Synthesis of microcrystalline alpha alane

• US 9,676,625 B1
• Filed: 11/07/2012
• Issued: 06/13/2017
• Est. Priority Date: 11/07/2011
• Status: Active Grant

• Current Assignee: Ardica Technologies Incorporated
• Original Assignee: Ardica Technologies Incorporated
• Inventors: Petrie, Mark A., Stout, David, Penwell, Paul E., Suman, Sigridur, Dodge, Allen
• Primary Examiner(s): Chung, Susannah
• Assistant Examiner(s): Butcher, Robert T
• Application Number:
  US13/671,090
• Time in Patent Office: 1,679 Days
• Field of Search: None
• CPC Class Codes: C01B 3/0078 Composite solid storage mediums, i.e. coherent or loose mixtures of different solid constituents, chemically or structurally heterogeneous solid masses, coated solids or solids having a chemically modified surface region
• CPC Class Codes: C01B 6/06 Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
• CPC Class Codes: H01M 10/26 Selection of materials as electrolytes
• CPC Class Codes: H01M 8/065 by dissolution of metals or alloys; by dehydriding metallic substances
• CPC Class Codes: Y02E 60/10 Energy storage using batteries
• CPC Class Codes: Y02E 60/32 Hydrogen storage
• CPC Class Codes: Y02E 60/50 Fuel cells

Abstract

Systems and methods for producing microcrystalline alpha alane are provided herein. An exemplary process for producing microcrystalline alpha alane includes reacting lithium aluminum hydride and aluminum chloride in a solvent to produce alane etherate, filtering alane etherate from the reactant, combining the filtered alane etherate with a lithium borohydride solution to produce solids that include microcrystalline alane etherate, removing remaining solvent from the solids, creating a slurry from the solids and an aromatic solvent, and heating the slurry to convert the microcrystalline alane etherate to microcrystalline alpha alane.

Claims

1. A method, comprising:

reacting lithium aluminum hydride and aluminum trichloride in an ether solvent to produce an alane etherate solution comprising alane etherate, lithium aluminum hydride, and lithium chloride precipitate;

filtering the lithium chloride precipitate from the alane etherate solution;

removing a portion of the ether solvent from the alane etherate solution to create a slurry, the slurry comprising alane etherate, lithium aluminum hydride, and ether;

adding approximately 110 milliliters of aromatic solvent per 20 grams of microcrystalline alpha alane expected; and

heating the slurry to convert the alane etherate to obtain microcrystalline alpha alane.

2. The method according to claim 1, wherein the reacting occurs over a range of temperatures of approximately −

15°

C. to 0°

C., inclusive.

3. The method according to claim 1, further comprising combining the filtered alane etherate solution with a lithium borohydride solution.

4. The method according to claim 1, wherein the heating includes increasing a temperature of the slurry to between approximately 70°

C. to 72°

C., inclusive, for a given period of time.

5. The method according to claim 1, wherein the heating includes increasing a temperature of the slurry to between approximately 60°

C. to 80°

C., inclusive, for a given period of time.

6. The method according to claim 1, further comprising rinsing the heated slurry with a solvent and filtering the solvent from the microcrystalline alpha alane.

7. The method according to claim 1, wherein the aromatic solvent is combined with an aliphatic solvent.

8. The method according to claim 1, further comprising passivating the microcrystalline alpha alane by combining the microcrystalline alpha alane with a non-aqueous solvent and an acid to create an aluminum oxide coating on the microcrystalline alpha alane.

9. The method according to claim 1, further comprising passivating the microcrystalline alpha alane by combining the microcrystalline alpha alane directly with an acid and without a non-aqueous solvent, to create an aluminum oxide coating on the microcrystalline alpha alane.

10. The method according to claim 3, further comprising reacting the slurry with an acid to remove alane polymorphs, aluminum metal, and residual lithium borohydride and lithium aluminum hydride.

11. The method according to claim 8, wherein the non-aqueous solvent is an organic solvent miscible with water.

12. The method according to claim 8, wherein the non-aqueous solvent comprises dimethoxyethane and an organic solvent that is miscible with water.

13. The method according to claim 1, wherein the removing a portion of the ether solvent to create a slurry is accomplished by vacuum distillation.

14. The method according to claim 1, wherein the aromatic solvent is a toluene solvent.

15. The method according to claim 1, wherein the removing a portion of the ether solvent to create a slurry comprises removing an amount between 75% to 90% of the ether from the alane etherate solution.