US20070202030A1 - Hydrophobic silica - Google Patents

Hydrophobic silica Download PDF

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Publication number
US20070202030A1
US20070202030A1 US11/741,381 US74138107A US2007202030A1 US 20070202030 A1 US20070202030 A1 US 20070202030A1 US 74138107 A US74138107 A US 74138107A US 2007202030 A1 US2007202030 A1 US 2007202030A1
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Prior art keywords
silica
effectiveness
hydrophobic
compacted
pyrogenically produced
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US11/741,381
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Gunther Michael
Volker Kasack
Rudiger Nowak
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Evonik Operations GmbH
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Gunther Michael
Volker Kasack
Rudiger Nowak
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Priority claimed from DE1999161933 external-priority patent/DE19961933A1/en
Application filed by Gunther Michael, Volker Kasack, Rudiger Nowak filed Critical Gunther Michael
Priority to US11/741,381 priority Critical patent/US20070202030A1/en
Publication of US20070202030A1 publication Critical patent/US20070202030A1/en
Assigned to EVONIK DEGUSSA GMBH reassignment EVONIK DEGUSSA GMBH CHANGE ADDRESS Assignors: EVONIK DEGUSSA GMBH
Assigned to DEGUSSA GMBH reassignment DEGUSSA GMBH CHANGE OF ENTITY Assignors: DEGUSSA AG
Assigned to EVONIK DEGUSSA GMBH reassignment EVONIK DEGUSSA GMBH CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: DEGUSSA GMBH
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3009—Physical treatment, e.g. grinding; treatment with ultrasonic vibrations
    • C09C1/3036—Agglomeration, granulation, pelleting
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3081—Treatment with organo-silicon compounds
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3684—Treatment with organo-silicon compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/10—Solid density
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/11—Powder tap density
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/20—Powder free flowing behaviour
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/90—Other properties not specified above
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
    • Y10T428/2995—Silane, siloxane or silicone coating

Definitions

  • This invention relates to a hydrophobic, pyrogenically produced silica, to a process for the production thereof and to the use thereof.
  • the tamped density is preferably from 60 to 200 g/l.
  • a feature of the present invention is a process for the production of the hydrophobic, pyrogenically produced silica having a bulk density of 55 to 200 g/l, which process is characterised in that pyrogenically produced silica is hydrophobized using known methods and then compacted.
  • Hydrophobing can preferably be performed by means of halogen-free silanes.
  • the chloride content of the silica can be less than or equal to 100 ppm, preferably from 10 to 100 ppm.
  • Compaction can be performed by means of a roller compactor.
  • Compaction can preferably be performed by means of a belt filter press according to EP 0 280 851 B1, which reference is relied on and incorporated by reference.
  • hydrophobic, pyrogenically produced silica used for purposes of the present invention can be, for example, the silicas known as:
  • Aerosil R 812 or Aerosil R 812S having the group -0-Si (CH 3 ) 3
  • Aerosil R 202 Aerosil MS 202, Aerosil MS 202, Aerosil R 106
  • Aerosil R 104 having the group Aerosil R 805 having the group
  • hydrophobic, pyrogenic silica according to the invention having a tamped density of 55 to 200 g/l exhibits the following advantages:
  • Transport costs are distinctly lower as a result of the higher tamped density.
  • the silica according to the invention is in the form of relatively small aggregates.
  • the dispersions are more finely divided because the silica according to the invention is more readily dispersible.
  • the dispersions produced using the silica according to the invention exhibit a lower Grindometer value.
  • Dispersions containing the silicas according to the invention exhibit distinctly increased stability because the tendency towards settling is distinctly lower.
  • silica according to the invention is reduced dustings during incorporation and the distinctly reduced incorporation or wetting time in, for example, liquid systems.
  • hydrophobicity of the silica according to the invention is unchanged. Thickening action is also unchanged.
  • CF silica compacted with a Carter filter
  • VV 60 silica compacted to a tamped density of approx. 60 g/l
  • VV 90 silica compacted to a tamped density of approx. 90 g/l
  • Aerosil grades R 202, US 202, US 204, R 812, R 812S and R 805 are investigated. The results are shown in Table 1.
  • US 202 and US 204 have very comparable rheological properties and are inferior to AEROSIL R 202.
  • the compacted variants in particular of R 812, R 202 and US 202/4, exhibit an incorporation time reduced by up to half.
  • the compacted silicas moreover exhibit reduced dusting.
  • 444701 444702 444703 444704 444705 444706 AER202 AER202 AER2O2 AER302 AER805 AER805 PA Test method CF CF VV60 VV90 bulk CF 0330 Viscosity, epoxy before cure 459 456 382 430 190 181 0335 Viscosity, epoxy after cure 54.4 54.7 49.4 52.8 42 41.7 0340 Thickening action 0410 Grindometer value 0420 Methanol wetability 0701 Tamped density 45 50 51 75 44 62 0920 Agglomerate strength 11 20 18 15 0930 Hands
  • Thixotroping agent R 202 and R 812 Additive: Storage time 5 rpm 50 rpm in days [mPa * s] [mPa * s] T.I.
  • Sample A R 812 10 kg 2-10123
  • Sample production date: 24.02.1994 Spindle: 5 0 16600 4460 3.72 80-85 ⁇
  • Sample A R 812 15 kg 1.0/8 min
  • Sample production date: 24.02.1994 Spindle: 5 0 15100 4060 3.72 50-60 ⁇
  • Sample production date: 24.02.1994 Spindle: 5 0 15100 4020 3.73 50-60 ⁇
  • Compaction may amount to a type of predispersion. Accordingly, effectiveness values rise with tamped density. i.e. the particles effectively present in the ethanol dispersion become smaller and the compacted samples exhibit distinctly less settling. Any suitable organic solvent can be used to form the dispersion.
  • Compaction has no influence on hydrophobicity, which in each case substantially corresponds to that of the standard sample.
  • the compacted AEROSIL R 202 samples behave in a similar manner to the compacted AEROSIL R 812 samples.
  • the parameter of “effectiveness” reported in the tables herein relates to the high degree of fineness of the particle. This is therefore an indicator of high transparency and good stability of the resulting dispersions.
  • German priority application filed Dec. 22, 2000 199 61 933.6 is relied on and incorporated herein by reference.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

