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Lars Steinke1 Siegfried Ripperger1

1

Research Article

Lehrstuhl fr Mechanische Verfahrenstechnik, Technische Universitt Kaiserslautern, Germany.

Classification of Suspensions by Means of Rotating Filter Discs and Autodynamic High-Frequency Backwashing
A new method for the classification of suspensions by means of rotating filter discs is presented. The classification without a filter cake buildup by means of a single shaft disc filter is possible using the high-frequency autodynamic backwashing method. High-frequency autodynamic backwashing results from an overpressure fluctuation between the filtrate and concentrate sides, resulting in different flow directions of the filtrate volume flow. The main parameters are the centrifugal force acting on the fluid inside the discs in combination with the fact that the discs are slightly inclined. It is demonstrated that the separation of coarse particles is entirely possible.
Keywords: Autodynamic backwashing, Classification, Filtration, Suspensions Received: March 29, 2010; revised: May 31, 2010; accepted: June 7, 2010 DOI: 10.1002/ceat.201000150

Introduction

The separation of coarse particle fractions from suspensions of nanoscale particles (particle size < 500 nm) is of great significance for a number of products and processes. The powders and dispersions that are most frequently in demand are those in which the particle spectrum has a sharp distribution that is clearly set under 500 nm. Such disperse systems are used, for example, as polishing and CMP (chemical-mechanical polishing) slurries, as pigments and as additives for nanocomposites. In all these applications, it is important that the products are free of coarse particles. Even slight traces of coarse particles cause scratches during the CMP process and may also cause a decreased yield in recyclable microchips. Coarse particles in pigments cause visual imperfections in paint layers. The presence of coarse particles in nanocomposites results in weak points, which can result in the failure of entire components. Therefore, there is a need for classification procedures that can reliably remove the less coarse particles from a suspension of nanoparticles. Coarse particles in corresponding material systems often arise through a possible, yet unwanted agglomerate formation. For this reason, it is advantageous to destroy corresponding agglomerates, e.g., by dispersion, or to remove them from the product by means of a classification procedure, e.g., by a classi-

Correspondence: Dipl.-Ing. L. Steinke (steinke@mv.uni-kl.de), Lehrstuhl fr Mechanische Verfahrenstechnik, Technische Universitt Kaiserslautern, Gottlieb-Daimler-Strae 44/456, D-67663 Kaiserslautern, Germany.

fying filtration. It is particularly advantageous to directly connect the classification with dispersion, e.g., deflector wheel classifiers. However, the latter systems are discharged with an air flow that involves a relatively low solid matter load. At high solid matter concentrations (> 2 vol.-%), depth filters with fiber-formed filter media are almost exclusively used for classification filtration in the fluid phase. Corresponding filters are used during the CMP process with a nominal separating limit of 510 lm, both in the main rings and at the point of use. Operating results have shown that the number of coarse particles can be reduced with this filter, but that it is not possible to completely remove coarse particles. Thus, for example, particles with a size of up to 7 lm have also been located behind filters with a nominal cutoff size of 3 lm [1]. The reason for this could be that the particles in the filters are deposited at preferred sites and form agglomerates there. It is known that the flow velocity can be locally increased in the pore system of the filter when there is an increase in the filter resistance as a result of the increase in dirt load, whereby, on the other hand, particles can be removed and flooded out. The classifying filtration can also be attained with screens. It is advantageous when the screen is overflowed during this process. Wignjosaputro [2] has investigated the use of bow screens with a mesh size of 500 lm for the classification of suspensions of glass spheres. Bott et al. [3] reported on screen classification using a dynamic filter (DYNO filter) with fixed screens, which were overflowed through the effect of impellers. Thus, separation sections of up to a minimum coarse particle size of 20 lm were attained. Taamneh et al. [4] have investigated the use of disc filters with overlapping and non-overlapping rotating screen discs

