US4765818A
Expired / Lapsed
US
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Porous glass monoliths
Assignee: CNA Holdings LLC
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Filing: 1987-02-24
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Granted: 1988-08-23
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Expires: 2007-02-24
Abstract
Abstract In one embodiment this invention provides a novel sol-gel process for the production of microporous inorganic oxide glass monolith structures which have improved mechanical strength and optical transparency. An essential feature of the process is the use of trioxane during the gellation phase, to provide a glass monolith with micropores which have uniformity of size and shape.
Inventors
- 👤 Tessie M. Che
- 👤 Raymond V. Carney
- 👤 Duane L. Dotson
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 21:51
CPC Classifications
C; C03; C03C; C03C1/00; C03C1/006; C03B; C03B19/00; C03B19/12; C03C11/00; Y; Y10; Y10S; Y10S65/00; Y10S65/90; Y10S65/901
Claims Analysis
Total Claims: 17
Claim 1
Independent Claim
119 words
A process for producing an inorganic oxide glass monolith composition with a microporous structure which comprises (1) hydrolyzing tetraalkoxysilane under acidic or basic pH conditions in a sol-gel reaction medium comprising water and trioxane until gellation of the reaction medium is completed; (2) heating and drying the gelled medium at a temperature between about 50°-200° C. to remove water and trioxane from the medium and form a microporous glass monolith; and (3) heating the microporous glass monolith at a temperature between about 600°-900° C. to provide a densified microporous glass monolith; wherein the microporous glass monolith has pore diameters in the range between about 15-2000 angstroms, and the pore diameters are within about a 100 angstrom diameter variation range.
Claim 2
Dependent Claim
119 words
A process for producing an inorganic oxide glass monolith composition with a microporous structure which comprises (1) hydrolyzing tetraalkoxysilane under acidic or basic pH conditions in a sol-gel reaction medium comprising water and trioxane until gellation of the reaction medium is completed; (2) heating and drying the gelled medium at a temperature between about 50°-200° C. to remove water and trioxane from the medium and form a microporous glass monolith; and (3) heating the microporous glass monolith at a temperature between about 600°-900° C. to provide a densified microporous glass monolith; wherein the microporous glass monolith has pore diameters in the range between about 15-2000 angstroms, and the pore diameters are within about a 100 angstrom diameter variation range.
Claim 3
Dependent Claim
27 words
A process in accordance with claim 1 wherein the inorganic oxide glass monolith composition comprises a microporous structure of silica and at least one additional inorganic oxide.
Claim 4
Dependent Claim
15 words
A process in accordance with claim 1 wherein the step(1) tetraalkoxysilane is tetramethoxysilane or tetraethoxysilane.
Claim 5
Dependent Claim
21 words
A process in accordance with claim 1 wherein the step(1) reaction is conducted under acidic pH conditions with hydrogen fluoride reagent.
Claim 6
Dependent Claim
21 words
A process in accordance with claim 1 wherein the step(1) reaction medium contains a water-miscible organic solvent as an additional component.
Claim 7
Dependent Claim
23 words
A process in accordance with claim 1 wherein the step(1) reaction medium contains between about 0.1-2 mole of trioxane per mole of tetraalkoxysilane.
Claim 8
Dependent Claim
23 words
A process in accordance with claim 1 wherein the step(1) reaction is conducted at a temperature between about -10° C. and 30° C.
Claim 9
Dependent Claim
35 words
A process in accordance with claim 1 wherein the step(2) heating cycle is commenced and completed within a lapsed time period of not more than about fifteen days after the step(1) gellation reaction is completed.
Claim 10
Dependent Claim
33 words
A process in accordance with claim 1 wherein the step(2) heating cycle is conducted with a ramp temperature profile from about 50° C. to 200° C. over a period of about 4-20 days.
Claim 11
Dependent Claim
21 words
A process in accordance with claim 1 wherein the step(3) heating cycle is conducted over a period of about 1-6 days.
Claim 12
Dependent Claim
144 words
A process for producing a composite composition comprising a homogeneous inorganic oxide glass monolith composition with a microporous structure containing an organic component which comprises (1) hydrolyzing tetraalkoxysilane under acidic or basic pH conditions in a sol-gel reaction medium comprising water and trioxane until gellation of the reaction medium is completed; (2) heating and drying the gelled medium at a temperature between about 50° C.-200° C. to remove water and trioxane from the medium and form a microporous glass monolith; (3) heating the microporous glass monolith at a temperature between about 600°-900° C. to provide a densified microporous glass monolith; and (4) impregnating the microporous glass monolith with an organic component to produce a composite composition; wherein the microporous glass monolith has pore diameters in the range between about 15-2000 angstroms, and the pore diameters are within about a 100 angstrom diameter variation range.
Claim 13
Dependent Claim
144 words
A process for producing a composite composition comprising a homogeneous inorganic oxide glass monolith composition with a microporous structure containing an organic component which comprises (1) hydrolyzing tetraalkoxysilane under acidic or basic pH conditions in a sol-gel reaction medium comprising water and trioxane until gellation of the reaction medium is completed; (2) heating and drying the gelled medium at a temperature between about 50° C.-200° C. to remove water and trioxane from the medium and form a microporous glass monolith; (3) heating the microporous glass monolith at a temperature between about 600°-900° C. to provide a densified microporous glass monolith; and (4) impregnating the microporous glass monolith with an organic component to produce a composite composition; wherein the microporous glass monolith has pore diameters in the range between about 15-2000 angstroms, and the pore diameters are within about a 100 angstrom diameter variation range.
Claim 14
Dependent Claim
33 words
A process in accordance with claim 11 wherein the step(2) heating cycle is conducted with a ramp temperature profile from about 50° C. to 200° C. over a period of about 4-7 days.
Claim 15
Dependent Claim
21 words
A process in accordance with claim 11 wherein the step(3) heating cycle is conducted over a period of about 1-4 days.
Claim 16
Dependent Claim
17 words
A process in accordance with claim 11 wherein the organic component in step(4) exhibits liquid crystalline properties.
Claim 17
Dependent Claim
17 words
A process in accordance with claim 11 wherein the organic component in step(4) exhibits nonlinear optical response.
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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) | 1991-08-23 | 1992-02-22 | 1992-08-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1995-08-23 | 1996-02-22 | 1996-08-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1999-08-23 | 2000-02-22 | 2000-08-23 | $7700.00 | Window Closed / Lapsed |