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US4619908A Expired / Lapsed US ⏱️ 0.0 years remaining

Non-aged inorganic oxide-containing aerogels and their preparation

Assignee: Akzo Nobel Inc
•
Filing: 1984-12-24
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Granted: 1986-10-28
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Expires: 2004-12-24
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Abstract

Abstract The invention is directed to inorganic oxide-containing aerogels and the method of preparing such oxide-containing aerogels which are characterized by high surface areas and high pore volume. The preparation comprises dissolving the inorganic alkoxide or metal salt in a solvent optionally containing a catalytic amount of an acid or base and hydrolyzing the metal compound which is then further treated with a fluid at or above its critical temperature and pressure to extract the solvent.

Inventors

  • 👤 Chung-Ping Cheng
  • 👤 Paul A. Iacobucci
  • 👤 Edward N. Walsh

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 16:04
CPC Classifications
C; C08; C08F; C08F4/00; C08F4/02; C08F4/025; B; B01; B01J; B01J13/00; B01J13/0052; B01J13/0091; B01J37/00; B01J37/02; B01J37/03; B01J37/036; C01; C01B; C01B33/00; C01B33/113; C01B33/12; C01B33/14; C01B33/157; C01B33/158; C01B33/1585; C01F; C01F7/00; C01F7/02; C01F7/34; C01F7/36; C01G; C01G23/00; C01G23/04; C01G23/047; C01G23/053; C01G9/00; C01G9/02; C07; C07C; C07C51/00; C07C51/16; C07C51/21; C07C51/255; C07C51/265; C07C51/31; C07C51/313; C01P; C01P2006/00; C01P2006/11; C01P2006/12

