Formation of high quality alane

Patent metadata

Field	Value
Publication number	US-11453585-B2
Application number	US-201916525898-A
Country	US
Kind code	B2
Filing date	Jul 30, 2019
Priority date	Jul 30, 2019
Publication date	Sep 27, 2022
Grant date	Sep 27, 2022

Abstract

Methods for forming alane are described. The method includes addition of toluene at a temperature above the crystallization temperature of alane to a lower temperature solution that includes alane adduct, ether, and toluene. Upon the addition, a crystallization mixture is formed that is at or near the crystallization temperature of alane. The alane of the mixture crystallizes over a period of time to form a high purity alane polymorph.

First claim

What is claimed is:

1. A method for forming alane comprising:
combining an alane adduct, an ether, and a first amount of toluene to form a liquid mixture, the liquid mixture including the ether in an amount of from about 1 vol. % to about 50 vol. %;
adding a second amount of toluene to the liquid mixture to form a crystallization mixture, wherein at the addition, the liquid mixture is at a temperature of from about 15° C. to about 45° C. and the second amount of toluene is at a temperature that is greater than the crystallization temperature of the alane, wherein upon the addition, the crystallization mixture thus formed is at a temperature of from about 70° C. to about 80° C.; and
maintaining the crystallization mixture at a temperature of from about 70° C. to about 80° C. for a period of from about 2 hours to about 5 hours, the alane of the alane adduct polymerizing during the period.

2. The method of claim 1 , wherein the alane adduct is an alane etherate adduct.

3. The method of claim 1 , wherein the liquid mixture includes the ether in an amount of from about 1 vol. % to about 15 vol. %.

4. The method of claim 1 , wherein the liquid mixture includes the ether in an amount of from about 25 vol. % to about 50 vol. %.

5. The method of claim 1 , wherein the ether comprises diethyl ether.

6. The method of claim 1 , wherein the second amount of toluene is at a temperature of from about 65° C. to about 110° C.

7. The method of claim 1 , wherein the second amount of toluene is at a temperature of from about 65° C. to about 100° C.

8. The method of claim 1 , wherein the second amount of toluene is at a temperature of from about 85° C. to about 110° C.

9. The method of claim 1 , further comprising distilling the ether from the crystallization mixture during the period.

10. The method of claim 1 , further comprising passivating the crystalized alane.

11. The method of claim 1 , the polymerized alane comprising α-alane in an amount of about 99% or greater.

12. The method of claim 1 , the polymerized alane comprising α′-alane in an amount of about 99% or greater.

13. The method of claim 1 , the polymerized alane comprising γ-alane in an amount of about 99% or greater.

14. A method for forming α-alane comprising:
combining an alane adduct, an ether, and a first amount of toluene to form a liquid mixture, the liquid mixture including the ether in an amount of from about 1 vol. % to about 15 vol. %;
adding a second amount of toluene to the liquid mixture to form a crystallization mixture, wherein at the addition, the liquid mixture is at a temperature of from about 15° C. to about 45° C. and the second amount of toluene is at a temperature of from about 85° C. to about 110°, wherein upon the addition, the crystallization mixture thus formed is at a temperature of from about 70° C. to about 80° C.;
maintaining the crystallization mixture at a temperature of from about 70° C. to about 80° C. for a period of from about 3 hours to about 5 hours; and
distilling the ether from the crystallization mixture during the period, the alane of the alane adduct polymerizing during the period, the polymerized alane comprising α-alane in an amount of about 99% or greater.

15. The method of claim 14 , wherein the alane adduct is an alane etherate adduct.

16. The method of claim 14 , wherein the ether comprises diethyl ether.

17. The method of claim 14 , further comprising passivating the polymerized alane.

18. The method of claim 14 , further comprising drying the polymerized alane.

19. The method of claim 14 , the polymerized alane comprising α-alane in an amount of about 99.9% or greater.

Assignees

• Savannah River Nuclear Solutions Llc

Inventors

• Zidan Ragaiy
• Mcwhorter Christopher S
• 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

• B01D9/005

  Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof · CPC title

• C01P2006/80

  Compositional purity · CPC title

• B01D9/0054

  Use of anti-solvent · CPC title

• B01D9/0063

  Control or regulation (control per se G05) · CPC title