离子液体存在下重结晶制备降感HMX

摘要

为建立安全、高效、绿色钝感奥克托今(HMX)制备方法,分别以甲基咪唑硝酸盐([mimH] NO3)、丁磺酸甲基咪唑硝酸盐([mimBSO3H]NO3)、三乙胺硝酸盐([Et3NH]NO3)、丁磺酸三乙胺硝酸盐([Et3NBSO3H]NO3)为晶型助剂,丙酮、环己酮为溶剂,采用溶剂-非溶剂法重结晶制备降感HMX.结果表明,在离子液体[mimBSO3H]NO3(质量为HMX的1.5％)存在的条件下,以环己酮为溶剂,在60℃,搅拌速度750 r·min-1条件下对HMX重结晶可使HMX晶体趋于球形化.所得HMX晶体表面光滑,边缘整齐,热分解峰温提高到288℃,撞击感度4％.%In order to establish a safe,effective and green method,the reduced-sensitivity HMX was prepared by recrystallization from ionic liquid-solvent system with solvent-nonsolvent technique, using a series of ionic liquids [ mimH ] NO3, [mimBSO3H] NO3, [Et3NH]NO3 and [Et3NBSO3H] NO3 as crystal assistants, acetone and cyclohexanone as solvent. Results show that the reduced-sensitivity HMX with spherical crystal can be recrystallized at 60 ℃ at the stirring rate of 750 r·min-1 in the presence of ionic liquid [mimBSO3H]NO3(1.5% weight of HMX) using cyclohexanone as solvent. The obtained HMX is smooth surface and neat edge with thermal decomposition peak temperature of 288 t,and impact sensitivity of 4%.