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with a separating limit in the region Lift Force pConcentate of 10 lm. It was possible to show that the shear gap with an overlapDrag Force Diffusion ping of the rotating discs could efCentrifugal Force pCentrifugal Force fectively prevent the formation of a filter cake and that, through this mode, a classification with a sepaFilter Surface rating limit in the area of the mesh size of the screen was made possible. On the other hand, when operHollow Shaft ating without a shear gap, particles were seen to deposit on the rotating discs, forming a covering layer that 1 p F ( r ) = F r 2 2 + p F hinders the classification. 2 A particle deposit on the discs, Filtrate as well as bridge formation and the subsequent cake formation assoFigure 1. Schematic representation of the forces that affect the particles close to the filter surface ciated with it should be prevented and the pressure conditions on the disc. with screen classification. During the course of the present research, rapidly rotating discs. Baffles and other flow hindrances in the screen classification of suspensions by means of single axis, the outer area of the discs ensure that the largest possible relarotating disc filters was investigated. During this work, autodytive velocity is set up between the fluid and the discs and that namic pressure fluctuation, which effectively suppresses partithe effect of the centrifugal force is decreased. On the inside of cle deposit on the screen discs was discovered and is further the discs, one can assume that the fluid rotates at the peripherdeveloped as a new mechanism. al speed of the discs, so that one can assume a rigid body vortex. From this, the profile of the radial pressure course in the 2 Theory disc hinted at in Fig. 1 arises, which must be taken into consideration in the following observations.
korr

2.1

Force Effects on the Particles

Disc filters with rotating filter discs are used, among other reasons, because of the various forces affecting the particles. They are intended to try and ensure that the particles are constantly moved and do not form deposits on the discs. The particles near the disc surface and the relevant forces are shown in Fig. 1. The drag force (resistance force) has an effect parallel to the direction of movement. The buoyancy force, or compressive force, results from the difference between the density of the particles and of the fluid in the suspension. The lift force (dynamic buoyancy) is caused by a shear flow. When the fluid flowing around the particles shows a higher velocity on the top side of the particle than on the bottom side, it follows that there is a slighter pressure on the former side. Therefore, a particle is moved away from the wall in a flow near the wall. This effect has been thoroughly investigated by other researchers [58]. The ratio of dynamic buoyancy force to drag force vertical to the surface of a filter medium is of special significance for the deposit condition of the particles. A particle is not deposited if the buoyancy force is greater than the resistance force through the permeate flow. The buoyancy force is itself dependent on the particle size, whereby a greater buoyancy force has an effect on larger particles.

Experimental

3.1 Test Facility

The tests were carried out with a single-shaft disc filter (model designation: SSDF) from Novoflow GmbH. The filter consists of a vertical hollow shaft upon which a maximum of 8 filter discs with a maximum diameter of dS = 300 mm can be mounted1). The filter discs are covered with a filter medium on both sides. The filter surface area is ca. 1 m2. The tests were carried out using discs with a twilled dutch weave fabric with a 2/2 twill weave out of stainless steel DIN 1.4301/AISI 304. The nominal separating limit of the fabric is dP = 10 lm (165 1400 mesh, 1618 lm absolute). By means of a patented procedure (Novoflow GmbH), the filter media are placed on a coarser backing fabric and fixed onto the edge with a plastic edging. Using this procedure, it is possible to equip discs with different filter media. The open facility with the built-in discs is shown in Fig. 2. The suspension is led into the storage tank with the rotating discs, starting from another storage tank, by means of a centrifugal pump under pressure from a vertical inlet located underneath. The suspension with the coarse particles leaves the container above the middle part of the tank and flows back into

2.2

Force Effect on the Fluid

The force effect on the fluid as a result of the rotary motion must also be taken into consideration with disc filters with

1) List of symbols at the end of the paper.

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3.2 Test Particle System

The following test particle system was selected: Al2O3/MgO (70/30) (IK Hochrhein GmbH, mean particle size ca. 8 lm). The results in Fig. 4 show the particle size distribution of this material system. The particle size distribution was selected so as to investigate a separation of a coarse particle fraction with the chosen screen fabric.

3.3
Figure 2. Arrangement of the filter discs in the SSD filter.

Measuring Technology

the storage tank. The storage tank has an agitator that can be regulated in its rotational speed by means of a frequency transformer. Thus, sedimentation of the particles in the storage tank can be prevented. The tank is equipped with a double housing, a heat exchanger and a separate circulation pump. Therefore, the suspension can be maintained at a constant temperature since a stable temperature is especially important to maintain the viscosity of the suspension. The average shear stress affecting the filter surfaces of the discs can be determined by means of a measurement of the torque of the wave with the discs. Flow meters were implemented for the suspension with the coarse particles (retentate) and the suspension with the fine particles (permeate), as well as pressure sensors in the tank, in the filtrate and a rotational speed sensor. A detailed sketch of the setup used for the measurements is shown in Fig. 3.

