METHOD OF PREPARATION OF ALANE-ETHERATE AND ALANE
The invention to preparing alane-etherate and alane by producing an alane-etherate complex using an acid including one or a combination of hydrochloric acid and methanesulfonic acid and a metal tetrahydroaluminate in a solvent including an ether such as diethyl ether. The alane-etherate can be desolvated using a spray desolvation process such as electrospraying.
1 . A method of producing solid α-alane comprising:
(a) reacting one or more acids, selected from hydrochloric acid and methanesulfonic acid, with one or more metal tetrahydroaluminates in a solvent comprising an ether to form an alane-ether mixture;
(b) removing the solvent from the alane-ether mixture by spray desolvation; and
(c) collecting the solid α-alane.
2 . The method of claim 1 , wherein the one or more acids consist of one or a combination of hydrochloric acid and methane sulfonic acid.
3 . The method of claim 2 , wherein the one or more acids consist of at least one of hydrochloric acid and methanesulfonic acid.
4 . (canceled)
5 . The method of claim 1 , wherein the one or more metal tetrahydroaluminates comprise LiAlH 4 .
6 . The method of claim 1 , wherein the one or more metal tetrahydroaluminates comprise NaAlH 4 .
7 . The method of claim 1 , wherein the solvent comprises diethyl ether.
8 . The method of claim 1 further comprising:
heating the solid α-alane at a temperature in a range of from greater than 60° C. to less than 120° C.
9 . (canceled)
10 . The method of claim 1 , wherein the spray desolvation comprises electrospinning.
11 . The method of claim 1 , wherein the spray desolvation comprises electrospraying.
12 . (canceled)
13 . The method of claim 8 , wherein the temperature is at least 65° C.
14 . The method of claim 13 , wherein the temperature is no greater than 100° C.
15 . The method of claim 1 , wherein desolvating the alane-ethereate complex comprises collecting electrosprayed material and annealing the collected electrosprayed material at a temperature of from 65° C. to 100° C. to form the α-alane.
16 . A composition prepared by the method of claim 1 , wherein the α-alane has a uniform particle size in a range of from 100 nm to 1000 nm.
17 . A composition prepared by the method of claim 16 , wherein the α-alane has a uniform particle size in a range of from 100 nm to 300 nm.
18 . A composition prepared by the method of claim 16 , wherein the α-alane has a uniform particle size in a range of from 500 nm to 1000 nm.