Crystallization and stabilization in the synthesis of microcrystalline alpha alane

• US 10,435,297 B2
• Filed: 06/16/2016
• Issued: 10/08/2019
• Est. Priority Date: 06/16/1999
• Status: Active Grant

• Current Assignee: Ardica Technologies Incorporated
• Original Assignee: Ardica Technologies Incorporated
• Inventors: Stout, David, Fong, Henry, McLaughlin, Elisabeth, Penwell, Paul E., Petrie, Mark A., Wilson, Robert
• Primary Examiner(s): Butcher, Robert T
• Application Number:
  US15/184,962
• Publication Number:
  US 20160368768A1
• Time in Patent Office: 1,209 Days
• Field of Search: None
• CPC Class Codes: C01B 3/0026 of one single metal or a rare earth metal; Treatment thereof
• 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: C01D 15/04 Halides
• CPC Class Codes: Y02E 60/32 Hydrogen storage

Abstract

Systems and methods for producing microcrystalline alpha alane are provided herein. An exemplary process comprises the elimination of the crystallization aid lithium borohydride through the use of excess lithium aluminum hydride or sodium borohydride. Further exemplary processes comprise methods for passivating microcrystalline alpha alane using a weak acid in a nonaqueous solvent solution.

Claims

1. A method for producing alpha alane, comprising:

in a first chemical reaction, reacting an excess amount of lithium aluminum hydride with aluminum trichloride, and an ether with a first solvent to produce an alane etherate solution comprising alane etherate and an excess portion of the lithium aluminum hydride not consumed in the first chemical reaction, wherein the excess portion of the lithium aluminum hydride acts as a crystallization aid providing reaction sites to produce an alane etherate solution in a second chemical reaction;

removing at least a portion of the first solvent from the alane etherate solution, forming an alane etherate concentrate comprising the alane etherate and the excess portion of the lithium aluminum hydride;

after the removing at least a portion of the first solvent from the alane etherate solution to form the alane etherate concentrate, suspending the alane etherate concentrate in an aromatic solvent; and

heating the suspension to convert the alane etherate concentrate to microcrystalline alpha alane in the second chemical reaction, wherein the crystallization of the alane etherate concentrate to the microcrystalline alpha alane is aided by the excess portion of the lithium aluminum hydride carried over from the first chemical reaction.

2. The method of claim 1, wherein the alane etherate solution further comprises lithium chloride precipitate, and the method further comprises filtering the lithium chloride precipitate from the alane etherate solution prior to removing the portion of solvent from the alane etherate solution to form the alane etherate concentrate.

3. The method of claim 1, wherein the producing the alane etherate solution occurs at a temperature of approximately −

5°

C. to 0°

C.

4. The method of claim 1, wherein the heating the suspension comprises heating the suspension to a temperature of approximately 65°

C. to 80°

C.

5. The method of claim 1, wherein the first solvent comprises an aromatic solvent, a hydrocarbon solvent, or a mixture thereof.

6. The method of claim 5, wherein the first solvent comprises toluene.

7. A method for producing alpha alane, comprising:

in a first chemical reaction, reacting lithium aluminum hydride with aluminum trichloride ether, and a first solvent and sodium borohydride to produce an alane etherate solution comprising alane etherate, lithium aluminum hydride, and lithium borohydride, wherein the lithium borohydride acts as a crystallization aid providing reaction sites to produce an alane etherate solution in a second chemical reaction;

removing at least a portion of the first solvent from the alane etherate solution, forming an alane etherate concentrate comprising the alane etherate, the lithium aluminum hydride, and the lithium borohydride;

after the removing at least a portion of the first solvent from the alane etherate solution to form the alane etherate concentrate, suspending the alane etherate concentrate in an aromatic solvent; and

heating the suspension to convert the alane etherate concentrate to microcrystalline alpha alane in the second chemical reaction, wherein the crystallization of the alane etherate concentrate to the microcrystalline alpha alane is aided by the lithium borohydride produced in the first chemical reaction and carried over to the second chemical reaction.

8. The method of claim 7, wherein the alane etherate solution further comprises lithium chloride precipitate, and the method further comprises filtering the lithium chloride precipitate from the alane etherate solution prior to removing the portion of solvent from the alane etherate solution to form the alane etherate concentrate.

9. The method of claim 7, wherein the producing the alane etherate solution occurs at a temperature of approximately −

5°

C. to 0°

C.

10. The method of claim 7, wherein the heating the suspension comprises heating the suspension to a temperature of approximately 65°

C. to 80°

C.

11. The method of claim 7, wherein the first solvent comprises an aromatic solvent, a hydrocarbon solvent, or a mixture thereof.

12. The method of claim 11, wherein the first solvent comprises toluene.