US4246139A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Silica production
Assignee: Phillips Petroleum Co
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Filing: 1975-09-15
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Granted: 1981-01-20
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Expires: 1995-09-15
Abstract
Abstract A method of producing silica compositions from hydrogels in which the hydrogel is washed in a first water-soluble organic liquid to remove a principal portion of the water. The washed composition is then washed in at least one second water-soluble organic liquid and the second organic liquid is removed from the composition by venting the second organic liquid from the composition at a temperature above the critical temperature of the second organic liquid to produce a silica composition.
Inventors
- 👤 Donald R. Witt
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 21:45
CPC Classifications
C; C08; C08F; C08F10/00; C08F10/02; B; B01; B01J; B01J21/00; B01J21/06; B01J21/063; B01J37/00; B01J37/02; B01J37/03; B01J37/036; Y; Y10; Y10S; Y10S502/00; Y10S502/506; Y10S502/513
Claims Analysis
Total Claims: 4
Claim 1
Independent Claim
177 words
A method of preparing a silica-containing composition comprising: (a) forming a silica-titanium hydrogel by adding a solution of sodium silicate to a solution of sulfuric acid containing titanyl sulfate; (b) aging the hydrogel; (c) removing substantially all of the sodium ions from said hydrogel to produce a purified hydrogel; (d) contacting said purified hydrogel with a plurality of contacts with methanol and then with a plurality of contacts with ethanol to displace a major portion of the water in the hydrogel thereby resulting in an organogel; (e) separating the organogel from the liquid not contained therein; (f) then contacting the thus separated organogel with a plurality of contacts with diethyl ether; (g) then removing the liquid remaining in the organogel by heating said organogel in a confined zero in such a manner that no substantial vaporization occurs until the critical temperature of the diethyl ether is reached; and (h) then venting the vapors from said confined zone at such a rate that the reduction in the porosity of the organogel is minimized to produce a dried gel.
Claim 2
Independent Claim
177 words
A method of preparing a silica-containing composition comprising: (a) forming a silica-titanium hydrogel by adding a solution of sodium silicate to a solution of sulfuric acid containing titanyl sulfate; (b) aging the hydrogel; (c) removing substantially all of the sodium ions from said hydrogel to produce a purified hydrogel; (d) contacting said purified hydrogel with a plurality of contacts with methanol and then with a plurality of contacts with ethanol to displace a major portion of the water in the hydrogel thereby resulting in an organogel; (e) separating the organogel from the liquid not contained therein; (f) then contacting the thus separated organogel with a plurality of contacts with diethyl ether; (g) then removing the liquid remaining in the organogel by heating said organogel in a confined zero in such a manner that no substantial vaporization occurs until the critical temperature of the diethyl ether is reached; and (h) then venting the vapors from said confined zone at such a rate that the reduction in the porosity of the organogel is minimized to produce a dried gel.
Claim 3
Dependent Claim
33 words
A method according to claim 1 wherein the solution of sulfuric acid contains enough titanyl sulfate to insure that the dried gel will contain from about 0.5 to about 10 weight percent titanium.
Claim 4
Dependent Claim
37 words
A method according to claim 1 wherein subtantial vaporization of the liquid remaining in the gel during the heating step is prevented by placing the confined zone containing the gel under sufficient pressure of an inert gas.
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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) | 1984-01-20 | 1984-07-21 | 1985-01-20 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-01-20 | 1988-07-21 | 1989-01-20 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-01-20 | 1992-07-21 | 1993-01-20 | $7700.00 | Window Closed / Lapsed |