Hydrophobic, pyrogenically produced silica having a tamped density of 55 to 200 g/l is produced by hydrophobizing pyrogenically produced silica and then compacting it. The silica may be used for the production of dispersions.

Description

    REFERENCE TO A RELATED APPLICATION
  • This application claims the benefit of provisional application 60/171.667 filed Dec. 27, 1999 which is relied on and incorporated by reference.
    • INTRODUCTION AND BACKGROUND
  • This invention relates to a hydrophobic, pyrogenically produced silica, to a process for the production thereof and to the use thereof.
  • It is known to compact hydrophilic, pyrogenically produced silica (EP 0 280 854 B1). Disadvantageously, as tamped or bulk density increases, thickening action declines in a linear manner. Dispersibility also falls as density increases. This results in unwanted speckling. Thus, once compacted, a hydrophilic, pyrogenically produced silica may only be used for a limited number of applications.
  • It is therefore an object of the present invention to avoid the problems of compacted, hydrophobic, pyrogenically produced silica of the past.
    • SUMMARY OF THE INVENTION
  • The above and other objects of the present invention can be achieved by developing a hydrophobic, pyrogenically produced silica having a tamped density of 55 to 200 g/l.
  • The tamped density is preferably from 60 to 200 g/l.
  • A feature of the present invention is a process for the production of the hydrophobic, pyrogenically produced silica having a bulk density of 55 to 200 g/l, which process is characterised in that pyrogenically produced silica is hydrophobized using known methods and then compacted.
  • Hydrophobing can preferably be performed by means of halogen-free silanes. The chloride content of the silica can be less than or equal to 100 ppm, preferably from 10 to 100 ppm.
  • Compaction can be performed by means of a roller compactor. Compaction can preferably be performed by means of a belt filter press according to EP 0 280 851 B1, which reference is relied on and incorporated by reference.
  • The hydrophobic, pyrogenically produced silica used for purposes of the present invention can be, for example, the silicas known as:
  • Aerosil R 812 or Aerosil R 812S, having the group -0-Si (CH3)3
  • Aerosil R 202, Aerosil MS 202, Aerosil MS 202, Aerosil R 106
  • or Aerosil R 104 having the group
    Figure US20070202030A1-20070830-C00001
    Aerosil R 805 having the group
  • These are commercially available products from Degussa Hüls AG.
  • The hydrophobic, pyrogenic silica according to the invention having a tamped density of 55 to 200 g/l exhibits the following advantages:
  • Transport costs are distinctly lower as a result of the higher tamped density.
  • Once dispersed, the silica according to the invention is in the form of relatively small aggregates.
  • In other words, the dispersions are more finely divided because the silica according to the invention is more readily dispersible.
  • The dispersions produced using the silica according to the invention exhibit a lower Grindometer value.
  • Both UV transmission transparency and visual transparency of the dispersions are distinctly improved by using the silica according to the invention.
  • Dispersions containing the silicas according to the invention exhibit distinctly increased stability because the tendency towards settling is distinctly lower.
  • Another advantage of the silica according to the invention is reduced dustings during incorporation and the distinctly reduced incorporation or wetting time in, for example, liquid systems.
  • In comparison with hydrophobic, pyrogenic silica of a lower bulk density, the hydrophobicity of the silica according to the invention is unchanged. Thickening action is also unchanged.
    • DETAILED DESCRIPTION OF THE INVENTION
  • The present invention will be farther understood with reference to the following detailed embodiments thereof.
    • Example 1
  • Various hydrophobic, pyrogenically produced silicas are investigated, wherein different compaction states are compared.
