饱和溶液-冷却结晶法制备棒状α-HMX

Preparation of Virgate α-HMX by Saturation-Cooling Crystallization

采用饱和溶液-冷却结晶法,研究了将β-HMX转化为α-HMX,通过设计正交试验,研究了β-HMX的质量浓度、混合液体中醋酸和水的体积比、冷却温度和冷却时间等4个因素对该过程转化率的影响;获得了β-HMX向α-HMX转化的最佳的工艺参数：β-HMX的质量为0.4g,冷却时间为3h,醋酸与水的体积比为1：1,冷却温度为95℃;在该工艺条件下,β-HMX完全转化为α-HMX。SEM观察结果表明,制备的α-HMX呈细长的棒状,直径在3~8μm。

In this work,β-HMX was switched to α-HMX using the saturation-cooling crystallization meth-od. According to the orthogonal comparisons,the influence of factors such as weight concentration of β-HMX,volume ratio of the acetic acid / water mixture,cooling temperature and cooling time on the conver-sion rate during the process were studied. The optimized conditions for the complete phase conversion of β-HMX to α-HMX were obtained. The result shows that the 100% conversion of industrial-grade β-HMX toα-HMX can be achieved on the conditions of 0. 4 g HMX,and the cooling for 3h,and the volume ratio be-ing 1：1,and initial water temperature being 95℃. The prepared α-HMX is virgate with the diameter in 3-8μm observing by SEM.