Patent US2600157A successfully refreshed from Google Patents.
Patent US4482656A successfully refreshed from Google Patents.
US4482656A
Expired / Lapsed
US
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Method for manufacturing a composition for coating substrates with an abrasion-resistant transparent and translucent film
Assignee: Battelle Development Corp
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Filing: 1983-09-29
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Granted: 1984-11-13
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Expires: 2003-09-29
Abstract
Abstract Mineral charge particles of silica or alumina are grafted with a hydrolysis product from a di- or trialkoxysilane whose functional group is compatible with an organic phase into which said grafted particles are ultimately incorporated. The grafted particles are separated from the aqueous hydrolysis medium by spray-drying. The organic phase comprising the grafted mineral particles is used to provide coatings with abrasion resistant properties.
Inventors
- 👤 Van T. Nguyen
- 👤 Gunter Bellmann
- 👤 Jean-Michel Armanet
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-27 18:08
CPC Classifications
C; C08; C08F; C08F292/00; C08G; C08G83/00; C08G83/001; C08K; C08K9/00; C08K9/04; C08K9/06; C09; C09D; C09D7/00; C09D7/40; C09D7/60; C09D7/61; C09D7/62; C08K3/00; C08K3/18; C08K3/20; C08K3/22; C08K3/34; C08K3/36; C08K9/08; Y; Y10; Y10T; Y10T428/00; Y10T428/31504; Y10T428/31652; Y10T428/31663
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
169 words
A process for producing a mineral charge of finely divided silica or alumina having organophilic substituents comprising: (a) hydrolyzing in a hydrolysis medium a di- or trialkoxysilane of formula (RO).sub.3-n SiR.sup.I r.sub.n.sup.2 (I) in which R represents identical or different lower alkyls and R 1 and R 2 are identical or different and selected from the group consisting of alkyl, cycloalkyl, alkylated cycloalkyl, amino alkyl, alkyl amine, alkoxy, alkoxy alkyl, epoxy alkyl, epoxy cycloalkyl, alkenyl, glycidoxy, acryloxy alkyl, methacryloxy alkyl, gamma-ureidopropyl, gamma-chloropropyl, gamma-mercaptopropyl groups, n being 0 or 1, said hydrolysis providing a corresponding di- or trihydroxy silane of formula (HO).sub.3-n SiR.sup.1 R.sub.n.sup.2 (II) in solution in the hydrolysis medium; (b) adding thereto a proportion of mineral particles of finely divided alumina or silica whereby compound II will react with said particles thus providing graft particles; (c) homogenizing the resultant mixture so as to provide a homogeneous dispersion of said graft particles in said medium; (d) spray-drying said homogeneous dispersion, thus forming a powdered substantially dry grafted mineral charge.
Claim 2
Dependent Claim
169 words
A process for producing a mineral charge of finely divided silica or alumina having organophilic substituents comprising: (a) hydrolyzing in a hydrolysis medium a di- or trialkoxysilane of formula (RO).sub.3-n SiR.sup.I r.sub.n.sup.2 (I) in which R represents identical or different lower alkyls and R 1 and R 2 are identical or different and selected from the group consisting of alkyl, cycloalkyl, alkylated cycloalkyl, amino alkyl, alkyl amine, alkoxy, alkoxy alkyl, epoxy alkyl, epoxy cycloalkyl, alkenyl, glycidoxy, acryloxy alkyl, methacryloxy alkyl, gamma-ureidopropyl, gamma-chloropropyl, gamma-mercaptopropyl groups, n being 0 or 1, said hydrolysis providing a corresponding di- or trihydroxy silane of formula (HO).sub.3-n SiR.sup.1 R.sub.n.sup.2 (II) in solution in the hydrolysis medium; (b) adding thereto a proportion of mineral particles of finely divided alumina or silica whereby compound II will react with said particles thus providing graft particles; (c) homogenizing the resultant mixture so as to provide a homogeneous dispersion of said graft particles in said medium; (d) spray-drying said homogeneous dispersion, thus forming a powdered substantially dry grafted mineral charge.
Claim 3
Dependent Claim
40 words
The method of claim 1, wherein step (a) is carried out in aqueous medium, the % by weight of compound of formula (1) being in the range from about 1 to 20% relative to the percent by weight of water.
Claim 4
Dependent Claim
30 words
The method of claim 2, wherein step (a) is carried out at a temperature of 10° to 50° C. under agitation for a period of 15 min to 15 hrs.
Claim 5
Dependent Claim
28 words
The method of claim 2, wherein R 1 is formulae I and II is a γ-methacryloxypropyl group and said aqueous medium has a pH between 3 and 5.5.
Claim 6
Dependent Claim
69 words
The method according to claim 1 wherein: step (a) is carried out in an aqueous medium; the percent by weight of alkoxysilane is 1 to 10% relative to the percent by weight of the water; the pH is maintained at 3.6; step (a) is carried out at a temperature between 15° through 25° inclusive under agitation and for 15 to 30 minutes; and R 1 is a γ-methacryloxypropyl group.
Claim 7
Dependent Claim
18 words
The method of claim 1, comprising using weight ratio of mineral charges to alkoxysilanes from 1:1 to 10:1.
Claim 8
Dependent Claim
25 words
The method of claim 6, wherein homogenizing is carried out for about 15 min. to 2 hrs. at temperatures of about 10° to 50° C.
Claim 9
Dependent Claim
14 words
The method of claim 6, which comprises homogenizing for 30 min. at room temperature.
Claim 10
Dependent Claim
18 words
The method of claim 1, comprising effecting said homogenizing at high stirring speed and under high shear conditions.
Claim 11
Dependent Claim
14 words
The method of claim 1, comprising effecting steps (a), (b) and (c) substantially simultaneously.
Claim 12
Dependent Claim
61 words
The method of claim 1, in which carrying out step (d) comprises injecting under pressure the aqueous dispersed charge resulting from step 2 into a current of hot air or gas within a spray-drying enclosure for effecting evaporation of said water and directing the resulting hot and wet air-charge mixture into a cyclone for separating said charge from said wet air.
Claim 13
Dependent Claim
28 words
The method of claim 11, wherein the temperature of said air is from about 160°-280° C. and the temperature of said enclosure is from 60° to 110° C.
Claim 14
Dependent Claim
22 words
The method of claim 12 wherein the temperature of said air is 260°-270° C. and that of said enclosure is 80°-90° C.
Claim 15
Dependent Claim
22 words
The method of claim 11, wherein said charge after separation from said wet air has a moisture content of 1 to 8%.
Claim 16
Dependent Claim
23 words
The method of claim 13, wherein said charge after separation from said hot air has a moisture content of about 2 to 4%.
Claim 17
Dependent Claim
36 words
The method of claim 1, wherein the step (e) the incorporation and milling of said dried charge into said organic phase is effected using, as a milling aid, glass beads of less than 2 mm diameter.
Claim 18
Dependent Claim
25 words
The claim according to claim 1 in which R is selected from the group of lower alkyls consisting of methyl, ethyl propyl, butyl, and pentyl.
Claim 19
Dependent Claim
12 words
The claim according to claim 17 in which R is a cycloalkyl.
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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) | 1987-11-13 | 1988-05-14 | 1988-11-13 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1991-11-13 | 1992-05-14 | 1992-11-13 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1995-11-13 | 1996-05-14 | 1996-11-13 | $7700.00 | Window Closed / Lapsed |