小尺寸LLM-105的重结晶控制方法研究

采用溶剂-非溶剂重结晶法研究了影响LLM-105晶体形貌和粒度大小的因素及影响觃律,选取浓硫酸为溶剂、水为反溶剂,采用反加法研究了溶剂反溶剂体积比、结晶温度、搅拌速度等主要因素对结晶形貌和粒度的影响。结果表明,在搅拌速度500r·min-1、溶剂非溶剂体积比2:15、结晶温度65℃的条件下,重结晶得到的LLM-105晶体形貌觃则,棱角圆滑,长径比在1~1.5之间,粒度均匀,粒度分布在1~10μm之间,平均粒径D50为4.48μm;放热峰温352.9℃,较原料提高了7.2℃,热安定性更好;机械感度降低,撞击感度和摩擦感度分别下降了80%和59%。

Research on Control Method of Recrystallization of Small-sized LLM-105

The solvent-non-solvent recrystallization method was used to study the factors affecting the crystal morphology and particle size of LLM-105 and the influencing laws. By adopting concentrated sulfuric acid as the solvent and water as the anti-solvent, the effects of volume ratio of solvent to nonsolvent, temperature, stirring speed and other major influencing factors on the morphology and particle size of the crystals were studied. The results show that under the conditions of stirring speed of 500 r · min-1, solvent-to-nonsolvent volume ratio of 2∶15, and crystallization temperature of 65℃, LLM-105 has a regular morphology, with a square shape, smooth edges and corners, uniform particle size, meanwhile, the particle size distribution is between 1 ~ 10μm, and an average particle size D50 is 4.48μm. The exothermic peak temperature is 352.9℃, which is 7.2℃ higher than the raw material. The stability of recrystallized LLM-105 is better, and the impact sensitivity and friction sensitivity are reduced by 80% and 59%, respectively.