Heating methods for aluminum hydride production

• US 10,233,079 B2
• Filed: 06/15/2016
• Issued: 03/19/2019
• Est. Priority Date: 06/16/1999
• Status: Active Grant

• Current Assignee: Ardica Technologies Incorporated
• Original Assignee: Ardica Technologies Incorporated
• Inventors: Stout, David, McLaughlin, Elisabeth, Fong, Henry, Hum, Georgina, Penwell, Paul E., Wilson, Robert, Petrie, Mark A.
• Primary Examiner(s): Butcher, Robert T
• Application Number:
  US15/183,626
• Publication Number:
  US 20160297678A1
• Time in Patent Office: 1,007 Days
• Field of Search: None
• CPC Class Codes: B01J 19/02 Apparatus characterised by being constructed of material selected for its chemically-resistant properties
• CPC Class Codes: B01J 2219/00495 Means for heating or cooling the reaction vessels
• CPC Class Codes: B01J 2219/0059 Sequential processes
• CPC Class Codes: B01J 2219/00716 Heat activated synthesis
• CPC Class Codes: B01J 2219/0075 Metal based compounds
• CPC Class Codes: B01J 2219/0245 of synthetic organic material
• 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

Abstract

Disclosed herein are systems and methods for heating alane etherate compositions for producing microcrystalline alpha alane. An exemplary heating method comprises introducing a preheated solvent into the alane etherate composition and rapidly stirring to effectuate rapid heating of the composition without the need to heat the reactor walls. In this way, the alane etherate composition can be heated while also reducing the risk of decomposition. In further embodiments, a two-stage reactor can be employed for producing alpha alane, wherein the heating occurs in the second stage.

Claims

1. A process for manufacture of aluminum hydride in a reactor, the process comprising:

creating a slurry from alane etherate, diethyl ether and toluene;

combining the slurry with a preheated toluene solution in the reactor, accomplishing initial heating of the slurry by the preheated toluene solution to a temperature of 68°

C. to 82°

C.;

applying heat to the reactor to further elevate the temperature of reactor contents; and

maintaining the temperature of the reactor to hold the reactor contents at the elevated temperature to complete a transition of alane etherate to aluminum hydride.

2. The process of claim 1, wherein the preheated toluene solution is preheated to approximately 85°

C.

3. The process of claim 1, wherein the temperature of the reactor contents is elevated to a range of 65°

C. -82°

C.

4. The process of claim 1, wherein the aluminum hydride is an alpha polymorph of aluminum hydride.

5. The process of claim 1, wherein the slurry further comprises lithium aluminum hydride and lithium borohydride.

6. The process of claim 1, wherein the preheated toluene solution is in gaseous form.

7. The process of claim 1, wherein the preheated toluene solution is in liquid form.

8. The process of claim 1, wherein the applying heat to the reactor further comprises heating the reactor contents in 10 minutes or less to elevate the reactor contents to a temperature range of 68°

C. to 82°

C.

9. The process of claim 1, wherein the preheated toluene solution comprises toluene vapor and an inert gas.

10. The process of claim 1, wherein the preheated toluene solution comprises toluene and ether.

11. The process of claim 1, wherein the applying heat to the reactor to elevate a temperature of reactor contents comprises applying heat to an external wall of the reactor.

12. The process of claim 1, wherein the applying heat to the reactor to elevate the temperature of reactor contents comprises applying an external heating loop with a filter to the reactor.

13. The process of claim 1, wherein the applying heat to the reactor to elevate the temperature of reactor contents comprises applying microwave heating to elevate the temperature of the reactor contents.

14. The process of claim 1, wherein the applying heat to the reactor to elevate the temperature of reactor contents comprises applying IR heating to elevate the temperature of the reactor contents.

15. The process of claim 1, wherein the applying heat to the reactor to elevate the temperature of the reactor contents is done in 15 minutes or less.