Claims Analysis

Total Claims: 37
Claim 1
Independent Claim 53 words
A method of preparing inorganic oxide-containing aerogels comprising: (a) hydrolyzing a compound comprising at least one metal dissolved in a solvent, to produce a gel; (b) contact the hydrolyzed compound with an extraction fluid above the critical temperature and pressure of the fluid to extract the solvent and optionally, (c) drying the gel.
Claim 2
Independent Claim 53 words
A method of preparing inorganic oxide-containing aerogels comprising: (a) hydrolyzing a compound comprising at least one metal dissolved in a solvent, to produce a gel; (b) contact the hydrolyzed compound with an extraction fluid above the critical temperature and pressure of the fluid to extract the solvent and optionally, (c) drying the gel.
Claim 3
Dependent Claim 40 words
The method of claim 1 further comprising depressurizing after step (b) at a rate necessary to maintain the temperature above the critical temperature of the fluid for the time necessary to prevent condensation and to obtain the solid dry aerogel.
Claim 4
Dependent Claim 26 words
The method of claim 1 wherein the metal is selected from Groups II to VI, Group VIIB and Group VIII of the Periodic Table of Elements.
Claim 5
Dependent Claim 10 words
The method of claim 3 wherein the metal is silicon.
Claim 6
Dependent Claim 10 words
The method of claim 3 wherein the metal is titanium.
Claim 7
Dependent Claim 10 words
The method of claim 3 wherein the metal is aluminum.
Claim 8
Dependent Claim 11 words
The method of claim 1 wherein the compound is an alkoxide.
Claim 9
Dependent Claim 11 words
The method of claim 1 wherein the compound is a salt.
Claim 10
Dependent Claim 19 words
The method of claim 1 wherein the hydrolysis is conducted by the addition of a stoichiometric amount of water.
Claim 11
Dependent Claim 23 words
The method of claim 9 wherein the water added is from about 1 to about 10 times in excess of the stochiometric amount.
Claim 12
Dependent Claim 21 words
The method of claim 10 wherein the water added is from about 1 to about 5 times in excess of stoichiometry.
Claim 13
Dependent Claim 16 words
The method of claim 1 wherein the hydrolysis is conducted in the presence of a catalyst.
Claim 14
Dependent Claim 11 words
The method of claim 12 wherein the catalyst is an acid.
Claim 15
Dependent Claim 11 words
The method of claim 12 wherein the catalyst is a base.
Claim 16
Dependent Claim 13 words
The method of claim 1 wherein the gel is washed prior to extraction.
Claim 17
Dependent Claim 13 words
The method of claim 15 wherein the gel is washed with a solvent.
Claim 18
Dependent Claim 16 words
The method of claim 16 wherein the solvent is a C 1 to C 5 alcohol.
Claim 19
Dependent Claim 16 words
The method of claim 1 wherein the extraction fluid has a low critical temperature and pressure.
Claim 20
Dependent Claim 12 words
The method of claim 18 wherein the fluid is CO 2 .
Claim 21
Dependent Claim 22 words
The method of claim 1 wherein the solvent used to dissolve the metal containing compound is a C 1 -C 5 alcohol.
Claim 22
Dependent Claim 10 words
The method of claim 20 wherein the alcohol is ethanol.
Claim 23
Dependent Claim 10 words
The method of claim 20 wherein the alcohol is isopropanol.
Claim 24
Dependent Claim 10 words
The method of claim 20 wherein the alcohol is sec-butanol.
Claim 25
Independent Claim 54 words
The method of preparing inorganic oxide-containing aerogels comprising hydrolyzing a metal alkoxide dissolved in a solvent, contacting the hydrolyzed metal compound with an extraction fluid at not less than the critical temperature and pressure of the extraction fluid such that the solvent is extracted and drying the gel to obtain the dried aerogel product.
Claim 26
Independent Claim 54 words
The method of preparing inorganic oxide-containing aerogels comprising hydrolyzing a metal alkoxide dissolved in a solvent, contacting the hydrolyzed metal compound with an extraction fluid at not less than the critical temperature and pressure of the extraction fluid such that the solvent is extracted and drying the gel to obtain the dried aerogel product.
Claim 27
Independent Claim 50 words
A method of preparing inorganic oxide-containing aerogels comprising hydrolyzing a metal containing compound dissolved in a solvent, contacting the hydrolyzed metal compound with an extraction fluid at not less than its critical temperature and pressure such that the solvent is extracted, drying the gel to obtain the dried aerogel product.
Claim 28
Independent Claim 50 words
A method of preparing inorganic oxide-containing aerogels comprising hydrolyzing a metal containing compound dissolved in a solvent, contacting the hydrolyzed metal compound with an extraction fluid at not less than its critical temperature and pressure such that the solvent is extracted, drying the gel to obtain the dried aerogel product.
Claim 29
Dependent Claim 42 words
The method of claim 25 further comprising depressurizing after extraction of the solvent at a rate necessary to maintain the temperature above the critical temperature of the fluid for the time necessary to prevent condensation and to obtain the solid dry aerogel.
Claim 30
Dependent Claim 13 words
A granular inorganic oxide-containing aerogel product, produced by the method of claim 1.
Claim 31
Dependent Claim 12 words
A granular inorganic oxide-containing aerogel produced by the method of claim 25.
Claim 32
Dependent Claim 12 words
The inorganic oxide-containing aerogel of claim 27 wherein the product is alumina.
Claim 33
Dependent Claim 15 words
The inorganic oxide-containing aerogel of claim 27 wherein the product is a zinc oxide aerogel.
Claim 34
Dependent Claim 14 words
The inorganic oxide-containing aerogel of claim 27 wherein the product is a silica-titania complex.
Claim 35
Dependent Claim 14 words
The inorganic oxide-containing aerogel of claim 27 wherein the product is a zirconia-silica complex.
Claim 36
Dependent Claim 14 words
The inorganic oxide-containing aerogel of claim 27 wherein the product is a silica-alumina complex.
Claim 37
Dependent Claim 31 words
In a method of manufacturing solid phosphoric acid catalyst utilizing an absorbent, the process comprising using as the absorbent a siliceous inorganic oxide aerogel prepared by the method of claim 1.

References Cited (Backward Citations)

US1819354A Cited
US2093454A Cited
US2188007A Cited
US2647875A Cited
US3193492A Cited
US3672833A Cited
US3673111A Cited
US4489172A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1989-10-27 1990-04-28 1990-10-28 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1993-10-27 1994-04-28 1994-10-28 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1997-10-27 1998-04-28 1998-10-28 $7700.00 Window Closed / Lapsed

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