  • The following definitions apply:
  • bulk=pulverulent, unmodified silica
  • CF=silica compacted with a Carter filter
  • VV 60=silica compacted to a tamped density of approx. 60 g/l
  • VV 90=silica compacted to a tamped density of approx. 90 g/l
  • Aerosil grades R 202, US 202, US 204, R 812, R 812S and R 805 are investigated. The results are shown in Table 1.
  • As evaluated by the Corning Glass methanol wettability method, the degree of compaction has virtually no appreciable influence on hydrophobicity. Viscosity also exhibits no clear systematic dependency upon tamped density. Especially for R 812, dispersibility improves with increasing density. R 812 S, which contains more SiOH groups than R 812, exhibits the above phenomenon less markedly.
  • US 202 and US 204 have very comparable rheological properties and are inferior to AEROSIL R 202.
  • Surprisingly, the compacted variants, in particular of R 812, R 202 and US 202/4, exhibit an incorporation time reduced by up to half. The compacted silicas moreover exhibit reduced dusting.
    444701 444702 444703 444704 444705 444706
    AER202 AER202 AER2O2 AER302 AER805 AER805
    PA Test method CF CF VV60 VV90 bulk CF
    0330 Viscosity, epoxy before cure 459 456 382 430 190 181
    0335 Viscosity, epoxy after cure 54.4 54.7 49.4 52.8 42 41.7
    0340 Thickening action
    0410 Grindometer value
    0420 Methanol wetability
    0701 Tamped density 45 50 51 75 44 62
    0920 Agglomerate strength 11 20 18 15
    0930 Hands|sic|sieve oversize 0 24 4 27 0 36
    0955 Effectiveness 258 274 203 266 235 260
    0965 Effectiveness (UT) 280 290 226 295 271 281
    0975 Settling (effectiveness) 15 15 15 8 10 15
    444707 444708 444709 444710 444711
    AER805 AER805 AER812 AER812 AER812
    PA Test method VV60 VV90 bulk CF VV60
    0330 Viscosity, epoxy before cure 185 178
    0335 Viscosity, epoxy after cure 39 43
    0340 Thickening action 11.7 13.3 11.5
    0410 Grindometer value 127 102 92
    0420 Methanol wetability
    0701 Tamped density 55 68 45 44 50
    0920 Agglomerate strength 15 20
    0930 Hands|sic|sieve oversize 7 19 0 0
    0955 Effectiveness 236 258 166 185 169
    0965 Effectiveness (UT) 270 288 197 213 209
    0975 Settling (effectiveness) 10 5 13 15 8
    444712 444713 444714 444715 444716 444717
    AER812 AER812S AER812S AER812S AER812S US202
    PA Test method VV90 bulk CF VV60 VV90 bulk
    0330 Viscosity, epoxy before core 350.4
    0335 Viscosity, epoxy after core 50.7
    0340 Thickening action 11.1 17.3 17.3 18.2 17
    0410 Grind meter value 77 93 110 110 100
    0420 Methanol wetability
    0701 Tamped density 73 49 50 58 75 39
    0920 Agglemerate strength 22 28
    0930 Hands/sie/sieve oversize 12 0 0 0 4 0
    0955 Effectiveness 159 168 169 187 209 320
    0965 Effectiveness (UT) 225 201 200 216 235 336
    0975 Settling (effectiveness) 5 8 8 3 0 15
    444718 444719 444720 444721 444722 444723
    US202 US202 US204 US204 US204 US204
    PA Test method CF VV60 bulk CF VV60 VV90
    0330 Viscosity, epoxy before core 377.6 380.8 379.2 350.4 358.4 368
    0335 Viscosity, epoxy after core 45.9 45.3 49.9 47 52.6 50.7
    0340 Thickening action
    0410 Grind meter value
    0420 Methanol wetability
    0701 Tamped density 50 67 44 45 57 71
    0920 Agglemerate strength 10 15 16 23
    0930 Hands/sie/sieve oversize 27 36 0 0 3 20
    0955 Effectiveness 304 320 186 193 192 201
    0965 Effectiveness (UT) 327 346 223 225 225 230
    0975 Settling (effectiveness) 10 3 10 10 10 10
    • Example 2
  • Investigation of the Influence of Higher Compaction on Applicational Properties
    AE R 812, AE R 812,
    AE R 812, compacted compacted
    uncom- RHE RHE
    pacted UB 3847-2 UB 3847-3
    UB 3847-1 (4) (5) AE R 812
    10 kg 15 kg 20 kg RHE
    sack sack sack specific.
    Tamped density g/l 50 87 106 approx.
    (DIN ISO 787/11) 50
    Effectiveness, 184 214 209 216  1)
    ethanol (0955)
    Effectiveness (UT), 218 260 290 236  1)
    ethanol (0965)
    Settling vol. % 10 1 1   1)
    (effectiveness,
    high-speed
    mixer)