The particle counter, AccuSizer 780 SIS (Particle Sizing Systems), was used for the investigation of the classification. The particle size measuring range extends from 500 nm to 500 lm. The area of concentration is limited to a maximum of 7500 9000 particles/mL. The extracted samples were appropriately diluted before measurement. The special advantages of a particle counter are that coarse particles can also be recorded with certainty in the smallest amounts of sample. The functional ability of the measurement technology was tested and ensured by means of a Latex standard.

4
4.1

Results
Classification by Means of Autodynamic Pressure Fluctuation

An effect that was surprisingly discovered during the course of the investigations was classification by means of autodynamic

FQIR

Sampling Concentrate

SSD-Filter

PIR

Storage Tank
QIR**

TI

FQIR

QIR*

PIR

Filtrate
* ** Conductivity Torque

Figure 3. Detailed schematic of the device used for the measurements.

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Figure 4. Particle size distribution of the Al2O3/MgO (70/30) test particle system, IK Hochrhein GmbH (measuring device: ANALYSETTE 22 NanoTec, Fritsch GmbH).

high-frequency backwashing. By using the SSD filter, it was possible to reduce the filter cake build-up with increasing rotational speed, but a classification completely free of particle coverage was not yet possible. Through skilled parameter selection, it was possible to show that strong pressure and slight volume flow fluctuations occur in the facility. The fluctuations lead to a high-frequency backwashing of the fabric, whereby filter cake build-up was prevented and a high, constant filter volume flow could be guaranteed. The new procedure is being introduced under the term autodynamic high-frequency backwashing. In the following section, a series of tests will be introduced in which classification without a covering layer was achieved by means of autodynamic high-frequency backwashing, and in which a constant volume flow could be ensured. Suspensions with concentrations of c = 1 g/L and 10 g/L were examined. The rotational speed was set at 200 min1 and 600 min1 respectively. In addition to the determination of the pressure conditions and volume flows, the particle size distribution in the concentrate and in the filtrate was examined. The data in Fig. 5 shows the course of the filtrate volume flows at a concentration of c = 10 g/L for different rotational speeds, n. At n = 200 min1, the filtrate volume flow drops from ca. 2300 L/m2h to ca. 570 L/m2h at the end of the test. The volume flow drops more than during the tests carried out at a concentration of 1 g/L, which is due to an increased filter cake build-up. In Fig. 6, the discs are shown with the filter cake after the end of the test at n = 200 min1 and c = 10 g/L. One can recognize detachment of the filter cake and cake-free areas on the filter surface. In the outer area of the disc, there was a turbulent flow during the classification that led to the removal of the filter cake.

Fluctuations in the filtrate volume flow can be observed at n = 600 min1. The mean value of the fluctuations is 1820 L/m2h with a standard deviation of r = 213 L/m2h. The minimal measured filtrate volume flow is 750 L/m2h and the highest filtrate volume flow is 2304 L/m2h. One could not observe a drop in the mean filtrate volume flow, which indicates a filter-cake-free classification. No filter cake could be established on the disc after the end of the test. The differential pressure between the concentrate side and the filtrate side was Dp = 0.7 bar during operation. At a rotational speed of n = 600 min1, there were fluctuations in the pressure range from Dp = 0.60.8 bar, while the pressure at n = 200 min1 remained almost constant. Only a few particles in the classes x = 7 lm and x = 11 lm could be established in the filtrate when there was a covering layer build-up after a test duration of t = 90 min above x = 4 lm. However, the number of these particles was so small that no unequivocal statement can be made as regards the accuracy of measurement. The shift of the separation limit to x = 4 lm is due to the influence of the covering layer. The numerical concentrations of the particles in the filtrate for t = 5, 10, 60 and 90 min at c = 1 g/L and n = 600 min1 (no filter cake build-up) are shown in Fig. 7. The maximum possible dissolution of the particle counter (512 particle classes) was utilized for this investigation. It can be seen that the particle spectrum in the filtrate shifts to the fine particle portion as the test duration increases, while the concentration drops. The decrease in concentration may be due to particle deposits on the inside of the discs. It is possible, due to centrifugal forces, that particles on the inside of the discs are pressed towards the outside and removed from the system.

