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US 2014/0235853 A1Published application
Method of Preparation of epsilon-2,4,6,8,10,12-Hexanitro-2,4,6,8,10,12-Hexaazaisowurtzitane with Reduced Impact Sensitivity
AssigneeUniversity of Pardubice
InventorsAhmed Ikhlas Mohamed Elbeih, Adela Husarova, Svatopluk Zeman
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Abstract
The present invention relates to a method of preparation of ε-2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane with reduced impact sensitivity by precipitation of a solution of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane in a solvent by an antisolvent, wherein phosphorus(V) oxide is added as a recrystallization promoter to the solution of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane in the solvent, the obtained mixture is stirred and filtered, and the filtrate is subsequently precipitated by the addition of the antisolvent.
Claims10
1:
- A method of preparation of ε-2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane with reduced impact sensitivity by precipitation of a solution of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane in a solvent by an antisolvent, characterized in that phosphorus(V) oxide is added as a recrystallization promoter to the solution of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane in the solvent, the obtained mixture is stirred and filtered, and the filtrate is subsequently precipitated by the addition of the antisolvent.
2:
- The method according to claim 1, wherein water is removed from the solution before or after the addition of phosphorus(V) oxide.
3:
- The method according to claim 1, wherein the solvent for the starting 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane solution is ethyl acetate.
4:
- The method according to claim 1, wherein the recrystallization promoter phosphorus(V) oxide is added in the amount of 1 to 15% w/w, relative to the weight of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane.
5:
- The method according to claim 1, wherein phosphorus(V) oxide is used together with another promoter, preferably with glycerol.
6:
- The method according to claim 1, wherein the mixture of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane solution with the recrystallization promoter is stirred for a time period within the range of 15 to 60 min.
7:
- The method according to claim 1, wherein the mixture of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane solution with the recrystallization promoter is stirred at a temperature within the range of 10 to 40° C.
8:
- The method according to claim 1, wherein the antisolvent is preferably selected from the group comprising paraffinic hydrocarbons, polychlorinated aliphatic hydrocarbons and aromatic hydrocarbons and their derivatives.
9:
- The method according to claim 1, wherein ultrasound is applied during the precipitation step and/or the mixture is stirred.
10:
- The method according to claim 1, wherein water is removed from 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane solution in ethyl acetate by means of vacuum azeotropic distillation, subsequently 3.57% w/w, relative to the weight of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane, of the recrystallization promoter phosphorus(V) oxide is added to the dehydrated solution, this mixture is stirred for 15 min at the temperature of 20° C., the resulting mixture is filtered and the final product is precipitated by means of addition of n-heptane or xylene as the antisolvent.