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为获得2,6–二氨基–3,5–二硝基吡啶(ANPy)的精制方法及工艺,分别以二甲基亚砜(DMSO)、硫酸和硝酸为溶剂,采用溶剂非溶剂法精制ANPy。结果表明,采用DMSO时能获得较好的收率及纯度,并对DMSO、非溶剂水的用量进行了优化,获得了较优ANPy精制工艺,在此条件下ANPy的收率>93%、质量分数>99%。同时用差示扫描量热对ANPy热分解性能进行了研究,结果表明,ANPy先后出现熔化峰(353℃左右)和分解峰(360℃左右),采用Kissinger法计算得到其熔化及分解的动力学常数。
In order to obtain the purification method and technology of 2,6-diamino-3,5-dinitropyridine (ANPy), ANPy was purified by solvent-free method using dimethylsulfoxide (DMSO), sulfuric acid and nitric acid as solvent . The results showed that the best yield and purity were obtained when DMSO was used, and the amount of DMSO and non-solvent water was optimized. The better ANPy purification process was obtained. Under these conditions, the yield of ANPy was> 93%, the mass Score> 99%. At the same time, the thermal decomposition performance of ANPy was studied by differential scanning calorimetry. The results show that ANPy has a melting peak (about 353 ℃) and a decomposition peak (about 360 ℃) successively. The kinetics of melting and decomposition constant.