Obtaining a solid form containing heat-stabilized borazane, said solid form, and the use thereof for generating hydrogen

Patent metadata

Field	Value
Publication number	US-9663360-B2
Application number	US-201414894646-A
Country	US
Kind code	B2
Filing date	May 28, 2014
Priority date	May 30, 2013
Publication date	May 30, 2017
Grant date	May 30, 2017

Abstract

A process for obtaining a solid form containing heat-stabilized borazane is described. The solid form is capable of generating hydrogen by thermal decomposition or by a self-maintained combustion reaction. Within the solid form containing borazane, the borazane is heat-stabilized. It has thus been heat-stabilized by making an oxidized layer at its surface.

First claim

The invention claimed is:

1. A process for obtaining a solid form containing heat-stabilized borazane, said solid form being capable of generating hydrogen by thermal decomposition or by a self-maintained combustion reaction, said process comprising:
a) making available at least one solid form of borazane chosen from grains of pulverulent powder, granules, pellets, blocks, and mixtures thereof,
b) heat treating said at least one solid form of borazane, in air, at a temperature of between 50 and 85° C., the heat treatment generating an oxidized layer at its surface; said at least one heat-treated solid form of borazane then constituting a solid form containing heat-stabilized borazane, which is capable of generating hydrogen by thermal decomposition; and
c1) recovering said at least one solid form containing heat-stabilized borazane, which is capable of generating hydrogen by thermal decomposition; or
c2) mixing said at least one solid form of borazane, chosen from grains of pulverulent powder and/or granules, heat-treated, with at least one inorganic oxidizing agent, which is in the form of a pulverulent powder and/or of granules; a resulting mixture, containing said at least one heat-treated solid form of borazane and said at least one inorganic oxidizing agent, then constituting a solid form containing heat-stabilized borazane, which is capable of generating hydrogen by a self-maintained combustion reaction, and recovering said at least one solid form containing heat-stabilized borazane, which is capable of generating hydrogen by a self-maintained combustion reaction; or
c3) mixing said at least one solid form of borazane, chosen from grains of pulverulent powder and/or granules, heat-treated, with at least one inorganic oxidizing agent, which is in the form of a pulverulent powder and/or of granules, followed by forming the resulting mixture to obtain pellets and/or blocks containing said at least one heat-treated solid form of borazane and said at least one oxidizing agent; said formed mixture containing said at least one heat-treated solid form of borazane and said at least one inorganic oxidizing agent then constituting a solid form containing heat-stabilized borazane, which is capable of generating hydrogen by a self-maintained combustion reaction, and recovering said at least one solid form containing heat-stabilized borazane, which is capable of generating hydrogen by a self-maintained combustion reaction.

2. The process as claimed in claim 1 , wherein said heat treatment is performed at atmospheric pressure.

3. The process as claimed in claim 1 , wherein said heat treatment is performed at a temperature of between 70 and 85° C.

4. The process as claimed in claim 1 , wherein said heat treatment is performed for several hours.

5. The process as claimed in claim 1 , wherein said oxidized layer consists essentially of ammonium borate of the type B5, which is tetrahydrated ammonium borate of formula NH 4 B 5 O 8 .4H 2 O.

6. The process as claimed in claim 1 , wherein said oxidized layer has a weight which represents less than 10% of a total weight of said at least one heat-treated solid form of borazane.

7. The process as claimed in claim 1 , wherein said oxidized layer has a weight which represents from 0.2% to 5% of a total weight of said at least one heat-treated solid form of borazane.

8. The process as claimed in claim 1 , comprising the mixing step, said at least one inorganic oxidizing agent being chosen from perchlorates, dinitroamides, nitrates and metal oxides, and mixtures thereof.

9. The process as claimed in claim 1 , comprising the mixing step and the forming step, said forming being performed via a dry route.

10. A solid form containing heat-stabilized borazane, which is capable of generating hydrogen by thermal decomposition or by a self-maintained combustion reaction, which may be obtained via the process as claimed in claim 1 .

11. The solid form as claimed in claim 10 , chosen from:
grains of pulverulent borazane powder coated with an oxidized layer, borazane granules coated with an oxidized layer, borazane pellets coated with an oxidized layer, borazane blocks coated with an oxidized layer, and mixtures thereof, and
mixtures of grains of pulverulent powders and/or of granules, pellets and/or blocks, containing grains of powder and/or of granules of borazane coated with an oxidized layer and grains of powders and/or granules of at least one inorganic oxidizing agent.

12. The solid form as claimed in claim 11 , said oxidized layer consisting essentially of ammonium borate of the type B5, which is tetrahydrated ammonium borate of formula NH 4 B 5 O 8 .4H 2 O.

13. The solid form as claimed in claim 11 , said oxidized layer representing less than 10% by weight of a total weight of said grains of pulverulent powder, granules, disks, pellets and/or blocks, coated with said oxidized layer.

14. The solid form as claimed in claim 11 , said at least one inorganic oxidizing agent being chosen from perchlorates, dinitroamides, nitrates, metal oxides, and mixtures thereof.

15. A process for generating hydrogen, comprising a thermal decomposition or the self-maintained combustion of a solid form containing borazane, wherein said solid form containing borazane is a solid form as claimed in claim 10 .

16. A process for generating hydrogen, comprising a thermal decomposition or the self-maintained combustion of a solid form containing borazane, wherein said solid form containing borazane is a solid form obtained according to the process of claim 1 .

17. The process as claimed in claim 4 , wherein said heat treatment is performed between 5 and 25 hours.

18. The process as claimed in claim 8 , wherein said at least one inorganic oxidizing agent is chosen from ammonium perchlorate, ammonium dinitroamide, strontium nitrate and iron oxide.

19. The solid form as claimed in claim 13 , wherein said oxidized layer represents from 0.2% to 5% by weight of the total weight of said grains of pulverulent powder, granules, disks, pellets and/or blocks, coated with said oxidized layer.

20. The solid form as claimed in claim 14 , wherein said at least one inorganic oxidizing agent is chosen from ammonium perchlorate, ammonium dinitroamide, strontium nitrate and iron oxide.

Assignees

• Herakles
• Centre Nat Rech Scient
• Centre Nat De La Rech Scient (Cnrs)

Inventors

• Blanchard Hélène
• Renouard Joël A
• Darwiche Ali
• Janot Raphaël L

Classifications

• Y02E60/36

  Hydrogen production from non-carbon containing sources, e.g. by water electrolysis · CPC title

• Y02E60/364

  Cross-Sectional Technologies · mapped topic

• C01B2203/1205

  Composition of the feed · CPC title

• C01B2203/0266

  containing a decomposition step · CPC title

• C06D5/04

  by auto-decomposition of single substances · CPC title