二硝基脲含能离子盐的合成及表征  

Preparation and Characterization of Energetic Ionic Salts of N,N-Dinitrourea

作　　者：李亚妮[1] 杨建明[1] 余秦伟[1] 薛云娜[1] 吕剑[1] 

机构地区：[1]西安近代化学研究所,陕西西安710065

出　　处：《含能材料》2011年第3期247-251,共5页Chinese Journal of Energetic Materials

基　　金：国防973项目资助(613740202)

摘　　要：利用三唑类、咪唑类化合物以及乙二胺与二硝基脲反应,合成了一系列二硝基脲含能离子盐,采用IR、1H NMR、13C NMR、元素分析等手段对这些盐的结构进行了表征。结果表明,乙二胺与二硝基脲形成二价盐,其它几种化合物形成二硝基脲的一价盐。热分析结果显示,二硝基脲成盐有效提高了其热稳定性,从热重曲线可以看出,乙二胺二硝基脲盐的起始失重温度为125℃(比二硝基脲高55℃),最大失重温度为165℃。探讨了溶剂、温度及反应时间对4-氨基三唑与二硝基脲成盐反应的影响,以乙腈为溶剂,10℃反应2 h,获得85%的收率。Through the reaction of ethylenediamine（EDA） and derivatives of triazole and imidazole with N,N-dinitrourea（DNU）,six energetic ionic salts were prepared.Among them,EDA gave diacid salt,others derivatives gave monoacidic ones.The effects of solvent,reaction temperature and time on yield of salt from 4-aminotriazole and DNU were analyzed.The yield could be up to 85% in acetonitrile and 71% in ethanol at 10 ℃ for 2 h.Generally,polar solvents with high dielectric constant are beneficial to the salt-forming reaction.The structures of all salts prepared were confirmed and discussed by IR,1H NMR,13C NMR and elemental analysis.The thermal stability of most salts surpasses DNU,for instance,EDA-DNU salt started its decomposition at 125 ℃（ca.55 ℃ higher than that of DNU）,exhibited the largest mass loss rate at 165 ℃ in TGA curve.

关 键 词：有机化学 含能离子盐 二硝基脲 三唑 咪唑 乙二胺 

分 类 号：TQ560.1[化学工程—炸药化工]