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US3924029A Expired / Lapsed US ⏱️ 0.0 years remaining

Method of modifying the surface properties of finely divided metal oxides

Assignee: Evonik Operations GmbH
•
Filing: 1972-03-27
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Granted: 1975-12-02
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Expires: 1992-03-27
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Abstract

Abstract A process for producing hydrophobic finely divided fume silica which comprises the following steps in the specified sequence: A. FORMING, IN A FIRST REACTION ZONE, PARTICLES OF A FUME SILICA HAVING A SIZE OF LESS THAN APPROXIMATELY 150 MILLIMICRONS BY THERMAL DECOMPOSITION AND HYDROLYSIS IN THE VAPOR PHASE OF A VOLATILE SILICON HALIDE, THE SAID FUME SILICA PARTICLES HAVING AN ACIDITY CORRESPONDING TO A PH of approximately 2.0, and including a hydrogen halide and water adsorbed on their surfaces, B. PASSING THE THUS-PRODUCED FUME SILICA PARTICLES OUT OF THE SAID FIRST REACTION ZONE AND SUBJECTING THEM TO A DEACIDIFICATION AND DEHYDRATION PRETREATMENT TO REDUCE THEIR ACIDITY TO A VALUE CORRESPONDING TO A PH of approximately 4.0 by removing substantially all of the adsorbed hydrogen halide and water therefrom, C. PASSING THE THUS-PRETREATED PARTICLES OF FUME SILICA TOGETHER WITH WATER VAPOR INTO A SECOND REACTION ZONE INTO CONTACT WITH A STREAM OF HOT GASES CONTAINING SUBSTANTIAL PROPORTIONS OF AN ORGANOHALOSILANE WHILE THE SECOND REACTION ZONE IS MAINTAINED AT A TEMPERATURE BETWEEN APPROXIMATELY 400* AND APPROXIMATELY 800* C and the particles therein are maintained in a fluidized state and maintained therein for a period sufficient to convert them to hydrophobic fume silica particles, THE FOREGOING STEP, (C) OF THE PROCESS BEING PERFORMED IN THE ABDENCE OF MOLECULAR OXYGEN, AND D. SEPARATING AND RECOVERING THE HYDROPHOBIC FUME SILICA PARTICLES THUS PRODUCED FROM THE HOT GASES AND HYDROGEN HALIDE FORMED FROM THE ORGANOHALOSILANE WHILE STILL CONTINUING TO EXCLUDE MOLECULAR OXYGEN FROM CONTACT WITH THE PARTICLES UNTIL THE PARTICLES HAVE COOLED TO A TEMPERATURE BELOW 400* C.

Inventors

  • 👤 Dieter Schutte
  • 👤 Jean Diether
  • 👤 Helmut Brunner

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-29 09:03
CPC Classifications
C; C09; C09C; C09C1/00; C09C1/28; C09C1/30; C09C1/309; C01; C01P; C01P2004/00; C01P2004/50; C01P2004/60; C01P2004/62; C01P2006/00; C01P2006/10; C01P2006/11; C01P2006/12; C01P2006/80; C01P2006/82; C01P2006/90

