IP Library Granted Patent US 7,101,449
Granted Patent B2
US 7,101,449 · App. 10/646,419 · Granted Sep 5, 2006

Method for recovery of nitramines from aluminized energetic materials

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Quick Facts
Patent No.
US 7,101,449
App. No.
10/646,419
Granted
Sep 5, 2006
Kind
B2
Abstract

Nitramines are one of the more expensive and often the more plentiful ingredients found in energetic materials, such as solid rocket motor propellants, explosives, and pyrotechnics. By treating aluminized energetic material with an aqueous nitric acid solution containing not more than 55% by weight aqueous nitric acid at a weight ratio of aqueous nitric acid to energetic material of about 4:1 to about 6:1, most constituents of conventional aluminized energetic materials are digested into solution, with the exception of nitramines, which remain substantially insoluble in the aqueous nitric acid and can be recovered without requiring recrystallization of the nitramines. A mineral acid other than nitric acid, preferably hydrochloric acid, may be added to increase the rate of aluminum digestion. Treatment of the energetic material can be performed without volatile organic solvents, thus obviating ecological, cost, and safety concerns raised by the use of volatile organic solvents.

Claims (29)

1. A method of recovering a nitramine from a nitramine-containing aluminized energetic material, comprising:

treating a nitramine-containing aluminized energetic material comprising aluminum, a nitramine, and at least one binder in aqueous nitric acid to digest the at least one binder into solution while neither solvating nor solvolyzing into solution at least substantially all of the nitramine; and

recovering at least a portion of the nitramine.

2. The method of claim 1 , wherein treating the nitramine-containing aluminized energetic material further comprises adding at least one plasticizer to the aluminum, the nitramine, and the at least one binder, and wherein treating the nitramine-containing aluminized energetic material further comprises digesting the at least one plasticizer into solution.

3. The method of claim 1 , wherein treating the nitramine-containing aluminized energetic material further comprises adding at least one plasticizer and at least one inorganic oxidizer to the aluminum, the nitramine, and the at least one binder, and wherein treating the nitramine-containing aluminized energetic material further comprises digesting the at least one plasticizer and the at least one inorganic oxidizer into solution.

4. The method of claim 1 , wherein treating the nitramine-containing aluminized energetic material comprising the aluminum, the nitramine, and the at least one binder in aqueous nitric acid comprises treating the nitramine-containing aluminized energetic material comprising the aluminum, the nitramine, and the at least one binder in aqueous nitric acid comprising at least 5 weight percent nitric acid.

5. The method of claim 1 , wherein treating the nitramine-containing aluminized energetic material comprising the aluminum, the nitramine, and the at least one binder in aqueous nitric acid comprises treating the nitramine-contaiing aluminized energetic material comprising the aluminum, the nitramine, and the at least one binder in aqueous nitric acid comprising at least 20 weight percent nitric acid.

6. The method of claim 1 , wherein treating the nitramine-containing aluminized energetic material comprising the aluminum, the nitramine, and the at least one binder in aqueous nitric acid comprises treating the nitramine-containing aluminized energetic material comprising the aluminum, the nitramine, and the at least one binder in aqueous nitric acid comprising at least 35 weight percent nitric acid.

7. The method of claim 1 , wherein treating the nitramine-containing aluminized energetic material comprising the aluminum, the nitramine, and the at least one binder in aqueous nitric acid comprises treating the nitramine-containing aluminized energetic material comprising the aluminum, the nitramine and the at least one binder in aqueous nitric acid comprising not more than 55 weight percent nitric acid.

8. The method of claim 1 , wherein treating the nitramine-containing aluminized energetic material comprising the aluminum, the nitramine, and the at least one binder in aqueous nitric acid comprises neither solvating nor solvolyzing at least 98% of the nitramine of the nitramine-containing aluminized energetic material into solution.

9. The method of claim 1 , wherein treating the nitramine-containing aluminized energetic material comprising the aluminum, the nitramine, and the at least one binder in aqueous nitric acid comprises neither solvating nor solvolyzing at least 99% of the nitramine of the nitramine-containing aluminized energetic material into solution.

10. The method of claim 1 , further comprising using digested portions of the nitramine-containing aluminized energetic material and residual nitric acid as feed stock for commercial blasting agents.

