Methods for producing DEMN eutectic

Patent metadata

Field	Value
Publication number	US-9650307-B2
Application number	US-201313804148-A
Country	US
Kind code	B2
Filing date	Mar 14, 2013
Priority date	Mar 14, 2013
Publication date	May 16, 2017
Grant date	May 16, 2017

Abstract

A method of producing DEMN eutectic comprises reacting a reactant mixture comprising ethylenediamine and diethylenetriamine with aqueous nitric acid to form a reaction mixture comprising diethylentriamine trinitrate and ethylenediamine dinitrate. The reaction mixture is combined with methylnitroguanidine and nitroguanidine to form an aqueous slurry. Water is removed from the aqueous slurry. A method of producing an energetic composition, and a system for producing DEMN eutectic are also described.

First claim

What is claimed is:

1. A method of producing DEMN eutectic, comprising:
reacting a reactant mixture comprising ethylenediamine and diethylenetriamine with aqueous nitric acid to form a reaction mixture comprising diethylentriamine trinitrate and ethylenediamine dinitrate;
combining the reaction mixture with methylnitroguanidine and nitroguanidine to form an aqueous slurry; and
removing water from the aqueous slurry.

2. The method of claim 1 , wherein the aqueous nitric acid comprises from about 60 percent by weight nitric acid to about 75 percent by weight nitric acid, and from about 40 percent by weight water to about 25 percent by weight water.

3. The method of claim 1 , wherein reacting a reactant mixture comprising ethylenediamine and diethylenetriamine with aqueous nitric acid comprises reacting the reactant mixture with the aqueous nitric acid at a temperature of from about 10° C. to about 90° C.

4. The method of claim 1 , wherein reacting a reactant mixture comprising ethylenediamine and diethylenetriamine with aqueous nitric acid comprises reacting the reactant mixture with the aqueous nitric acid at a temperature of from about 35° C. to about 55° C.

5. The method of claim 1 , wherein reacting a reactant mixture comprising ethylenediamine and diethylenetriamine with aqueous nitric acid comprises controlling a ratio of the reactant mixture to the aqueous nitric acid such that the reaction mixture exhibits a pH within a range of from about 0 to about 7.

6. The method of claim 1 , wherein reacting a reactant mixture comprising ethylenediamine and diethylenetriamine with aqueous nitric acid comprises controlling a ratio of the reactant mixture to the aqueous nitric acid such that the reaction mixture exhibits a pH within a range of from about 3 to about 5.

7. The method of claim 1 , wherein combining the reaction mixture with methylnitroguanidine and nitroguanidine comprises combining at least one of methylnitroguanidine in water and nitroguanidine in water with the reaction mixture.

8. The method of claim 1 , wherein combining the reaction mixture with methylnitroguanidine and nitroguanidine comprises combining at least one of solid methylnitroguanidine and solid nitroguanidine with the reaction mixture.

9. The method of claim 1 , wherein removing water from the aqueous slurry comprises heating the aqueous slurry at a temperature of from about 50° C. to about 150° C.

10. The method of claim 1 , wherein removing water from the aqueous slurry comprises heating the aqueous slurry at a temperature of from about 90° C. to about 110° C.

11. The method of claim 1 , further comprising exposing the aqueous slurry to at least one of negative pressure and air sparge while removing water from the aqueous slurry.

12. The method of claim 1 , wherein removing water from the aqueous slurry comprises heating the aqueous slurry for a sufficient time to form a molten DEMN eutectic comprising ethylenediamine dinitrate, diethylentriamine trinitrate, methylnitroguanidine, nitroguanidine, and from about 0.1 percent by weight water to about 2 percent by weight water.

13. The method of claim 1 , wherein heating the aqueous slurry to remove water therefrom comprises heating the aqueous slurry for a sufficient time to form molten DEMN eutectic comprising ethylenediamine dinitrate, diethylentriamine trinitrate, methylnitroguanidine, nitroguanidine, and from about 0.3 percent by weight water to about 0.5 percent by weight water.

14. The method of claim 1 , wherein reacting a reactant mixture comprising ethylenediamine and diethylenetriamine with aqueous nitric acid and combining the reaction mixture with methylnitroguanidine and nitroguanidine comprises reacting the reactant mixture with aqueous nitric acid and combining the reaction mixture with methylnitroguanidine and nitroguanidine in a single vessel.

15. A method producing DEMN eutectic, comprising:
reacting a reactant mixture comprising ethylenediamine and diethylenetriamine with an aqueous solution comprising from about 60 percent by weight nitric acid to about 75 percent by weight nitric acid at a temperature of from about 10° C. to about 90° C. to form a reaction mixture comprising ethylenediamine dinitrate and diethylentriamine trinitrate and exhibiting a pH within a range of from about 0 to about 7;
combining the reaction mixture with methylnitroguanidine and nitroguanidine to form an aqueous slurry; and
heating the aqueous slurry at a temperature of from about 50° C. to about 150° C. and under at least one of negative pressure and air sparge to form a eutectic composition comprising ethylenediamine dinitrate, diethylentriamine trinitrate, methylnitroguanidine, nitroguanidine, and from about 0.1 percent by weight water to about 2 percent by weight water.

16. The method of claim 15 , further comprising cooling the eutectic composition to form a solid eutectic composition.

17. The method of claim 15 , further comprising forming particles from the eutectic composition.

Assignees

• Orbital Atk Inc

Inventors

• Velarde Stephen P
• Johnston Harold E

Classifications

• C06B25/00

  Compositions containing a nitrated organic compound · CPC title

• C06B25/34 Primary

  the compound being a nitrated acyclic, alicyclic or heterocyclic amine · CPC title

• C06B21/00

  Apparatus or methods for working-up explosives, e.g. forming, cutting, drying · CPC title

• C06B21/005

  By a process involving melting at least part of the ingredients · CPC title