溶剂/非溶剂法制备球形硝基胍

Preparation of Spherical Nitroguanidine by Solvent/non-solvent Method

以N-甲基吡咯烷酮为溶剂,丙酮为非溶剂,硝酸镍为添加剂,采用溶剂/非溶剂法将堆积密度较低的针状硝基胍重结晶制备成堆积密度较高的球形硝基胍。采用扫描电镜(SEM)和差示扫描量热法(DSC)分析了球形硝基胍的晶体形貌和热性能。讨论了影响硝基胍堆积密度的主要因素,确定了制备较高堆积密度的球形硝基胍的工艺条件。结果表明,在温度为80℃,溶剂与非溶剂体积比为1∶3,添加剂质量分数为0.005%,搅拌速率为400r/min的条件下,制备的球形硝基胍堆积密度最大,为1.08g/cm3,球形硝基胍的热分解温度较文献值略有提高。

Spherical nitroguanidine（NQ）with higher bulk density was prepared from needle shaped NQ with lower bulk density by a solvent/non-solvent method using N-methyl pyrrolidone as solvent,acetone as non-solvent and nickel nitrate as additive.The crystal morphology and thermal properties of spherical NQ were analyzed by scanning electron microscope（SEM）and differential scanning calorimetry（DSC）.The principal factors affecting the bulk density of NQ were studied.The technical conditions of preparing spherical NQ with higher bulk density were determined.The results show that under the conditions of temperature 80℃,volume ratio of solvent and non-solvent as1∶3,mass fraction of additive as 0.005% and stirring rate as 400r/min,the bulk density of the spherical NQ prepared is the biggest with the value of 1.08g/cm^3.The thermal decomposition temperature of spherical NQ has slight increase than that of reference value.