    1. Determined on standard sample (UB 3391)

    RHE in the above table indicates the Rheinfelden plant located in Germany.

    Rheological Testing:
    Polymer: Araldit M (biphenol-1-expoxy resin by Ciba-Geogy, in the form of clear yellow liquid).
  • Thixotroping agent: R 202 and R 812 Additive:
    Storage time 5 rpm 50 rpm
    in days [mPa * s] [mPa * s] T.I.
    Sample A R 812 10 kg 2-10123
    Sample production date: 24.02.1994   Spindle: 5
    0 16600 4460 3.72
    80-85 μ
    Sample A R 812 15 kg 1.0/8 min
    Sample production date: 24.02.1994   Spindle: 5
    0 15100 4060 3.72
    50-60 μ
    Sample A R 812 20 kg 0.6/14 min
    Sample production date: 24.02.1994   Spindle: 5
    0 15100 4020 3.73
    50-60 μ
  • Compaction may amount to a type of predispersion. Accordingly, effectiveness values rise with tamped density. i.e. the particles effectively present in the ethanol dispersion become smaller and the compacted samples exhibit distinctly less settling. Any suitable organic solvent can be used to form the dispersion.
  • The compacted samples accordingly have a more favourable Grindometer value in Araldit. However, since the larger particles have a decisive influence on thickening action, the property declines slightly on compaction.
  • It may be seen from the graph of effectiveness values that, while the highly compacted AEROSIL R 812 sample may indeed still be broken up with the Ultra-Turrax mixer (0965), it can no longer be broken up with the high speed mixer (0955). Due to the smaller surface area of AEROSIL R 202 (and to the consequently theoretically improved dispersibility), this phenomenon hardly occurs with AEROSIL R 202.
  • As compaction rises, the particles effectively present in an ethanol dispersion thus become smaller and 90° angle scattering rises due to Rayleigh scattering. Total scattering (over all angles), however, falls and the samples become distinctly more transparent on visual inspection, as is also substantiated by the UV transmission spectra.
  • Compaction has no influence on hydrophobicity, which in each case substantially corresponds to that of the standard sample.
    • Example 3
  • Investigation of the Influence of Higher Compaction on Applicational Properties.
    AE R 812, AE R 202, AE R 202,
    uncom- compacted compacted
    pacted RHE RHE
    UB 3848-1 UB 3848-2 UB 3848-3
    2-02024 2-01024- 2-01024- AE R 202
    10 kg (2) (3) RHE
    sack 15 kg sack 20 kg sack specific.
    Tamped density g/l 51 93 119 approx.
    (DIN ISO 787/11)  60  3)
    Effectiveness, 319 334 336 334  1)
    ethanol (0955)
    Effectiveness (UT), 346 365 373 339  1)
    ethanol (0965)
    Settling vol. % 10 5 1
    (effectiveness,
    high-speed
    mixer)

