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US4814017A Expired / Lapsed US ⏱️ 0.0 years remaining

Aqueous organoalkoxysilane/metal oxide sol-gel compositions

Assignee: PPG Industries Ohio Inc
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Filing: 1986-10-03
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Granted: 1989-03-21
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Expires: 2006-10-03
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Abstract

Abstract A method is disclosed for making an organoalkoxysilane/metal oxide sol-gel composition in an essentially aqueous medium by partially hydrolyzing an organoalkoxysilane with a limited amount of water which is essentially completely consumed in the hydrolysis reaction, adding a metal alkoxide of titanium or zirconium to the essentially anhydrous partially hydrolyzed organoalkoxysilane, completely reacting the metal alkoxide with the partially hydrolyzed organoalkoxysilane to form an oxide network and then completely hydrolyzing the composition in water.

Inventors

  • 👤 Bulent E. Yoldas
  • 👤 Chia-Cheng Lin

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-30 08:21
CPC Classifications
C; C09; C09D; C09D183/00; C09D183/14; C09D183/04

Claims Analysis

Total Claims: 11
Claim 1
Independent Claim 194 words
A method of making an organoalkoxysilane/metal oxide sol-gel composition in an aqueous medium comprising the steps of: a. adding a less than equivalent quantity of water to an organoalkoxysilane of the general formula R.sub.x Si(OR').sub.4-x wherein R is an organic radical, R' is a low molecular weight alkyl radical, and x is at least one and less than 4; b. partially hydrolyzing said organoalkoxysilane according to the general reaction R.sub.4 Si(OR').sub.4-x +yH.sub.2 O→R.sub.x Si(OR').sub.4-x-y (OH).sub.y +yR'OH wherein y is at least one and less than 4-x, until said quantity of water is essentially completely reacted; c. adding to said essential anhydrous partially hydrolyzed organoalkoxysilane a metal alkoxide of the general formula M(OR") z wherein M is a metal selected from the group consisting of titanium and zirconium, R" is a low molecular weight alkyl radical, and z is the valence of M; d. reacting said metal alkoxide with said partially hydrolyzed organoalkoxysilane according to the following general reaction ##STR5## until substantially all of said metal alkoxide has reacted with said partially hydrolyzed organoalkoxysilane to form an oxide network; and e. adding sufficient water to essentially completely hydrolyze said composition to form an aqueous sol.
Claim 2
Independent Claim 194 words
A method of making an organoalkoxysilane/metal oxide sol-gel composition in an aqueous medium comprising the steps of: a. adding a less than equivalent quantity of water to an organoalkoxysilane of the general formula R.sub.x Si(OR').sub.4-x wherein R is an organic radical, R' is a low molecular weight alkyl radical, and x is at least one and less than 4; b. partially hydrolyzing said organoalkoxysilane according to the general reaction R.sub.4 Si(OR').sub.4-x +yH.sub.2 O→R.sub.x Si(OR').sub.4-x-y (OH).sub.y +yR'OH wherein y is at least one and less than 4-x, until said quantity of water is essentially completely reacted; c. adding to said essential anhydrous partially hydrolyzed organoalkoxysilane a metal alkoxide of the general formula M(OR") z wherein M is a metal selected from the group consisting of titanium and zirconium, R" is a low molecular weight alkyl radical, and z is the valence of M; d. reacting said metal alkoxide with said partially hydrolyzed organoalkoxysilane according to the following general reaction ##STR5## until substantially all of said metal alkoxide has reacted with said partially hydrolyzed organoalkoxysilane to form an oxide network; and e. adding sufficient water to essentially completely hydrolyze said composition to form an aqueous sol.
Claim 3
Dependent Claim 35 words
A method according to claim 1, wherein the organoalkoxy is selected from the group of R x Si(OR') 4-x wherein R is selected from the group consisting of alkyl, vinyl, methoxyethyl, phenyl, γ-glycidoxypropyl and γ-methacryloxypropyl.
Claim 4
Dependent Claim 32 words
A method according to claim 2, wherein said organoalkoxysilane is selected from the group R x Si(OR') 4-x wherein R' is selected from the group consisting of methyl, ethyl, propyl and butyl.
Claim 5
Dependent Claim 14 words
A method according to claim 3, wherein R is methyl and R' is ethyl.
Claim 6
Dependent Claim 10 words
A method according to claim 4, wherein x is 1.
Claim 7
Dependent Claim 11 words
A method according to claim 1, wherein the organoalkoxysilane comprises γ-glycidoxypropyltrimethoxysilane.
Claim 8
Dependent Claim 22 words
A method according to claim 1, wherein M is selected from the group consisting of titanium and zirconium and z is 4.
Claim 9
Dependent Claim 26 words
A method according to claim 7, wherein the metal alkoxide is selected from the group consisting of tetraethyl titanate tetrapropyl titanate, tetrabutyl titanate and zirconium propoxide.
Claim 10
Dependent Claim 11 words
A method according to claim 8, wherein the organoalkoxysilane is γ-glycidoxypropyltrimethoxysilane.
Claim 11
Dependent Claim 27 words
A method according to claim 9, wherein the metal alkoxide is tetraethyl titanate, and the weight ratio of tetraethyl titanate to organoalkoxysilane is between 0.25 and 0.6.

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1992-03-20 1992-09-19 1993-03-21 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1996-03-20 1996-09-19 1997-03-21 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2000-03-20 2000-09-19 2001-03-21 $7700.00 Window Closed / Lapsed

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