US5332429A
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Method for treating fluoroaluminosilicate glass
Assignee: 3M Co
•
Filing: 1992-05-22
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Granted: 1994-07-26
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Expires: 2012-05-22
Abstract
Abstract Fluoroaluminosilicate dental cement glasses are treated with an aqueous silanol treating solution and optionally with an additional organic compound. The treated glasses form cements with improved strength. The silanol can be ethylenically-unsaturated and can contain acidic groups, and, if so, is novel in its own right.
Inventors
- 👤 Sumita B. Mitra
- 👤 Scott R. Culler
- 👤 Bing Wang
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-26 10:51
CPC Classifications
C; C03; C03C; C03C17/00; C03C17/28; C03C17/30; A; A61; A61K; A61K6/00; A61K6/70; A61K6/71; A61K6/76; A61K6/80; A61K6/884; A61K6/887; A61K6/889; C07; C07F; C07F7/00; C07F7/02; C07F7/08; C07F7/0834; C07F7/0836; C07F7/18; C07F7/1804; C08; C08F; C08F30/00; C08F30/04; C08F30/08; Y; Y10; Y10T; Y10T428/00; Y10T428/29; Y10T428/2982; Y10T428/2991; Y10T428/2993; Y10T428/2995; Y10T428/2996; Y10T428/2998; Y10T428/31504; Y10T428/31551; Y10T428/31609; Y10T428/31612
Claims Analysis
Total Claims: 39
Claim 1
Independent Claim
41 words
A method for treating fluoroaluminosilicate glass, comprising the steps of: a. mixing finely-divided fluoroaluminosilicate glass with an aqueous silanol solution, and b. drying the glass, said glass being capable of forming a cement when mixed with water and a polyalkenoic acid.
Claim 2
Independent Claim
41 words
A method for treating fluoroaluminosilicate glass, comprising the steps of: a. mixing finely-divided fluoroaluminosilicate glass with an aqueous silanol solution, and b. drying the glass, said glass being capable of forming a cement when mixed with water and a polyalkenoic acid.
Claim 3
Dependent Claim
17 words
A method according to claim 1, wherein the silanol is ionic and at least 0.1 percent hydrolyzed.
Claim 4
Dependent Claim
17 words
A method according to claim 1, wherein the silanol is nonionic and at least 0.1 percent hydrolyzed.
Claim 5
Dependent Claim
16 words
A method according to claim 1, wherein the solution is acidic and the silanol is ethylenically-unsaturated.
Claim 6
Dependent Claim
16 words
A method according to claim 1, wherein the solution is basic and the silanol is ethylenically-unsaturated.
Claim 7
Dependent Claim
19 words
A method according to claim 1, wherein the solution is acidic and the acid is borne on the silanol.
Claim 8
Dependent Claim
25 words
A method according to claim 1, wherein the solution is acidic and the acid is borne on the silane from which the silanol is formed.
Claim 9
Dependent Claim
19 words
A method according to claim 1, wherein the solution is basic and the base is borne on the silanol.
Claim 10
Dependent Claim
25 words
A method according to claim 1, wherein the solution is basic and the base is borne on the silane from which the silanol is formed.
Claim 11
Dependent Claim
17 words
A method according to claim 1, wherein the silanol has one or more pendant carboxylic acid groups.
Claim 12
Dependent Claim
30 words
A method according to claim 1, wherein the silanol has the formula R n Si(OH) 4-n wherein R is a non-hydrolyzable polymerizable organic group and n is one to three.
Claim 13
Dependent Claim
97 words
A method according to claim 1, wherein the silanol was formed by hydrolysis of the alkoxy groups of an ethylenically-unsaturated alkoxysilane of the formula: ##STR3## wherein R 1 , R 2 , R 3 and R 4 are independently H, CH 3 , COOH or CH 2 COOH; R 5 and R 6 are independently divalent alkylene linking groups; each R 7 is independently an alkyl group; T 1 and T 2 are independently terminating groups such as H or alkyl; w is 0 to 12; and each of x, y and z is at least one.
Claim 14
Dependent Claim
23 words
A method according to claim 1, wherein the solution is acidic and the acid is present as a separate component of the solution.
Claim 15
Dependent Claim
23 words
A method according to claim 1, wherein the solution is basic and the base is present as a separate component of the solution.
Claim 16
Dependent Claim
61 words
A method according to claim 13, wherein the acid is selected from the group consisting of formic acid, acetic acid, trifluoroacetic acid, propionic acid, pentafluoropropionic acid, hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, lactic acid, citric acid and tartaric acid, and said solution further comprises a solvent selected from the group consisting of methanol, ethanol, propanol, isopropanol, tert-butanol and acetone.
