Mechanochemical solid/liquid reaction in formation of alane

Patent metadata

Field	Value
Publication number	US-10138122-B2
Application number	US-201715482913-A
Country	US
Kind code	B2
Filing date	Apr 10, 2017
Priority date	Apr 10, 2017
Publication date	Nov 27, 2018
Grant date	Nov 27, 2018

Abstract

Methods for forming alane are described. The method drives the alane producing chemical reaction by a mechanical energy source such as a ball mill and includes stabilization of the product with solvent. At least one of the reactants is insoluble in the solvent. Thus, the product is both stabilized and phase-separated from the reactant(s) immediately upon formation. The method can be used to form α-alane, for instance for use in hydrogen storage.

First claim

What is claimed is:

1. A method for forming alane comprising:
combining in a reactor a solid phase reactant comprising an alkali metal, an aluminum halide, and a liquid phase Lewis base, wherein the solid phase reactant comprising the alkali metal is not soluble in the Lewis base; and
repeatedly transferring mechanical energy to the reactants via the action of the reactor to encourage a mechanochemical reaction between the solid phase alkali metal containing reactant and the aluminum halide to form alane, the alane upon formation and within the reactor as the mechanochemical reaction proceeds forming a liquid phase adduct with the Lewis base.

2. The method of claim 1 , wherein the reactor comprises a shaker mill, a planetary ball mill, a jet mill, a twin-screw extruder, a rotary ball mill, or a grinder.

3. The method of claim 1 , wherein the reactor comprises a ball mill.

4. The method of claim 1 , wherein the alkali metal containing reactant comprises an alkali metal based tetrahydroaluminate, an alkali metal hydride, an alkali metal, or a combination thereof.

5. The method of claim 1 , wherein the alkali metal containing reactant comprises sodium.

6. The method of claim 1 , wherein the alkali metal containing reactant is free of lithium.

7. The method of claim 1 , wherein the aluminum halide comprises aluminum chloride, aluminum bromide, aluminum iodide, or a combination thereof.

8. The method of claim 1 , wherein a conjugate acid of the Lewis base has a pKa of about −2.5 or less.

9. The method of claim 1 , wherein the Lewis base comprises an ether or an amine.

10. The method of claim 1 , wherein the Lewis base comprises diethyl ether.

11. The method of claim 1 , wherein the Lewis base comprises, ethyl amine, diethyl amine, tri-ethyl amine, tri-methyl amine, aniline, or a combination thereof.

12. The method of claim 1 , further comprising isolating and crystallizing the alane from the adduct.

13. The method of claim 12 , wherein the isolated and crystallized alane comprises α-alane.

Assignees

• Savannah River Nuclear Solutions Llc

Inventors

• Zidan Ragaiy
• Ward Patrick A

Classifications

• C01B6/06 Primary

  Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof · CPC title

• B01J19/28

  Moving reactors, e.g. rotary drums (B01J19/08 takes precedence) · CPC title

• B01J8/10

  moved by stirrers or by rotary drums or rotary receptacles {or endless belts} · CPC title