Claims Analysis

Total Claims: 6
Claim 1
Independent Claim 260 words
A PROCESS FOR PRODUCING HYDROPHOBIC FINELY DIVIDED FINE SILICA WHICH COMPRISES THE FOLLOWING STEPS IN THE SPECIFIED SEQUENCE: A. FORMING, IN A FIRST REACTION ZONE, PARTICLES OF A FUME SILICA HAVING A SIZE OF LESS THAN APPROXIMATELY 150 MILLIMICRONS BY THERMAL DECOMPOSITION AND HYDROLYSIS IN THE VAPOR PHASE OF A VOLATILE SILICON HALIDE, THE SAID FUME SILICA PARTICLES HAVING AN ACIDITY CORRESPONDING TO A PH OF APPROXIMATELY 2.0, AND INCLUDING A HYDROGEN HALIDE AND WATER ADSORBED ON THEIR SURFACES, B. PASSING THE THUS-PRODUCED FUME SILICA PARTICLES OUT OF THE SAID FIRST REACTION ZONE AND SUBJECTING THEM TO A DEACIDIFICATION AND DEHYDRATION PRETREATMENT TO REDUCE THEIR ACIDITY TO A VALUE CORRESPONDING TO A PH OF APPROXIMATELY 4.0 BY REMOVING SUBSTANTIALLY ALL OF THE ADSORBED HYDROGEN HALIDE AND WATER THEREFROM, C. PASSING THE THUS-PRETRATED PARTICLES OF FUME SILICA TOGETHER WITH WATER VAPOR INTO A SECOND REACTION ZONE INTO CONTACT WITH A STREAM OF HOT GASES CONTAINING SUBSTANTIAL PROPORTIONS OF AN ORGANOHALOSILANE WHILE THE SECOND REACTION ZONE IS MAINTAINED AT A TEMPERATURE BETWEEN APPROXIMATELY 400* AND APPROXIMATELY 800*C AND THE PARTICLES THEREIN ARE MAINTAINED IN A FLUIDIZED STATE AND MAINTAINED THEREIN FOR A PERIOD SUFFICIENT TO CONVERT THEM TO HYDROPHOBIC FUME SILICA PARTICLES, THE FOREGOING STEP (C) OF THE PROCESS BEING PERFORMED IN THE ABSENCE OF MOLECULAR OXYGEN, AND D. SEPARATING AND RECOVERING THE HYDROPHOBIC FUME SILICA PARTICLES THUS PRODUCED FROM THE HOT GASES AND HYDROGEN HALIDE FORMED FROM THE ORGANOHALOGENOSILANE WHILE STILL CONTINUING TO EXCLUDE MOLECULAR OXYGEN FROM CONTACT WITH THE PARTICLES UNTIL THE PARTICLES HAVE COOLED TO A TEMPERATURE BELOW 400*C.
Claim 2
Dependent Claim 260 words
A PROCESS FOR PRODUCING HYDROPHOBIC FINELY DIVIDED FINE SILICA WHICH COMPRISES THE FOLLOWING STEPS IN THE SPECIFIED SEQUENCE: A. FORMING, IN A FIRST REACTION ZONE, PARTICLES OF A FUME SILICA HAVING A SIZE OF LESS THAN APPROXIMATELY 150 MILLIMICRONS BY THERMAL DECOMPOSITION AND HYDROLYSIS IN THE VAPOR PHASE OF A VOLATILE SILICON HALIDE, THE SAID FUME SILICA PARTICLES HAVING AN ACIDITY CORRESPONDING TO A PH OF APPROXIMATELY 2.0, AND INCLUDING A HYDROGEN HALIDE AND WATER ADSORBED ON THEIR SURFACES, B. PASSING THE THUS-PRODUCED FUME SILICA PARTICLES OUT OF THE SAID FIRST REACTION ZONE AND SUBJECTING THEM TO A DEACIDIFICATION AND DEHYDRATION PRETREATMENT TO REDUCE THEIR ACIDITY TO A VALUE CORRESPONDING TO A PH OF APPROXIMATELY 4.0 BY REMOVING SUBSTANTIALLY ALL OF THE ADSORBED HYDROGEN HALIDE AND WATER THEREFROM, C. PASSING THE THUS-PRETRATED PARTICLES OF FUME SILICA TOGETHER WITH WATER VAPOR INTO A SECOND REACTION ZONE INTO CONTACT WITH A STREAM OF HOT GASES CONTAINING SUBSTANTIAL PROPORTIONS OF AN ORGANOHALOSILANE WHILE THE SECOND REACTION ZONE IS MAINTAINED AT A TEMPERATURE BETWEEN APPROXIMATELY 400* AND APPROXIMATELY 800*C AND THE PARTICLES THEREIN ARE MAINTAINED IN A FLUIDIZED STATE AND MAINTAINED THEREIN FOR A PERIOD SUFFICIENT TO CONVERT THEM TO HYDROPHOBIC FUME SILICA PARTICLES, THE FOREGOING STEP (C) OF THE PROCESS BEING PERFORMED IN THE ABSENCE OF MOLECULAR OXYGEN, AND D. SEPARATING AND RECOVERING THE HYDROPHOBIC FUME SILICA PARTICLES THUS PRODUCED FROM THE HOT GASES AND HYDROGEN HALIDE FORMED FROM THE ORGANOHALOGENOSILANE WHILE STILL CONTINUING TO EXCLUDE MOLECULAR OXYGEN FROM CONTACT WITH THE PARTICLES UNTIL THE PARTICLES HAVE COOLED TO A TEMPERATURE BELOW 400*C.
Claim 3
Dependent Claim 12 words
The process of claim 1 in which the organohalosilane is dimethyl dichlorosilane.
Claim 4
Dependent Claim 33 words
A process as defined in claim 1 in which the amount of water vapor that is passed into the second reaction zone is between about 10 and about 100 grams per cubic meter.
Claim 5
Dependent Claim 19 words
A process as defined in claim 1 in which the organohalosilane is a mixture comprising monomethylchlorosilane, dimethylchlorosilane, and trimethylchlorosilane.
Claim 6
Dependent Claim 60 words
A process as defined in claim 1 in which the second reaction zone is a vertical zone, the hot gases containing the organohalosilane are passed upwardly therethrough, the fluidized fume silica particles are also passed therethrough concurrently with the gases and are separated from the gases directly after leaving the said reaction zone while their temperature is still above 400*C.

References Cited (Backward Citations)

US2306222A Cited
US2689166A Cited
US2705222A Cited
US2705206A Cited
US2739078A Cited
US2938009A Cited
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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) 1978-12-01 1979-06-02 1979-12-02 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1982-12-01 1983-06-02 1983-12-02 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1986-12-01 1987-06-02 1987-12-02 $7700.00 Window Closed / Lapsed

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