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Procedures for the synthesis of ethylenediamine bisborane and ammonia borane
US9534002B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9534002-B2 |
| Application number | US-201113809316-A |
| Country | US |
| Kind code | B2 |
| Filing date | Jul 6, 2011 |
| Priority date | Jul 9, 2010 |
| Publication date | Jan 3, 2017 |
| Grant date | Jan 3, 2017 |
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Abstract
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A method for synthesizing ammonia borane includes (a) preparing a reaction mixture in one or more solvents, the reaction mixture containing sodium borohydride, at least one ammonium salt, and ammonia; and (b) incubating the reaction mixture at temperatures between about 0° C. to about room temperature in an ambient air environment under conditions sufficient to form ammonia borane. Methods for synthesizing ethylenediamine bisborane, and methods for dehydrogenation of ethylenediamine bisborane are also described.
First claim
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The invention claimed is: 1. A method for synthesizing ammonia borane comprising: preparing a reaction mixture in one or more solvents, the reaction mixture comprising sodium borohydride, at least one ammonium salt, and ammonia, wherein the concentration of ammonia in the solvent is between about 1 to about 10% v/v; and incubating the reaction mixture at temperatures between about 0° C. to about room temperature in an ambient air environment under conditions sufficient to form ammonia borane. 2. The method of claim 1 , wherein the at least one ammonium salt is selected from the group consisting of ammonium sulfate, ammonium chloride, ammonium fluoride, ammonium carbonate, ammonium nitrate, ammonium acetate, ammonium bicarbonate ammonium carbamate, ammonium perchlorate, ammonium hydrogen fluoride, ammonium phosphate, and ammonium hydrogen sulfate. 3. The method of claim 1 , wherein the ratio of sodium borohydride to ammonium salts used is between about 1:1 to about 1:4. 4. The method of claim 1 , wherein the solvent is THF. 5. The method of claim 1 , wherein the conditions are formulated for synthesizing ammonia borane at a yield of >50%. 6. The method of claim 1 , wherein the conditions are formulated for synthesizing ammonia borane at a purity of >90%. 7. A method for synthesizing ammonia borane comprising: preparing a reaction mixture in one or more solvents, the reaction mixture comprising sodium borohydride, at least one ammonium salt, and ammonia, wherein the concentration of ammonia in the solvent is between about 2.5 to about 5% v/v; and incubating the reaction mixture at temperatures between about 0° C. to about room temperature in an ambient air environment under conditions sufficient to form ammonia borane. 8. The method of claim 7 , wherein the at least one ammonium salt is selected from the group consisting of ammonium sulfate, ammonium chloride, ammonium fluoride, ammonium carbonate, ammonium nitrate, ammonium acetate, ammonium bicarbonate ammonium carbamate, ammonium perchlorate, ammonium hydrogen fluoride, ammonium phosphate, and ammonium hydrogen sulfate. 9. The method of claim 7 , wherein the ratio of sodium borohydride to ammonium salts used is between about 1:1 to about 1:4. 10. The method of claim 7 , wherein the solvent is THF. 11. The method of claim 7 , wherein the conditions are formulated for synthesizing ammonia borane at a yield of >50%. 12. The method of claim 7 , wherein the conditions are formulated for synthesizing ammonia borane at a purity of >90%.
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Classifications
Compounds containing elements of Groups 3 or 13 of the Periodic Table · CPC title
Compounds containing boron and nitrogen, phosphorus, sulfur, selenium or tellurium · CPC title
- C07F5/022Primary
without C-boron linkages · CPC title
Compounds containing boron and nitrogen, e.g. borazoles (ammonium tetrafluoborates C01B35/063; ammonium borates C01B35/12) · CPC title
Chemistry & Metallurgy · mapped topic
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- What does patent US9534002B2 cover?
- A method for synthesizing ammonia borane includes (a) preparing a reaction mixture in one or more solvents, the reaction mixture containing sodium borohydride, at least one ammonium salt, and ammonia; and (b) incubating the reaction mixture at temperatures between about 0° C. to about room temperature in an ambient air environment under conditions sufficient to form ammonia borane. Methods for …
- Who is the assignee on this patent?
- Ramachandran Padi Veeraraghavan, Gagare Pravin D, Mistry Hitesh, and 2 more
- What technology area does this patent fall under?
- Primary CPC classification C07F5/022. Mapped technology areas include Chemistry & Metallurgy.
- When was this patent published?
- Publication date Tue Jan 03 2017 00:00:00 GMT+0000 (Coordinated Universal Time) (B2). Legal status and post-grant events are not shown on this page.
- What related patents are in patentsdb?
- We list 8 related publications on this page (citations in our corpus or others sharing the same primary CPC).