11. The method of claim 1 , wherein recovering the at least a portion of the nitramine comprises recovering at least 90 weight percent of the nitramine.

12. The method of claim 1 , wherein treating the nitramine-containing aluminized energetic material comprising the aluminum, the nitramine, and the at least one binder in aqueous nitric acid comprises treating the nitramine-contaiing aluminized energetic material comprising the aluminum, the nitramine comprising at least one member selected from the group consisting of 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane (HMX), 1,3,5-trinitro-1,3,5-triazacyclohexane (RDX), 4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo[5.5.0.0 5,9 0 3,11 ]dodecane) (TEX), and 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetracyclo[5.5.0.0 5,9 0 3,11 ]dodecane (CL-20), and the at least one binder in aqueous nitric acid.

13. The method of claim 1 , wherein treating the nitramine-containing aluminized energetic material comprising the aluminum, the nitramine, and the at least one binder in aqueous nitric acid comprises using a weight ratio of the aqueous nitric acid to the nitramine-containing aluminized energetic material in a range of about 4:1 to about 6:1.

14. A method of recovering 1,3,5,7-tetranitro-1,3,5,7-tetraaza-cyclooctane (HMX) from an aluminized energetic material, comprising:

treating an aluminized energetic material comprising aluminum, HMX, and at least one binder in aqueous nitric acid to digest the at least one binder into solution while neither solvating nor solvolyzing into solution at least substantially all of the HMX; and

recovering at least a portion of the HMX.

15. The method of claim 14 , wherein treating the aluminized energetic material further comprises adding at least one plasticizer to the aluminum, the HMX, and the at least one binder, and wherein treating the aluminized energetic material further comprises digesting the at least one plasticizer into solution.

16. The method of claim 14 , wherein treating the aluminized energetic material further comprises adding at least one plasticizer and at least one inorganic oxidizer to the aluminum, the HMX and the at least one binder, and wherein treating the aluminized energetic material further comprises digesting the at least one plasticizer and the inorganic oxidizer into solution.

17. The method of claim 14 , wherein treating the aluminized energetic material comprising the aluminum, the HMX, and the at least one binder in aqueous nitric acid comprises treating the alumiized energetic material comprising the aluminum, the HMX, and the at least one binder in aqueous nitric acid comprising at least 5 weight percent nitric acid.

18. The method of claim 14 , wherein treating the aluminized energetic material comprising the aluminum, the HMX and the at least one binder in aqueous nitric acid comprises treating the aluminized energetic material comprising the aluminum, the HMX, and the at least one binder in aqueous nitric acid comprising at least 20 weight percent nitric acid.

19. The method of claim 14 , wherein treating the aluminized energetic material comprising the aluminum, the HMX, and the at least one binder in aqueous nitric acid comprises treating the aluminized energetic material comprising the aluminum the HMX, and the at least one binder in aqueous nitric acid comprising at least 35 weight percent nitric acid.

20. The method of claim 14 , wherein treating the aluminized energetic material comprising the aluminum, the HMX, and the at least one binder in aqueous nitric acid comprises treating the aluminized energetic material comprising the aluminum, the HMX, and the at least one binder in aqueous nitric acid comprising not more than 55 weight percent nitric acid.

21. The method of claim 14 , wherein treating the aluminized energetic material comprising the aluminum, the HMX, and the at least one binder in aqueous nitric acid comprises neither solvating nor solvolyzing at least 98% of the HMX of the aluminized energetic material into solution.

22. The method of claim 14 , wherein treating the aluminized energetic material comprising the aluminum, the HMX, and the at least one binder in aqueous nitric acid comprises neither solvating nor solvolyzing at least 99% of the HMX of the aluminized energetic material into solution.

23. The method of claim 14 , further comprising using digested portions of the aluminized energetic material and residual nitric acid as feed stock for commercial blasting agents.

24. The method of claim 14 , wherein recovering the at least a portion of the HMX comprises recovering at least 90 weight percent of the HMX.

25. The method of claim 14 , wherein treating the aluminized energetic material comprising the aluminum, the HMX and the at least one binder in aqueous nitric acid comprises using a weight ratio of the aqueous nitric acid to the aluminized energetic material in a range of about 4:1 to about 6:1.

