US4649037A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Spray-dried inorganic oxides from non-aqueous gels or solutions
Assignee: Honeywell International Inc
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Filing: 1985-03-29
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Granted: 1987-03-10
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Expires: 2005-03-29
Abstract
Abstract Inorganic metal oxides having high surface area and pore volume are prepared by spray drying. The admixture which is spray dried to yield the metal oxides is produced from reactants comprising at least one hydrolyzable metal compound, a sufficient amount of water to at least partially hydrolyze the metal compound and an organic solvent. The admixture is supplied as a plurality of droplets to a reaction zone operated under conditions of temperature and pressure below the critical temperature and pressure of the reactants but sufficient to produce a product comprising metal oxide powders and a gas comprising organic solvent vapors. The powders are separated from the gas in a known fashion and collected. Spray drying of non-aqueous systems unexpectedly produces metal oxides having properties generally intermediate conventionally produced oxides and aerogels.
Inventors
- 👤 Gary B. Marsh
- 👤 Anthony J. Fanelli
- 👤 John N. Armor
- 👤 Patrick M. Zambri
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-06 02:36
CPC Classifications
B; B01; B01J; B01J2/00; B01J2/02; B01J2/04; B01J2/06; B01J2/08; B01J21/00; B01J21/02; B01J21/04; B01J21/06; B01J21/063; B01J21/066; B01J37/00; B01J37/0009; B01J37/0027; B01J37/0045; B82; B82Y; B82Y30/00; C; C01; C01B; C01B13/00; C01B13/14; C01B13/34; C01F; C01F5/00; C01F5/02; C01F7/00; C01F7/02; C01F7/16; C01F7/162; C01F7/164; C01F7/34; C01F7/36; C01G; C01G23/00; C01G23/003; C01G23/006; C01G25/00; C01G25/02; C01P; C01P2002/00; C01P2002/70; C01P2004/00; C01P2004/01; C01P2004/03; C01P2004/50; C01P2004/60; C01P2004/61; C01P2004/62; C01P2004/64; C01P2006/00; C01P2006/10; C01P2006/12; C01P2006/14
Claims Analysis
Total Claims: 26
Claim 1
Independent Claim
95 words
A process of producing metal oxide powders which comprises: (a) admixing reactants comprising an organic solvent, at least one hydrolyzable metal compound, and a sufficient amount of water to at least partially hydrolyze said hydrolyzable metal compound; (b) supplying the admixture as a plurality of droplets to a heating zone operated under conditions of temperature and pressure below the critical temperature and pressure of the reactants but sufficient to produce a product comprising metal oxide powders, and a gas comprising organic solvent vapors; (c) separating said product from said gas; and, (d) collecting the product.
Claim 2
Dependent Claim
95 words
A process of producing metal oxide powders which comprises: (a) admixing reactants comprising an organic solvent, at least one hydrolyzable metal compound, and a sufficient amount of water to at least partially hydrolyze said hydrolyzable metal compound; (b) supplying the admixture as a plurality of droplets to a heating zone operated under conditions of temperature and pressure below the critical temperature and pressure of the reactants but sufficient to produce a product comprising metal oxide powders, and a gas comprising organic solvent vapors; (c) separating said product from said gas; and, (d) collecting the product.
Claim 3
Dependent Claim
21 words
The process of claim 1 wherein the admixture is supplied to the heating zone of a closed cycle spray drying apparatus.
Claim 4
Dependent Claim
28 words
The process of claim 1 wherein the organic solvent is selected from the group consisting of hydrocarbons, ketones, aliphatic or aromatic hydrocarbons, kerosenes, ethers, alcohols, or mixtures thereof.
Claim 5
Dependent Claim
36 words
The process of claim 1 wherein the hydrolyzable metal compound is an organometallic compound selected from the group of metal alkoxides, metal acetates, metal alkanoates, metal acetylacetonates, metal carboxylates, metal oxalates, metal citrates, or mixtures thereof.
Claim 6
Dependent Claim
25 words
The process of claim 1 wherein the energy supplied to the heating zone is sufficient to evaporate substantially all of the organic solvent and water.
Claim 7
Dependent Claim
17 words
The process of claim 5 wherein the heating zone operates at a pressure of about 1 atm.
Claim 8
Dependent Claim
20 words
The process of claim 1 wherein the plurality of droplets are formed by supplying the admixture through a spray nozzle.
Claim 9
Dependent Claim
25 words
The process of claim 1 wherein the plurality of droplets are formed by supplying the admixture to a rotating disk located within the heating zone.
Claim 10
Dependent Claim
18 words
The process of claim 4 wherein the organic solvent is an alcohol having one to five carbon atoms.
Claim 11
Dependent Claim
47 words
The process of claim 1 wherein the metal of the hydrolyzable metal compound is selected from the group of aluminum, barium, calcium, lithium, potassium, magnesium, cerium, lanthanum, titanium, zirconium, chromium, zinc, gallium, silicon, antimony, bismith, strontium, lead, iron, copper, yttrium, molybdenum, boron, tungsten, tin, or mixtures thereof.
Claim 12
Dependent Claim
14 words
The process of claim 1 wherein the hydrolyzable metal compound is a metal alkoxide.
