Patent US4066736A successfully refreshed from Google Patents.
US4066736A
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US
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Process for producing concentrated solutions of hydroxylammonium nitrate and hydroxylammonium perchlorate
Assignee: United States Department of the Navy
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Filing: 1976-03-19
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Granted: 1978-01-03
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Expires: 1996-03-19
Abstract
Abstract A process for preparing concentrated solutions of hydroxylammonium nitrate (HAN) or hydroxylammonium perchlorate (HAP) which comprise reacting hydroxylammonium sulfate with either barium nitrate or barium perchlorate, in such a way that the dissolved barium salt is reacted with the dissolving hydroxylammonium sulfate while agitating the system so as to keep the slurried barium salt from directly contacting the hydroxylammonium sulfate. The rate of addition of the hydroxylammonium sulfate is slower than the rate of solution of the barium salt. An excess of barium nitrate or barium perchlorate ions is needed in the solution to which the hydroxylammonium sulfate is added until the reaction is terminated. The concentration of the HAN or HAP in the final solution can be increased still further if a solution of HAN or HAP is respectively used in forming the barium salt slurry.
Inventors
- 👤 Thomas Liggett
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-07 08:23
CPC Classifications
C; C01; C01B; C01B21/00; C01B21/082; C01B21/14; C01B21/1409; C01B21/1454
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
142 words
In a process for producing concentrated hydroxylammonium nitrate solutions by reacting an alkaline earth nitrate salt selected from the group consisting of barium nitrate and calcium nitrate with a hydroxylammonium salt selected from the group consisting of hydroxylammonium sulfate and hydroxylammonium acid sulfate, the improvement comprising: adding the hydroxylammonium salt to a slurry of particles of the alkaline earth nitrate salt suspended in a solvent selected from the group consisting of water and an aqueous hydroxylammonium nitrate solution at a rate which is slower than the rate of solution of the alkaline earth nitrate into the solvent so that an excess of alkaline earth ions over sulfate ions is maintained in the solvent to prevent the formation of a coating of the insoluble alkaline earth sulfate byproduct on the surfaces of the alkaline earth nitrate particles which would prematurely stop the reaction.
Claim 2
Dependent Claim
142 words
In a process for producing concentrated hydroxylammonium nitrate solutions by reacting an alkaline earth nitrate salt selected from the group consisting of barium nitrate and calcium nitrate with a hydroxylammonium salt selected from the group consisting of hydroxylammonium sulfate and hydroxylammonium acid sulfate, the improvement comprising: adding the hydroxylammonium salt to a slurry of particles of the alkaline earth nitrate salt suspended in a solvent selected from the group consisting of water and an aqueous hydroxylammonium nitrate solution at a rate which is slower than the rate of solution of the alkaline earth nitrate into the solvent so that an excess of alkaline earth ions over sulfate ions is maintained in the solvent to prevent the formation of a coating of the insoluble alkaline earth sulfate byproduct on the surfaces of the alkaline earth nitrate particles which would prematurely stop the reaction.
Claim 3
Dependent Claim
16 words
The process of claim 1 wherein the nitrate salt is suspended in the solvent by agitation.
Claim 4
Dependent Claim
12 words
The process of claim 1 wherein the hydroxylammonium salt is in solution.
Claim 5
Dependent Claim
11 words
The process of claim 1 wherein the hydroxylammonium salt is crystalline.
Claim 6
Dependent Claim
12 words
The process of claim 1 wherein the hydroxylammonium salt is hydroxylammonium sulfate.
Claim 7
Dependent Claim
14 words
The process of claim 1 wherein the alkaline earth nitrate salt is barium nitrate.
Claim 8
Dependent Claim
141 words
In a process for producing concentrated hydroxylammonium perchlorate solutions by reacting an alkaline earth perchlorate selected from the group consisting of barium perchlorate and calcium perchlorate with a hydroxylammonium salt selected from the group consisting of hydroxylammonium sulfate and hydroxylammonium acid sulfate, the improvement comprising: adding the hydroxylammonium salt to a slurry of particles of the alkaline earth perchlorate salt suspended in a solvent selected from the group consisting of water and an aqueous hydroxylammonium perchlorate solution at a rate which is slower than the rate of solution of the alkaline earth perchlorate into the solvent so that an excess of alkaline earth ions over sulfate ions is maintained in the solvent to prevent the formation of a coating of the insoluble alkaline earth sulfate byproduct on the surfaces of the alkaline earth perchlorate particles which would prematurely stop the reaction.
Claim 9
Dependent Claim
141 words
In a process for producing concentrated hydroxylammonium perchlorate solutions by reacting an alkaline earth perchlorate selected from the group consisting of barium perchlorate and calcium perchlorate with a hydroxylammonium salt selected from the group consisting of hydroxylammonium sulfate and hydroxylammonium acid sulfate, the improvement comprising: adding the hydroxylammonium salt to a slurry of particles of the alkaline earth perchlorate salt suspended in a solvent selected from the group consisting of water and an aqueous hydroxylammonium perchlorate solution at a rate which is slower than the rate of solution of the alkaline earth perchlorate into the solvent so that an excess of alkaline earth ions over sulfate ions is maintained in the solvent to prevent the formation of a coating of the insoluble alkaline earth sulfate byproduct on the surfaces of the alkaline earth perchlorate particles which would prematurely stop the reaction.
Claim 10
Dependent Claim
16 words
The process of claim 7 wherein the perchlorate salt is suspended in the solvent by agitation.
Claim 11
Dependent Claim
12 words
The process of claim 7 wherein the hydroxylammonium salt is in solution.
Claim 12
Dependent Claim
11 words
The process of claim 7 wherein the hydroxylammonium salt is crystalline.
Claim 13
Dependent Claim
12 words
The process of claim 7 wherein the hydroxylammonium salt is hydroxylammonium sulfate.
Claim 14
Dependent Claim
14 words
The process of claim 7 wherein the alkaline earth perchlorate salt is barium perchlorate.
References Cited (Backward Citations)
US2768874A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1981-01-02 | 1981-07-04 | 1982-01-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1985-01-02 | 1985-07-04 | 1986-01-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1989-01-02 | 1989-07-04 | 1990-01-03 | $7700.00 | Window Closed / Lapsed |