Assignments (9)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 8, 2021
From: NORTHROP GRUMMAN INNOVATION SYSTEMS LLC
To: NORTHROP GRUMMAN SYSTEMS CORPORATION
Reel/Frame 055256/0892 →
CHANGE OF NAME Recorded Feb 4, 2021
From: NORTHROP GRUMMAN INNOVATION SYSTEMS, INC.
To: NORTHROP GRUMMAN INNOVATION SYSTEMS LLC
Reel/Frame 055223/0425 →
CHANGE OF NAME Recorded Nov 1, 2018
From: ORBITAL ATK, INC.
To: NORTHROP GRUMMAN INNOVATION SYSTEMS, INC.
Reel/Frame 047400/0381 →
RELEASE OF SECURITY INTEREST Recorded Oct 8, 2015
From: BANK OF AMERICA, N.A.
To: ALLIANT TECHSYSTEMS INC.; FEDERAL CARTRIDGE CO.; EAGLE INDUSTRIES UNLIMITED, INC.; AMMUNITION ACCESSORIES, INC.; ORBITAL ATK, INC. (F/K/A ALLIANT TECHSYSTEMS INC.)
Reel/Frame 036816/0624 →
CHANGE OF NAME Recorded May 22, 2015
From: ALLIANT TECHSYSTEMS INC.
To: ORBITAL ATK, INC.
Reel/Frame 035753/0373 →
SECURITY AGREEMENT Recorded Nov 4, 2010
From: ALLIANT TECHSYSTEMS INC.; AMMUNITION ACCESSORIES INC.; ATK COMMERCIAL AMMUNITION COMPANY INC.; ATK COMMERCIAL AMMUNITION HOLDINGS COMPANY; ATK LAUNCH SYSTEMS INC.; ATK SPACE SYSTEMS INC.; FEDERAL CARTRIDGE COMPANY; EAGLE INDUSTRIES UNLIMITED, INC.; EAGLE MAYAGUEZ, LLC; EAGLE NEW BEDFORD, INC.
To: BANK OF AMERICA, N.A.
Reel/Frame 025321/0291 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 18, 2007
From: THIOKOL PROPULSION CORP.
To: ALLIANT TECHSYSTEMS INC.
Reel/Frame 019171/0604 →
CHANGE OF NAME Recorded Mar 22, 2007
From: CORDANT TECHNOLOGIES INC.
To: THIOKOL PROPULSION CORP.
Reel/Frame 019047/0266 →
SECURITY INTEREST Recorded May 28, 2004
From: ALLIANT AMMUNITION AND POWDER COMPANY LLC; ALLIANT TECHSYSTEMS INC.; ALLIANT AMMUNITION SYSTEMS COMPANY LLC; ALLIANT HOLDINGS LLC; ALLIANT INTERNATIONAL HOLDINGS INC.; ALLIANT LAKE CITY SMALL CALIBER AMMUNITION COMPANY LLC; ALLIANT PROPULSION AND COMPOSITES LLC; ALLIANT SOUTHER COMPOSITES COMPANY LLC; AMMUNITION ACCESSORIES INC.; ATK AEROSPACE COMPANY INC.; ATK AMMUNITION AND RELATED PRODUCTS LLC; ATK COMMERCIAL AMMUNITION COMPANY INC.; ATK ELKTON LLC; ATK INTERNATIONAL SALES INC.; ATK LOGISTICS AND TECHNICAL SERVICES LLC; ATK MISSILE SYSTEMS COMPANY LLC; ATK ORDNANCE AND GROUND SYSTEMS LLC; ATK PRECISION SYSTEMS LLC; ATK TACTICAL SYSTEMS COMPANY LLC; COMPOSITE OPTICS, INCORPORATED; FEDERAL CARTRIDGE COMPANY; GASL, INC.; MICRO CRAFT INC.; MISSION RESEARCH CORPORATION; NEW RIVER ENERGETICS, INC.; THIOKOL TECHNOLOGIES INTERNATIONAL, INC.
To: BANK OF AMERICA, N.A.
Reel/Frame 015018/0254 →