Claim 13
Dependent Claim
28 words
The process of claim 1 wherein the amount of water is not more than about the stoichiometric amount of water necessary to substantially hydrolyze said hydrolyzable metal compound.
Claim 14
Dependent Claim
19 words
The process of claim 1 wherein the organic solvent and the hydrolyzable metal compound comprise the same organic radical.
Claim 15
Dependent Claim
19 words
The process of claim 1 wherein the organic solvent is isopropanol and the hydrolyzable metal compound is aluminum isopropoxide.
Claim 16
Dependent Claim
17 words
The process of claim 1 wherein the organic solvent dissolves substantially all of the hydrolyzable metal compound.
Claim 17
Dependent Claim
26 words
The process of claim 1 wherein the water is added to hydrolyze hydrolyzable metal compound after the hydrolyzable metal compound is added to the organic solvent.
Claim 18
Dependent Claim
23 words
The process of claim 1 wherein the reaction product comprises metal oxide powders having a primary particle size of less than about 1μ.
Claim 19
Dependent Claim
25 words
The process of claim 17 wherein at least about 50% metal oxide powders have a pri-mary particle size equal to or less than about 0.5μ.
Claim 20
Dependent Claim
11 words
A process according to claim 3 wherein said alcohols are glycols.
Claim 21
Dependent Claim
107 words
A process of producing metal oxide powders which comprises: (a) admixing reactants comprising an organic solvent, at least one hydrolyzable metal compound and a sufficient amount of water in an amount not greater than about 110% of the stoichiometric amount of water necessary to substantially completely hydrolyze said hydrolyzable metal compound; (b) supplying the admixture as a plurality of droplets to a heating zone operated under conditions of temperature and pressure below the critical temperature and pressure of the reactants but sufficient to produce comprising metal oxide powders, and a gas comprising organic solvent vapors; (c) separating said product from said gas; and, (d) collecting the product.
Claim 22
Dependent Claim
107 words
A process of producing metal oxide powders which comprises: (a) admixing reactants comprising an organic solvent, at least one hydrolyzable metal compound and a sufficient amount of water in an amount not greater than about 110% of the stoichiometric amount of water necessary to substantially completely hydrolyze said hydrolyzable metal compound; (b) supplying the admixture as a plurality of droplets to a heating zone operated under conditions of temperature and pressure below the critical temperature and pressure of the reactants but sufficient to produce comprising metal oxide powders, and a gas comprising organic solvent vapors; (c) separating said product from said gas; and, (d) collecting the product.
Claim 23
Dependent Claim
111 words
A process of producing metal oxide powders which comprises: (a) admixing reactants comprising an organic solvent, at least one hydrolyzable metal compound, and a sufficient amount of water to at least partially hydrolyze said hydrolyzable metal compound; (b) supplying the admixture as a plurality of droplets to a heating zone operated under conditions of temperature and pressure below the critical temperature and pressure of the reactants but sufficient to produce a product comprising metal oxide powders, and a gas comprising organic solvent vapors; (c) separating said product from said gas; and, (d) collecting the product, the product comprising metal oxide powders having a primary particle size of less than about 1μ.
Claim 24
Dependent Claim
111 words
A process of producing metal oxide powders which comprises: (a) admixing reactants comprising an organic solvent, at least one hydrolyzable metal compound, and a sufficient amount of water to at least partially hydrolyze said hydrolyzable metal compound; (b) supplying the admixture as a plurality of droplets to a heating zone operated under conditions of temperature and pressure below the critical temperature and pressure of the reactants but sufficient to produce a product comprising metal oxide powders, and a gas comprising organic solvent vapors; (c) separating said product from said gas; and, (d) collecting the product, the product comprising metal oxide powders having a primary particle size of less than about 1μ.
Claim 25
Dependent Claim
107 words
A process of producing metal oxide powders which comprises: (a) admixing reactants comprising an organic solvent, at least one hydrolyzable metal compound, and a sufficient amount of water to at least partially hydrolyze said hydrolyzable metal compound, the admixture having a pH of between about 2 and about 10; (b) supplying the admixture as a plurality of droplets to a heating zone operated under conditions of temperature and pressure below the critical temperature and pressure of the reactants but sufficient to produce a product comprising metal oxide powders, and a gas comprising organic solvent vapors; (c) separating said product from said gas; and, (d) collecting the product.
Claim 26
Dependent Claim
107 words
A process of producing metal oxide powders which comprises: (a) admixing reactants comprising an organic solvent, at least one hydrolyzable metal compound, and a sufficient amount of water to at least partially hydrolyze said hydrolyzable metal compound, the admixture having a pH of between about 2 and about 10; (b) supplying the admixture as a plurality of droplets to a heating zone operated under conditions of temperature and pressure below the critical temperature and pressure of the reactants but sufficient to produce a product comprising metal oxide powders, and a gas comprising organic solvent vapors; (c) separating said product from said gas; and, (d) collecting the product.
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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) | 1990-03-09 | 1990-09-08 | 1991-03-10 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1994-03-09 | 1994-09-08 | 1995-03-10 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1998-03-09 | 1998-09-08 | 1999-03-10 | $7700.00 | Window Closed / Lapsed |