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3000

2500

n = 600 min

-1

2000 V / Lm-2h-1

1500

1000

500
n = 200 min
-1

0 0 10 20 30 40 t / min 50 60 70 80 90

Figure 5. Filtrate volume flows at different rotational speeds, c = 10 g/L.

Figure 6. Filter cake build-up (topmost filter disc) after t = 90 min, c = 10 g/L, n = 200 min1.

The data in Fig. 7 shows the measured particle concentrations in the filtrate following operating times of t = 5, 15 and 90 min at a suspension concentration of c = 1 g/L and a rotational speed of n = 600 min1 (no filter cake build-up). It can be seen, even after 15 min, that only very few particles of over 20 lm can be found in the filtrate. It can also be observed that the particle concentration decreases with increasing test duration. This effect is due to particle deposition on the inside of the disc. No further particles above a particle size of x = 20 lm can be found in the filtrate after t = 90 min. The result shows that a reliable separation of coarse particles (x > 20 lm, absolute separation limit of the filter medium: 18 lm) is possible with the tested procedure under the given conditions. In addition to the tests with Al2O3/MgO (70/30), extensive tests were carried out with titanium dioxide (2305, Kronos Int., Inc., mean particle size ca. 280 nm) as a model substance.

The particle size distribution was selected in order to investigate the influence of the classification on a highly concentrated suspension by means of the corresponding screen fabric with which the larger portion was to be strained as fine particles. This material system serves as a model suspension for a CMP slurry. A classification by means of high-frequency autodynamic backwashing was also possible with the titanium dioxide material system at concentrations of up to 30 g/L. A classification free of filter cake by means of titanium dioxide was not possible. At high rotational speeds of n = 600 min1, the cake could be minimized, but a slight build-up of a covering layer could not be avoided. The overall results lead to the following summary: I. A classification free of a covering layer by means of the SSD filter is possible at high rotational speeds (n = 600 min1). The effect is due to the high-frequency autodynamic backwashing, the background of which will be explained in the next section. II. The separation of coarse particles is entirely possible. In this regard, one must take into consideration that the pore width of dP = 10 lm represents a nominal separation limit since the absolute filter particle size is 18 lm maximum.

4.2

Origin of the Autodynamic Pressure Fluctuation

The data in Fig. 8 shows the pressure conditions of filtrate and concentrate at different rotational speeds, n, with pure water. The fluctuations in the pressure appear at a rotational speed of n = 400 and 600 min1. To clarify the cause of the fluctuations, the radial pressure increase in the interior of the filter disc due

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Figure 7. Numerical concentration of the particles in the filtrate for t = 590 min, c = 1 g/L, n = 600 min1 (no filter cake build-up).

to the centrifugal force has been considered, as schematically represented in Fig. 1. The filtrate pressure has been corrected by the influence of this pressure gradient. In so doing, it was assumed that a rotation of the fluid in the same direction through

the baffles in the outer area of the disc was suppressed for the most part. The results in Fig. 8 show the measured pressure in the outer area of the disc and the pressure expansion by the centrifugal portion for two radii in the interior of the disc.

n = 600 min-1 n = 0 min-1 n = 200 min-1 n = 400 min-1

Figure 8. Dependence of the corrected filtrate pressures (considering the pressure gradients resulting from the centrifugal force) on the rotational speed at different filter disc radii compared to the measured pressure in the filter housings.

