Process for obtaining a charge of hexanitrohexaazaisowurtzitane crystals having a rounded morphology; charge and corresponding energetic material

Patent metadata

Field	Value
Publication number	US-9353456-B2
Application number	US-201214110621-A
Country	US
Kind code	B2
Filing date	Apr 5, 2012
Priority date	Apr 8, 2011
Publication date	May 31, 2016
Grant date	May 31, 2016

Abstract

The present invention provides a process for obtaining a charge of hexanitrohexaazaisowurtzitane crystals having rounded morphology. It also provides said charge, the energetic material comprising it, and a process for manufacturing said material. Said process for obtaining said charge comprises:
preparing a saturated solution of any polymorphic form of hexanitrohexaazaisowurtzitane in a mixture comprising both an organic solvent for said hexanitrohexaazaisowurtzitane and an organic nonsolvent for said hexanitrohexaazaisowurtzitane, said solvent being more volatile than said nonsolvent; seeding this saturated solution with a few hexanitrohexaazaisowurtzitane crystals; and then concentrating the seeded, saturated solution by at least partial evaporation of the solvent, said evaporation of the solvent being performed at a temperature of between 35° C. and 15° C. and at a pressure adjusted, to plus or minus 12 mbar, to the boiling pressure of the solvent in said solution, throughout the process of evaporating said solvent from said solution.

First claim

The invention claimed is:

1. A process for obtaining a charge of hexanitrohexaazaisowurtzitane crystals, said process comprising:
preparing a saturated solution of any polymorphic form of hexanitrohexaazaisowurtzitane in a mixture comprising both an organic solvent for said hexanitrohexaazaisowurtzitane and an organic nonsolvent for said hexanitrohexaazaisowurtzitane, said organic solvent being more volatile than said organic nonsolvent;
seeding the saturated solution with a few hexanitrohexaazaisowurtzitane crystals to form a seeded saturated solution; and then
concentrating the seeded saturated solution by at least partial evaporation of the organic solvent, said evaporation of the organic solvent being performed at a temperature of from 35° C. to 15° C. and at a pressure that is in a range from a boiling pressure of the organic solvent in the seeded saturated solution plus 1.2×10 3 Pa (12 mbar) to the boiling pressure of the organic solvent in the seeded saturated solution minus 1.2×10 3 Pa (12 mbar) throughout the process of evaporating said organic solvent from said seeded saturated solution.

2. The process according to claim 1 ,
wherein said organic solvent is selected from the group consisting of esters, nitriles, ethers, ketones, and mixtures thereof; or
said organic nonsolvent is selected from the group consisting of aliphatic hydrocarbons, halogenated aliphatic hydrocarbons, aromatic hydrocarbons, nonflammable hydrofluoroethers, and mixtures thereof.

3. The process according to claim 1 , wherein said evaporation of the organic solvent is performed at the pressure that is in a range from a boiling pressure of the organic solvent in the seeded saturated solution plus 5×10 2 Pa (5 mbar) to the boiling pressure of the organic solvent in the seeded saturated solution minus 5×10 2 Pa (5 mbar) throughout the process of evaporating said organic solvent from said seeded saturated solution.

4. The process according to claim 1 , wherein the pressure on startup of the evaporation is greater than the boiling pressure of the solvent in said solution.

5. The process according to claim 1 , wherein said organic solvent is evaporated to give a suspension of the crystals in a solvent/nonsolvent mixture, said solvent/nonsolvent mixture containing less than 15% by mass of the organic solvent.

6. The process according to claim 5 , which further comprises washing said suspension with the organic nonsolvent.

7. The process according to claim 1 , which further comprises recovering the crystals by filtration.

8. The process according to claim 1 , wherein seeding is carried out with crystals of polymorphic form ε.

9. A charge of crystals which is obtainable by the process according to claim 1 .

10. The charge of crystals according to claim 9 , wherein at least 80% of the crystals in the charge have an elongation ratio of less than or equal to 1.5.

11. The process according to claim 1 , wherein said organic solvent is selected from the group consisting of esters, nitriles, ethers, ketones, and mixtures thereof, and said organic non solvent is selected from the group consisting of aliphatic hydrocarbons, halogenated aliphatic hydrocarbons, aromatic hydrocarbons, nonflammable hydrofluoroethers, and mixtures thereof.

12. The process according to claim 1 , wherein said organic solvent is evaporated to give a suspension of the crystals in a solvent/nonsolvent mixture, said solvent/nonsolvent mixture containing less than 5% by mass of the organic solvent.

13. The process according to claim 12 , wherein it further comprises washing said suspension with the organic nonsolvent.

14. The process according to claim 1 , wherein said seeding is carried out with crystals of polymorphic form ε, the saturated solution containing hexanitrohexaazaisowurtzitane in a polymorphic form other than the ε polymorphic form.

15. The charge of crystals according to claim 9 , wherein at least 80% of the crystals in the charge have an elongation ratio between 1.5 and 1.

Assignees

• Muscatelli Florent
• Lescop Philippe
• Herakles
• Eurenco France

Inventors

• Muscatelli Florent
• Lescop Philippe

Classifications

• C30B29/54

  Organic compounds · CPC title

• C07D487/22

  in which the condensed system contains four or more hetero rings · CPC title

• C06B25/34 Primary

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

• C30B7/06 Primary

  using non-aqueous solvents · CPC title