1-甲基-3,5-二硝基-1,2,4-三唑的合成及表征

摘要

1-Methyl-3,5-dininitro-1 ,2,4-triazole (MDNT) was synthesized from hydrazine dihydrochloride and cyanoguanidine. The total yield is 16.75% .melting point is 95 -96 ℃ ,and purity is more than 99% for the purified MDNT.%以双氰胺、二盐酸肼为起始原料,经缩合环化、重氮化硝化、甲基化等三步反应合成1-甲基-3,5-二硝基-1,2,4-三唑(MDNT),总收率为16.75％.精制后,熔点95 ～96℃,纯度大于99％,用核磁氢谱(1 H NMR)、红外光谱(IR)、元素分析对其结构进行了表征.同时,改善了3,5-二氨基-1,2,4-三唑( DAT)的萃取工艺,改用热的甲醇萃取,DAT收率由89.0％提高到96.5％.用差示扫描量热法(DSC)研究了MDNT的热分解性质.结果表明,MDNT的热分解分为两个阶段,分别为95.7℃和230.2℃,它的熔化热为16.505 kJ·mol-1,分解热为112.582 kJ·mol-1.