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From Fig. 8, one can recognize that the corrected filtrate pressure at a radius of r = 50 mm for the entire test duration lies below the pressure in the outer area of the disc, i.e., the tank pressure, pK. At a radius of r = 150 mm, the corrected filtrate pressure at a rotational speed of n = 400 min1 lies slightly below the pressure pK in the outer area of the disc and at n = 600 min1 it is of the same magnitude as the tank pressure, pK. The results in Fig. 9 show a comparison of the corrected filtrate pressure, pF,korr., with the pressure on the concentrate side, pK, as a differential pressure, Dpkorr. = pK pF,korr. The differential pressure is positive at n = 0 and 200 min1, which means that the pressure is constantly higher than in the filtrate in the outer area of the disc. At n = 400 min1, the differential pressure fluctuates slightly above p = 0 bar and at n = 600 min1, the differential pressure is in the range from ca. +0.1 bar to ca. 0.8 bar. The overpressure fluctuates between the filtrate and concentrate sides, resulting in different flow directions of the filtrate volume flow. Therefore, a high-frequency periodic backwashing is set up through the rapid changes in pressure conditions. In order to determine the validity of the statements made, the pressure in the facility was increased to the extent that the pressure pK in the tank was constantly above the pressure inside the filter discs. It was possible to prevent pressure fluctuations in this way. The facility had to be rebuilt for this test procedure. The number of filter discs was reduced to 2, since the corresponding pressures could not be set up with closed concentrate effluent and at full pump efficiency. The data in Fig. 10 show the results of this investigation. It can be clearly recognized that there are no fluctuations at increased pressure. The counter-sample with this facility setup has shown that the

fluctuations can be reproduced when the pressure is correspondingly reduced. A further condition that contributes to fluctuation, assuming suitable pressure conditions, is the fact that the discs opposite the hollow shaft on which they are mounted reveal a slight incline. In the tests investigated, the corresponding angle of inclination was ca. 1. A schematic representation of the test structure is shown in Fig. 11. When the disc rotates at an angle of inclination, this causes a fluctuating movement that leads to the pressure fluctuations shown in Fig. 9. The incline of the filter discs will be investigated in further studies. In addition, the influence of other parameters, such as the concentration of the suspension and/ or its viscosity, will be further examined.

Conclusions

Autodynamic high-frequency backwashing has been introduced here as a new procedure for the dynamic classification of suspensions. The rotational velocity has an influence on the pressure on the inside of the disc. By adjusting the rotational velocity, the connection of the differential pressure between the outer disc area and the disc interior with the inclined position of the filter discs can be set up so that a periodic backwashing of the filter media takes place. It was possible to attain a classification free of any covering layer with the SSD filter from the firm Novoflow GmbH by means of autodynamic high-frequency backwashing. The separation of coarse particles was shown to be entirely possible.

Figure 9. Differential pressure on the outside edge of the filter disc.

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n = 0 min

-1

n = 200 min

-1

n = 400 min

-1

n = 600 min

-1

Figure 10. Elimination of the fluctuations by increasing the differential pressure between the concentrate and the filtrate.

Outlet Filterdisc Quill Shaft

pK pZ

[bar] [bar]

Dp Dpkorr.
Flowbreaker

[bar] [bar] [%] [mm] [min] [lm]

dq3 R T x

pressure in the outer area of the disc (tank pressure) pressure resulting from the influence of the centrifugal force on the fluid differential pressure corrected differential pressure (calculated by means of pFkorr.) sum distribution (differential) radius time particle size

Filterhousing

Greek symbols qf x [kg/m3] [min1] density of the fluid annular velocity

Permeate

Inlet

Figure 11. Schematic representation of the disc inclines in the filter housing.

References
[1] T. Kuntzsch, et al., Ind. Chem. Eng. Technol. 2003, 26 (12), 1235. [2] A. Wignjosaputro, VDI Prog. Rep. 1985, Series 3, No. 106. [3] R. Bott, Th. Langeloh, E. Ehrfeld, Filtr. Separ. 2002, 16 (2), 58. [4] Y. Taamneh, L. Steinke, S. Ripperger, Chem. Eng. Technol. 2008, 31 (7), 1035. [5] P. G. Saffmann, J. Fluid Mech. 1971, 22, 385. [6] D. Hall, J. Fluid Mech. 1988, 187, 451. [7] J. B. McLaughlin, J. Fluid Mech. 1993, 246, 249. [8] H. Nirschl, GVC Annual Meeting, Strasbourg, September 1995.

Symbols used
C dP dS n p pF pF,korr. [g/L] [lm] [mm] [min1] [bar] [bar] [bar] concentration pore size (nominal) diameter of the discs rotational velocity pressure pressure on the filtrate side corrected filtrate pressure (by considering pZ)

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