Salting-out process of crystallizing...

Details Salting-out process of crystallizing... Salting-out process of crystallizing...

C - Chemistry, Metallurgy

07

D

C07D 259/00 (2006.01) C07D 487/22 (2006.01)

Patent

CA 2275317

A process of crystallizing CL-20 is disclosed. In the process, a wet CL-20 solvent/CL-20 solution is dried by azeotropic distillation of a CL-20 solvent/water azeotrope. Removal of water from the CL-20 solution permits crystallization of high density CL-20. A low density, CL-20 non-solvent is added to the resulting dry CL-20 solvent/CL-20 solution to cause precipitation of .epsilon.-polymorph CL-20. The CL-20 crystals are separated from the non- solvent and the solvent by adding sufficient water to displace the non-solvent and the solvent from the surface of the CL-20 crystals. In this fashion, the .epsilon.-polymorph CL-20 is made wet for later handling, packaging, and shipping.

Cette invention concerne un procédé de cristallisation de CL-20, lequel procédé consiste à sécher une solution humide solvant de CL-20/CL-20 par distillation azéotropique d'un azéotrope solvant de CL-20/eau. L'élimination de l'eau de la solution à base de CL-20 permet ainsi de cristalliser un CL-20 d'une densité élevée. Un produit de faible densité et ne dissolvant pas le CL-20 est ajouté à la solution sèche solvant de CL-20/CL-20 ainsi obtenue, ceci de manière à entraîner la précipitation d'un CL-20 .epsilon.-polymorphe. Les cristaux de CL-20 sont ensuite séparés du produit non solvant et du solvant en ajoutant une quantité d'eau suffisante pour enlever ces derniers de la surface desdits cristaux de CL-20. Il est ainsi possible d'obtenir un CL-20 .epsilon.-polymorphe humide en vue de sa manutention, de son conditionnement et de son transport dans le futur.

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