US4236014A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Production of the ammonium salt of 3,5-dinitro-1,2,4-triazole by solvent extraction
Assignee: United States Department of Energy
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Filing: 1979-11-07
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Granted: 1980-11-25
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Expires: 1999-11-07
Abstract
Abstract The ammonium salt of 3,5-dinitro-1,2,4-triazole has utility as a chemical explosive. In accordance with the present invention, it may readily be produced by solvent extraction using high-molecular weight, water-insoluble amines followed by amination with anhydrous ammonia gas. The aqueous reaction mixture produced in the synthesis of the parent compound, 3,5-dinitro-1,2,4-triazole, is quite suitable--and indeed is preferred--for use as the feed material in the process of the invention.
Inventors
- 👤 Kien Y. Lee
- 👤 Donald G. Ott
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-06 14:28
CPC Classifications
C; C07; C07D; C07D249/00; C07D249/02; C07D249/08; C07D249/10
Claims Analysis
Total Claims: 7
Claim 1
Independent Claim
150 words
A method for the production of the ammonium salt of 3,5-dinitro-1,2,4-triazole which comprises: (a) forming an aqueous phase which comprises an aqueous solution of 3,5-dinitro-1,2,4-triazole; (b) forming an organic phase which comprises in a desired ratio a water-insoluble secondary or tertiary aliphatic amine capable of acting as an anion exchanger and a desired diluent, said diluent having a good solubility for ammonia gas and little or no solubility for the ammonium salt of 3,5-dinitro-1,2,4-triazole; (c) contacting said aqueous phase with said organic phase for a time sufficient for partitioning of said 3,5-dinitro-1,2,4-triazole between said aqueous phase and said organic phase to occur; (d) separating the depleted aqueous phase from said organic phase; (e) drying said organic phase; (f) contacting said dried organic phase with ammonia gas; and (g) separating the precipitate produced by the reaction of said ammonia gas with the amine salt of said 3,5-dinitro-1,2,4-triazole from said organic phase.
Claim 2
Independent Claim
150 words
A method for the production of the ammonium salt of 3,5-dinitro-1,2,4-triazole which comprises: (a) forming an aqueous phase which comprises an aqueous solution of 3,5-dinitro-1,2,4-triazole; (b) forming an organic phase which comprises in a desired ratio a water-insoluble secondary or tertiary aliphatic amine capable of acting as an anion exchanger and a desired diluent, said diluent having a good solubility for ammonia gas and little or no solubility for the ammonium salt of 3,5-dinitro-1,2,4-triazole; (c) contacting said aqueous phase with said organic phase for a time sufficient for partitioning of said 3,5-dinitro-1,2,4-triazole between said aqueous phase and said organic phase to occur; (d) separating the depleted aqueous phase from said organic phase; (e) drying said organic phase; (f) contacting said dried organic phase with ammonia gas; and (g) separating the precipitate produced by the reaction of said ammonia gas with the amine salt of said 3,5-dinitro-1,2,4-triazole from said organic phase.
Claim 3
Dependent Claim
98 words
The method of claim 1 wherein said aqueous phase comprises a reaction mixture formed in accordance with the following reaction ##STR2## and wherein the method comprises the additional steps of (h) washing said precipitate with a solvent in which said amine is soluble but said precipitate is insoluble; (i) dissolving said precipitate in a solvent in which other ammonium salts formed when said organic phase is contacted with said ammonia gas are insoluble; (j) removing any solids from the resultant solution; (k) precipitating the ammonium salt of 3,5-dinitro-1,2,4-triazole therefrom; and (l) removing said precipitated salt from said solution.
Claim 4
Dependent Claim
48 words
The method of claim 1 or claim 2 wherein said ammonia gas is anhydrous and is contacted with said organic phase in an amount and for a time sufficient for essentially all the amine salt of said 3,5-dinitro-1,2,4-triazole in said organic phase to react with said ammonia gas.
Claim 5
Dependent Claim
22 words
The method of claim 3 wherein said organic phase is cooled substantially below room temperature before being contacted with said ammonia gas.
Claim 6
Dependent Claim
10 words
The method of claim 4 wherein said diluent is toluene.
Claim 7
Dependent Claim
11 words
The method of claim 5 wherein said amine is trilauryl amine.
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) | 1983-11-25 | 1984-05-26 | 1984-11-25 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1987-11-25 | 1988-05-26 | 1988-11-25 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1991-11-25 | 1992-05-26 | 1992-11-25 | $7700.00 | Window Closed / Lapsed |