GB797982A - Improvements relating to the preparation of cyclonite - Google Patents

Abstract

Cyclotrimethylenetrinitramine (cyclonite) is prepared by the nitrolysis of hexamethylenetetramine which comprises reacting 98-100 per cent by weight concentrated nitric acid with hexamethylenetetramine in ratios between 8 : 1 and 15 : 1 by weight while agitating the mixture and maintaining the temperature between -42 DEG C. and -10 DEG C., adding an excess of cold water to the reaction mixture and separating the cyclonite which precipitates from the mixture. The yield of cyclonite can be increased by heating the reaction mixture immediately after nitrolysis to a temperature between 0 DEG C. and 20 DEG C. and maintaining it at that temperature for 20 to 40 minutes, or by rapidly heating the mixture to between 80 DEG and 90 DEG C. and immediately quenching with an excess of cold water. It is possible to combine both of these operations by warming the reaction mixture to between 0 DEG and 20 DEG C. for 20 to 40 minutes and then rapidly heating the mixture to between 80 DEG and 90 DEG prior to adding an excess of cold water. The reaction mixture must be heated as rapidly as possible as by passing a thin layer of the mixture over a series of heated baffles. The preferred conditions for the nitrolysis comprise reacting about 11 parts of 98-100 per cent by weight concentrated nitric acid with 1 part of hexamethylenetetramine while agitating the mixture at approximately -30 DEG C., adding an excess of cold water and separating the cyclonite which precipitates. Detailed examples are given.