressure is shown in Table 5.
The specific cake resistance increases as pressure increases, but the rate of increase decreases gradually.
4.3

Cake compressibility coefficient n

Based on the specific resistance at different


pressures as listed in Table 5, the cake compressibility
coefficient n can be determined by plotting lgav against
lgp as given by Eq. (13). The enzyme solution plot at
1.0% (mass) concentration is shown in Fig. 8. The
cake compressibility coefficients for varying wood
pulp fiber concentration are listed in Table 6. The results

Figure 8

Plotting of lgav vs. lgp

Table 6 Cake compressibility coefficient


at different wood pulp concentration
mass concentration/%

0.50

0.75

1.00

1.25

1.50

compressibility coefficient n

0.32

0.38

0.41

0.42

0.45

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Chin. J. Chem. Eng., Vol. 19, No. 5, October 2011

Table 7

Filtrate flow rate vs. pressure and filter aid concentration


q/ms1

Pressure/MPa

0.50%

0.75%

1.00%

1.25%

1.50%

0.10

1.25

0.91

0.71

0.59

0.57

0.15

1.67

1.43

1.00

1.11

0.91

0.20

2.50

2.00

1.72

1.43

1.40

0.25

3.23

2.44

2.17

2.19

0.30

3.70

3.33

2.63

2.62

Table 8

Rejection efficiency with precoat of wood pulp fiber fine particles


Rejection efficiency of certain sized particles/%

Cake thickness
/mm

Pressure
/MPa

2 m

4 m

6 m

8 m

9 m

10 m

11 m

12 m

9.5

0.20

48.43

66.34

90.05

91.63

93.75

97.04

99.04

99.70

6.0

0.40

48.79

66.79

91.68

93.81

94.69

97.19

99.08

99.74

indicate that the wood pulp fiber filter aid particles are
soft and flexible and the cake compressibility coefficient varies with concentration in tested pressure
range. In the range from 0.5% to 1.5% range, the cake
compressibility coefficient of precoat increases with
feed slurry concentration. The increase at higher concentration is larger than that at lower concentration.
4.4 Effect of filtration pressure and filter aid concentration on filtrate flow rate

Table 7 shows the filtrate flow rate at different


filtration pressures and wood pulp fiber filter aid concentrations. The relationship of flow rate vs. filtration
pressure is linear at certain feeding slurry concentrations. The filtrate flow rate increases as filtration pressure increases and decreases as wood pulp fiber concentration increases.
4.5

Fine particle rejection efficiency

Fine particle rejection ratio or efficiency is an


important evaluation for the effectiveness of filtration.
Standard particles 5 m + 10 m are used to test the
rejection efficiency with wood pulp fiber precoat fine
particles [20, 21]. The efficiency is from the ratio of
total number of certain sized particles after and prior
to filtration. KT-2 particle counter is used to count the
total number of certain sized particles in feeding slurry
and in the filtrate. The precoat efficiency tests were
conducted under 0.02 and 0.40 MPa.
The data in Table 8 show that
(1) the larger the particles, the higher the rejection efficiency with the wood pulp fiber precoat;
(2) precoat under higher pressure presents a
higher rejection efficiency, which can be explained by
more compact cake indicated by lower cake thickness,
and therefore lower cake porosity at higher pressure;

(3) higher filtration pressure reduces cake thickness and increase particle rejection efficiency.
5

CONCLUSIONS

Rigid particulate filter aid diatomaceous earth 3#


is selected to assist the filtration of a biological health
product enzyme solution. The cake compressibility
coefficient of the DE filter aid is 0.15 in the range
from 0.015 to 0.09 MPa, which falls into the incompressible cake category. Optimized filter aid dosage
and filtration pressure are determined in the study. The
process has been successfully applied to industrial
filtration.
A flexible wood pulp fiber filter aid is selected
for filtration of highly viscous chemical fiber polymer
melt. Filtration tests show that the fiber filter aid is a
moderately compactible material with cake compressibility coefficient n = 0.46, and cake specific resistance av = (2.24-3.675)1011 mkg1 in the range
of 0.1-0.5 MPa. The tests to study the fiber filter aid
precoat filtration under operating conditions and rejection efficiency for precoat fine particles provides
important information for industrial process trial and
operation.
NOMENCLATURE
A
cg
Fs
K
Kp
L
m
p
pa

filtration area, m2
slurry concentration
the accumulated frictional stress on the network of solid particles
in the cake
permeability of cake dx, m2
cake permeability, m2
cake thickness, m
wet and dry cake rate
filtration applied pressure, Pa
empirical constant, Pa

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Chin. J. Chem. Eng., Vol. 19, No. 5, October 2011

pL
pm
ps
pc
Q
Rm
t
V
v
x

av
0
, , n
s

hydraulic pressure, Pa
liquid pressure required to overcome the medium resistance, Pa
efficient pressure, Pa
pressure drop across cake, Pa
filtrate flow rate, ms1
resistance of filter media, m1
filtration time, s
volume of filtrate, m3
volume of filtrate per unit area, m3/m2
distance from medium, m
specific cake resistance of cake d, mkg1
average specific cake resistance, mkg1
specific cake resistance under unit pressure, mkg1
cake compressibility coefficients
cake solid content ratio
filtrate density , kgm3
viscosity of filtrate, Pas
volume of solids per unit filter area in distance 0 to x, Fig. 1
volume of cake per unit area, m

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