US4741894A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method of producing halide-free metal and hydroxides
Assignee: ATK Launch Systems LLC
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Filing: 1986-06-03
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Granted: 1988-05-03
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Expires: 2006-06-03
Abstract
Abstract Niobium (V) and tantalum (V) halides are converted to Nb 2 O 5 and Ta 2 O 5 that are free of detectable levels of halide in a two step process. In the first step, the metal halide is reacted with an alcohol and with a replacement species, such as ammonia, which reacts with the halide. This produces a metal alkoxide which is soluble and a halide salt of the replacement species which is insoluble in the alcohol and precipitates. After physically separating the alkoxide in alcohol solution from the precipitate, in a second step, the metal alkoxide is hydrolyzed with purified water to produce the oxide.
Inventors
- 👤 Andreas A. Melas
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 19:04
CPC Classifications
C; C01; C01B; C01B13/00; C01B13/14; C01G; C01G33/00; C01B13/32; C01F; C01F17/00; C01F17/20; C01F17/206; C01G17/00; C01G17/02; C01G28/00; C01G28/005; C01G35/00; C01G56/00; C07; C07C; C07C29/00; C07C29/68; C07C29/70; C07C31/00; C07C31/28; C01P; C01P2006/00; C01P2006/80
Claims Analysis
Total Claims: 15
Claim 1
Independent Claim
161 words
A method for producing a halide-free oxide or hydroxide of a subject element from the corresponding subject element halide, comprising: in a first reaction step, providing a liquid medium comprising a water-free alcohol and contacting said alcoholic medium with the subject element halide and further contacting said alcohol and said subject element halide with a replacement species that reacts with halides, said alcohol being provided at at least about a ten-fold stoichiometric excess relative to said subject element halide, thereby producing a subject element alkoxide and a salt of the replacement species and the halide, said alcohol being selected such that the subject element alkoxide is soluble in said medium and said replacement halide salt is insoluble and precipitates from said medium, physically separating said medium containing said alkoxide from said precipitate salt, and in a second reaction step, hydrolyzing said subject element alkoxide with 18 mega ohm purity water to produce the corresponding subject element oxide or subject element hydroxide.
Claim 2
Independent Claim
161 words
A method for producing a halide-free oxide or hydroxide of a subject element from the corresponding subject element halide, comprising: in a first reaction step, providing a liquid medium comprising a water-free alcohol and contacting said alcoholic medium with the subject element halide and further contacting said alcohol and said subject element halide with a replacement species that reacts with halides, said alcohol being provided at at least about a ten-fold stoichiometric excess relative to said subject element halide, thereby producing a subject element alkoxide and a salt of the replacement species and the halide, said alcohol being selected such that the subject element alkoxide is soluble in said medium and said replacement halide salt is insoluble and precipitates from said medium, physically separating said medium containing said alkoxide from said precipitate salt, and in a second reaction step, hydrolyzing said subject element alkoxide with 18 mega ohm purity water to produce the corresponding subject element oxide or subject element hydroxide.
Claim 3
Dependent Claim
24 words
A method according to claim 1 wherein said replacement species is selected from the group consisting of ammonia, alkali metals and alkaline earth metals.
Claim 4
Dependent Claim
35 words
A method according to claim 1 wherein the said subject element is a member of groups IB-VIIIB, a member of groups IIIA-VIA or a member of the lanthanide and actinide series of the periodic table.
Claim 5
Dependent Claim
22 words
A method according to claim 1 wherein the subject element is selected from the metals of Group VB of the periodic table.
Claim 6
Dependent Claim
14 words
A method according to claim 1 wherein the subject element is tantalum or niobium.
Claim 7
Dependent Claim
26 words
A method according to claim 1 wherein said halide moiety of the subject element halide is selected from the group consisting of chlorine, bromine and iodine.
Claim 8
Dependent Claim
19 words
A method according to claim 1 wherein the subject element halide is a pentavalent halide of tantalum or niobium.
