IP Library Granted Patent US 8,367,027
Granted Patent B2
US 8,367,027 · App. 12/762,895 · Granted Feb 5, 2013

Regeneration of ammonia borane from polyborazylene

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Quick Facts
Patent No.
US 8,367,027
App. No.
12/762,895
Granted
Feb 5, 2013
Kind
B2
Abstract

Method of producing ammonia borane, comprising providing a reagent comprising a dehydrogenated material in a suitable solvent; and combining the reagent with a reducing agent comprising hydrazine, a hydrazine derivative, or combinations thereof, in a reaction which produces a mixture comprising ammonia borane.

Claims (28)

1. A method of producing ammonia borane, comprising:

a) providing a reagent comprising a dehydrogenated material in a suitable solvent; and

b) combining the reagent with a reducing agent comprising hydrazine, a hydrazine derivative, or combinations thereof, in a reaction which produces a mixture comprising ammonia borane.

2. The method of claim 1 , wherein the dehydrogenated material comprises polyborazylene, cyclopentaborazane, spent fuel products, or combinations thereof.

3. The method of claim 1 , wherein the reducing agent comprises tetrahydrofuran, hydrazine, glyme, diglyme, tetraglyme, toluene, hexane, triethylamine, diethylamine, trioctylamine, liquid ammonia, diethyl ether, or combinations thereof.

4. The method of claim 1 , wherein the reaction proceeds for a period of time of 24 hours or less.

5. The method of claim 1 , wherein the reaction proceeds at a temperature of from about −4° C. to about 96° C.

6. The method of claim 4 , wherein the temperature is about 25° C.

7. The method of claim 1 , wherein the reaction proceeds at a temperature of from about 40° C. to about 60° C. and at a pressure of from about 200 psi to about 400 psi.

8. The method of claim 7 , wherein the ammonia borane is substantially free from byproducts.

9. The method of claim 1 , wherein the mixture comprises produces a byproduct.

10. The method of claim 9 , further comprising the step of reacting the byproduct with an ammonia-containing reagent to produce ammonia borane.

11. The method of claim 10 , wherein the ammonia-containing reagent is ammonia, triethylamine, diethylamine, trioctylamine, and combinations thereof.

12. The method of claim 1 , wherein the spent fuel components comprise alkyl substituted aminoboranes, aryl substituted aminoboranes, borazine, cyclotriborazine, diborane, diammoniate of diborane, aminoborane, iminoborane, methylaminoborane, or combinations thereof.

13. A method of producing ammonia borane, comprising:

a) providing a reagent comprising polyborazylene, cyclopentaborazane, spent fuel products, or combinations thereof;

b) digesting the reagent with a thiol-containing agent to produce at least one borosulfide compound; and

c) reacting the borosulfide compound with a reducing agent comprising hydrazine, a hydrazine derivative, or combinations thereof, to produce a mixture comprising ammonia borane.

14. The method of claim 13 , wherein the thiol-containing agent is an aromatic dithiol.

15. The method of claim 14 , wherein the aromatic dithiol comprises benzenedithiol, toluene-3,4-dithiol, or combinations thereof.

16. The method of claim 13 , wherein the reaction proceeds for a period of time of 24 hours or less.

17. A method of producing ammonia borane, comprising:

a) providing polyborazylene in a suitable solvent; and

b) combining the polyborazylene with a reducing agent comprising hydrazine, a hydrazine derivative, or combinations thereof, in a reaction which produces ammonia borane,

wherein the reaction occurs in a sealed reaction vessel at a temperature of from about 40° C. to about 60° C.

18. The method of claim 17 , wherein the solvent comprises tetrahydrofuran, hydrazine, glyme, diglyme, tetraglyme, toluene, hexane, triethylamine, diethylamine, trioctylamine, liquid ammonia, diethyl ether, and combinations thereof.

19. The method of claim 18 , wherein the solvent is liquid ammonia.

20. The method of claim 17 , wherein the ammonia borane is substantially free from byproducts.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 7, 2018
From: LOS ALAMOS NATIONAL SECURITY, LLC
To: TRIAD NATIONAL SECURITY, LLC
Reel/Frame 047447/0201 →