Claim 17
Dependent Claim
64 words
A method according to claim 14, wherein the base is selected from the group consisting of sodium hydroxide, ammonium hydroxide, potassium hydroxide, barium hydroxide, lithium hydroxide, magnesium hydroxide, calcium hydroxide, sodium bicarbonate, ammonia, methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, n-propylamine, n-butylamine, isobutylamine, sec-butylamine, and tert-butylamine and said solution further comprises a solvent selected from the group consisting of methanol, ethanol, propanol, isopropanol, tert-butanol and acetone.
Claim 18
Dependent Claim
27 words
A method according to claim 1, wherein the solution contains about 0.1 to about 20 weight % silanol and about 80 to about 99.9 weight % water.
Claim 19
Dependent Claim
17 words
A method according to claim 1 wherein the glass is further treated with an additional organic compound.
Claim 20
Dependent Claim
26 words
A method according to claim 18, wherein the additional organic compound has at least one functional group selected from the group consisting of acrylates and methacrylates.
Claim 21
Dependent Claim
26 words
A method according to claim 18, wherein the additional organic compound has a weight avenge molecular weight per double bond of between about 100 and 5000.
Claim 22
Dependent Claim
14 words
A method according to claim 18, wherein the additional organic compound comprises polyethyleneglycol dimethacrylate.
Claim 23
Dependent Claim
21 words
A method according to claim 18, wherein the silanol solution and the additional organic compound are sequentially applied to the glass.
Claim 24
Dependent Claim
35 words
A method according to claim 1, wherein the solution contains about 0.1 to about 20 weight % silanol, at least about 40 weight % volatile solvent, and about 20% to about 60 weight % water.
Claim 25
Dependent Claim
32 words
A method according to claim 1, wherein the solution contains about 0.1 to about 10 weight % silanol, water, and sufficient acid to provide a pH of about 1 to about 4.5.
Claim 26
Dependent Claim
32 words
A method according to claim 1, wherein the solution contains about 0.1 to about 10 weight % silanol, water, and sufficient base to provide a pH of about 8 to about 12.
Claim 27
Dependent Claim
45 words
A method according to claim 1, wherein the dried treated glass a forms a cement upon being mixed with water and a polyacrylic acid, and one day after forming said cement releases fluoride at a rate greater than a like glass having a silane treatment.
Claim 28
Independent Claim
41 words
A method of making a glass ionomer cement, comprising the steps of: a. treating finely-divided fluoroaluminosilicate glass with an aqueous silanol solution; b. mixing the treated glass with a polyalkenoic acid; and c. allowing the mixture of step b) to harden.
Claim 29
Independent Claim
41 words
A method of making a glass ionomer cement, comprising the steps of: a. treating finely-divided fluoroaluminosilicate glass with an aqueous silanol solution; b. mixing the treated glass with a polyalkenoic acid; and c. allowing the mixture of step b) to harden.
Claim 30
Dependent Claim
16 words
A method according to claim 27, wherein the solution is acidic and the silanol is ethylenically-unsaturated.
Claim 31
Dependent Claim
30 words
A method according to claim 27, wherein the silanol has the formula R n Si(OH) 4-n wherein R is a non-hydrolyzable polymerizable organic group and n is one to three.
Claim 32
Dependent Claim
97 words
A method according to claim 27, wherein the silanol was formed by hydrolysis of the alkoxy groups of an ethylenically-unsaturated alkoxysilane of the formula: ##STR4## wherein R 1 , R 2 , R 3 and R 4 are independently H CH 3 , COOH or CH 2 COOH; R 5 and R 6 are independently divalent alkylene linking groups; each R 7 is independently an alkyl group; T 1 and T 2 are independently terminating groups such as H or alkyl; w is 0 to 12; and each of x, y and z is at least one.
Claim 33
Dependent Claim
23 words
A method according to claim 27, wherein the solution is acidic and the acid is present as a separate component of the solution.
Claim 34
Dependent Claim
17 words
A method according to claim 27, wherein the glass is further treated with an additional organic compound.
Claim 35
Dependent Claim
26 words
A method according to claim 32, wherein the additional organic compound has at least one functional group selected from the group consisting of acrylates and methacrylates.
Claim 36
Dependent Claim
21 words
A method according to claim 32, wherein the silanol solution and the additional organic compound are sequentially applied to the glass.
Claim 37
Dependent Claim
35 words
A method according to claim 27, wherein the solution contains about 0.1 to about 20 weight % silanol, at least about 40 weight % volatile solvent and about 20 to about 60 weight % water.
Claim 38
Dependent Claim
31 words
A method according to claim 27, wherein one day after mixing with the polyalkenoic acid the cement releases fluoride at a rate greater than a like glass having a silane treatment.
Claim 39
Dependent Claim
28 words
A method according to claim 27, wherein twelve days after mixing with the polyalkenoic acid the cumulative fluoride release rate of the cement is at least 52 μg/g.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
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| 3.5 Years (Year 4) | 1997-07-25 | 1998-01-24 | 1998-07-26 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2001-07-25 | 2002-01-24 | 2002-07-26 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2005-07-25 | 2006-01-24 | 2006-07-26 | $7700.00 | Window Closed / Lapsed |