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US4068024A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for preparing finely divided hydrophobic oxide particles

Assignee: Evonik Operations GmbH
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Filing: 1974-08-12
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Granted: 1978-01-10
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Expires: 1994-08-12
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Abstract

Abstract A process for preparing hydrophobic finely divided particles of oxides of metals and/or oxides of silicon by chemically bonding hydrocarbon radicals to the surface of the oxide particles, said process comprising intensively mixing oxide particles having a water content less than about 1% by weight with a hydrolyzable metal or metalloid compound containing OR groups, wherein said compound is an ester of the general formula: Me(OR).sub.4 wherein Me is an element from group IV of the periodic table, and each R is independently selected from C 1 -C 8 alkyl radicals or an aryl radical. A hydrophobic silicon dioxide particle is provided. Particles prepared by the process are useful as fillers in elastomers.

Inventors

  • 👤 Siegmar Laufer

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-24 13:34
CPC Classifications
C; C09; C09C; C09C3/00; C09C3/12; C01; C01B; C01B13/00; C01B13/14; C01B13/145; C01B33/00; C01B33/113; C08; C08K; C08K9/00; C08K9/04; C08K9/06; C09C1/00; C09C1/28; C09C1/30; C09C1/3081; C09C1/309; C09C3/006; C09C3/08; C01P; C01P2004/00; C01P2004/80; C01P2006/00; C01P2006/90

Claims Analysis

Total Claims: 16
Claim 1
Independent Claim 131 words
A process for preparing hydrophobic finely divided oxide particles consisting essentially of pyrogenic or precipitated silicic acid particles by chemically bonding hydrocarbon radicals to the surface of said particles, said process comprising rendering said particles hydrophobic by intensively mixing said particles with a hydrolysable metal or metalloid compound containing OR groups, wherein said compound is an ester of the formula: Me(OR).sub.4 wherein Me is an element from group IV of the Periodic Table, and each R is independently selected from C 1 -C 8 alkyl radicals, an aryl radical or an alkaryl radical; wherein prior to mixing, during mixing, or after mixing of the oxides and ester, said particles are contacted with anhydrous NH 3 gas; and further wherein said particles have a water content less than about 1% by weight.
Claim 2
Dependent Claim 131 words
A process for preparing hydrophobic finely divided oxide particles consisting essentially of pyrogenic or precipitated silicic acid particles by chemically bonding hydrocarbon radicals to the surface of said particles, said process comprising rendering said particles hydrophobic by intensively mixing said particles with a hydrolysable metal or metalloid compound containing OR groups, wherein said compound is an ester of the formula: Me(OR).sub.4 wherein Me is an element from group IV of the Periodic Table, and each R is independently selected from C 1 -C 8 alkyl radicals, an aryl radical or an alkaryl radical; wherein prior to mixing, during mixing, or after mixing of the oxides and ester, said particles are contacted with anhydrous NH 3 gas; and further wherein said particles have a water content less than about 1% by weight.
Claim 3
Dependent Claim 22 words
Process according to claim 1 in which said silicic acid particles are in admixture with Al 2 O 3 or TiO.sub. 2.
Claim 4
Dependent Claim 11 words
Process of claim 1 in which Me is titanium or silicon.
Claim 5
Dependent Claim 34 words
Process of claim 1 in which mixing is conducted at a pressure of about 1000 Torr to about 10 -2 Torr, and at about 20°-300° C for a few minutes to about 24 hours.
Claim 6
Dependent Claim 17 words
Process of claim 4 in which the oxides have a water content of about 0-0.2% by weight.
Claim 7
Dependent Claim 14 words
Process of claim 5 in which mixtures of oxides are treated with the ester.
Claim 8
Dependent Claim 40 words
Process of claim 4 in which the oxide particles are activated prior to mixing with the ester, said activation comprising heating the oxide particles at about 700°-1000° C for less than about 60 seconds in a stream of inert gas.
Claim 9
Dependent Claim 14 words
Process of claim 7 in which activation is carried out in a fluidized bed.
Claim 10
Dependent Claim 15 words
Process of claim 8 in which the ester is a tetraalkoxysilane or an oligomer thereof.
Claim 11
Dependent Claim 14 words
Process of claim 4 in which the mixing is conducted at about 20°-200° C.
Claim 12
Dependent Claim 13 words
Process of claim 4 in which mixing is conducted at about 20°-35° C.
Claim 13
Dependent Claim 10 words
Process of claim 9 in which the ester is tetrakis-ethylhexoxy-silane.
Claim 14
Dependent Claim 18 words
Process according to claim 1 in which said hydrolyzable metal or metalloid compound is in a gaseous phase.
Claim 15
Dependent Claim 154 words
A process for preparing hydrophobic finely divided oxide particles consisting essentially of pyrogenic or precipitated silicic acid particles by chemically bonding hydrocarbon radicals to the surface of said particles, said process consisting of rendering said particles hydrophobic by intensively mixing said particles at a pressure of about 1000 Torr to about 10 -2 Torr, and at about 20° to about 300° C for a few minutes to about 24 hours with a hydrolysable metal or metalloid compound containing OR groups, wherein said compound is an ester of the formula: ME(OR).sub.4 wherein Me is titanium or silicon, and each R is independently selected from C 1 -C 8 alkyl radicals, an aryl radical or an alkaryl radical, wherein prior to mixing, during mixing, or after mixing of the oxides and ester, said particles are contacted with anhydrous NH 3 gas; and further wherein said particles have a water content less than about 1% by weight.
Claim 16
Dependent Claim 154 words
A process for preparing hydrophobic finely divided oxide particles consisting essentially of pyrogenic or precipitated silicic acid particles by chemically bonding hydrocarbon radicals to the surface of said particles, said process consisting of rendering said particles hydrophobic by intensively mixing said particles at a pressure of about 1000 Torr to about 10 -2 Torr, and at about 20° to about 300° C for a few minutes to about 24 hours with a hydrolysable metal or metalloid compound containing OR groups, wherein said compound is an ester of the formula: ME(OR).sub.4 wherein Me is titanium or silicon, and each R is independently selected from C 1 -C 8 alkyl radicals, an aryl radical or an alkaryl radical, wherein prior to mixing, during mixing, or after mixing of the oxides and ester, said particles are contacted with anhydrous NH 3 gas; and further wherein said particles have a water content less than about 1% by weight.

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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-01-09 1981-07-11 1982-01-10 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-01-09 1985-07-11 1986-01-10 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-01-09 1989-07-11 1990-01-10 $7700.00 Window Closed / Lapsed

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