    1) Determined on standard sample (UB 3391)

    3) Guide value
  • The compacted AEROSIL R 202 samples behave in a similar manner to the compacted AEROSIL R 812 samples.
  • Reference is thus made to Example 2 with regard to the discussion.
  • The parameter of “effectiveness” reported in the tables herein relates to the high degree of fineness of the particle. This is therefore an indicator of high transparency and good stability of the resulting dispersions.
  • Further variations and modifications of the foregoing will be apparent to those skilled in the art and are intended to be encompassed by the claims appended hereto.
  • German priority application filed Dec. 22, 2000 199 61 933.6 is relied on and incorporated herein by reference.

Claims (6)

1. A finely divided, readily dispersible hydrophobic, pyrogenically produced silica in the form of aggregates, having a tamped density of 55 to 200 g/l and which has been produced by a process comprising:
(1) hydrophobicizing by reaction of the silica with a halogen-free silane and
(2) compacting the silica by compacting means consisting of a roller compactor or a belt filter press.
2. The finely divided, readily dispersible hydrophobic, pyrogenically produced silica according to claim 1 having a tamped density of 60 to 200 g/l.
3. (canceled)
4. The hydrophobic, pyrogenically produced silica according to claim 1 wherein said silica has a chloride content of less than or equal to 100 ppm.
5.-9. (canceled)
10. A dispersion of a hydrophobic, pyrogenically produced silica according to claim 1.
US11/741,381 1999-12-22 2007-04-27 Hydrophobic silica Abandoned US20070202030A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US11/741,381 US20070202030A1 (en) 1999-12-22 2007-04-27 Hydrophobic silica

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
DE1999161933 DE19961933A1 (en) 1999-12-22 1999-12-22 Silica having higher density useful for production of dispersions is prepared by hydrophobising pyrogenically produced silica and compacting it
DE19961933.6 1999-12-22
US17166799P 1999-12-27 1999-12-27
US09/740,039 US20020037936A1 (en) 1999-12-22 2000-12-20 Hydrophobic silica
US10/623,051 US7282236B2 (en) 1999-12-22 2003-07-18 Hydrophobic silica
US11/741,381 US20070202030A1 (en) 1999-12-22 2007-04-27 Hydrophobic silica

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US10/623,051 Continuation US7282236B2 (en) 1999-12-22 2003-07-18 Hydrophobic silica

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US20070202030A1 true US20070202030A1 (en) 2007-08-30

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US10/623,051 Expired - Lifetime US7282236B2 (en) 1999-12-22 2003-07-18 Hydrophobic silica
US11/741,381 Abandoned US20070202030A1 (en) 1999-12-22 2007-04-27 Hydrophobic silica

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US11352510B2 (en) 2017-10-06 2022-06-07 Evonik Operations Gmbh Aqueous dispersion containing silicon dioxide and trimethyl-1,6-hexamethylendiamine

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US7282236B2 (en) 2007-10-16
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US20040024070A1 (en) 2004-02-05
GB2357497A (en) 2001-06-27

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