Claim 9
Dependent Claim
21 words
A method according to claim 1 wherein said replacement species is ammonia and said ammonia is continuously bubbled through said alcohol.
Claim 10
Dependent Claim
35 words
A method according to claim 1 wherein said subject element halide is insoluble in said selected alcohol, said subject element halide being in the form of particulates, said particulates being suspended in said selected alcohol.
Claim 11
Dependent Claim
23 words
A method according to claim 1 wherein said subject element halide is in the form of particulates of 60 Standard mesh or finer.
Claim 12
Independent Claim
146 words
A method for producing a halide-free oxide or hydroxide of a subject element from the corresponding subject element halide, comprising: in a first reaction step, providing a medium comprising water-free alcohol and contacting said alcoholic medium with the subject element halide, said alcohol being provided at at least about a ten-fold stoichiometric excess relative to said subject element halide, contacting said alcohol and said subject element halide with an excess of ammonia, thereby producing a subject element alkoxide and an ammonium halide salt, said alcohol being selected such that the subject element alkoxide is soluble in said medium and said ammonium halide salt is insoluble and precipitates said medium, physically separating said alkoxide-containing medium from said precipitated salt, and in a second reaction step, hydrolyzing said subject element alkoxide with 18 mega ohm purity water to produce the corresponding subject element oxide or subject element hydroxide.
Claim 13
Independent Claim
146 words
A method for producing a halide-free oxide or hydroxide of a subject element from the corresponding subject element halide, comprising: in a first reaction step, providing a medium comprising water-free alcohol and contacting said alcoholic medium with the subject element halide, said alcohol being provided at at least about a ten-fold stoichiometric excess relative to said subject element halide, contacting said alcohol and said subject element halide with an excess of ammonia, thereby producing a subject element alkoxide and an ammonium halide salt, said alcohol being selected such that the subject element alkoxide is soluble in said medium and said ammonium halide salt is insoluble and precipitates said medium, physically separating said alkoxide-containing medium from said precipitated salt, and in a second reaction step, hydrolyzing said subject element alkoxide with 18 mega ohm purity water to produce the corresponding subject element oxide or subject element hydroxide.
Claim 14
Independent Claim
129 words
A method for producing a halide-free oxide or hydroxide of a subject element from the corresponding subject element halide, comprising: in a first reaction step, providing a medium consisting essentially of a water-free alcohol and contacting said alcoholic medium with the subject element halide and further contacting said alcoholic medium and said subject element halide with an excess of ammonia, producing a subject element alkoxide and an ammonium halide salt, said alcohol being selected such that the subject element alkoxide is soluble therein and said ammonium salt is insoluble and precipitates therefrom, physically separating said alkoxide-in-alcohol solution from said precipitated salt, and in a second reaction step, hydrolyzing said subject element alkoxide with 18 mega ohm purity water to produce the corresponding subject element oxide or subject element hydroxide.
Claim 15
Independent Claim
129 words
A method for producing a halide-free oxide or hydroxide of a subject element from the corresponding subject element halide, comprising: in a first reaction step, providing a medium consisting essentially of a water-free alcohol and contacting said alcoholic medium with the subject element halide and further contacting said alcoholic medium and said subject element halide with an excess of ammonia, producing a subject element alkoxide and an ammonium halide salt, said alcohol being selected such that the subject element alkoxide is soluble therein and said ammonium salt is insoluble and precipitates therefrom, physically separating said alkoxide-in-alcohol solution from said precipitated salt, and in a second reaction step, hydrolyzing said subject element alkoxide with 18 mega ohm purity water to produce the corresponding subject element oxide or subject element hydroxide.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1991-05-03 | 1991-11-02 | 1992-05-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1995-05-03 | 1995-11-02 | 1996-05-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1999-05-03 | 1999-11-02 | 2000-05-03 | $7700.00 | Window Closed / Lapsed |