耐热炸药PYX制备工艺改进

Improvement on preparation of the heat-resistant explosive PYX

对耐热炸药PYX制备工艺进行了较大改进,以苦基氯和2,6-二氨基吡啶为原料,利用廉价的混合溶剂代替昂贵的DMF,在高效促进剂碱金属酸式碳酸盐NH的作用下进行缩合反应获得2,6-双(苦氨基)吡啶(PAP);简化了硝化工艺,在浓硝酸中直接硝化制备了2,6-双(苦氨基)-3,5-二硝基吡啶(PYX),总收率有大幅度提高,达到89%以上,产品纯度为99.8%,差热分解峰温(DSC)为385.7℃。探讨了促进剂和溶剂对缩合反应的影响,以及硝化反应的影响因素,确定了最佳工艺条件。

The preparation process of heat-resistant explosive PYX was greatly improved and as followed as：taking a cheap mixture solvent instead of the expensive DMF and adding an effective promoter, 2,6- bispicrylamino pyridine（PAP） was synthesized by condensation reaction using picryl chloride and 2,6-diaminopyridine as starting materials. In order to simplify the nitration process of PYX, PYX by direct nitra- tion process in concentrated nitric acid the heat-resistant explosive PYX with a yield above 89% ,purity of 99.8% and thermal decomposition peak temperature（DCS） of 385.7 ℃. The effect of some promoters and solvents on condensation reaction and effect factors of nitration reaction were also discussed, and the optimal reaction conditions were confirmed.