N~1-(2,2,2-三硝基乙基)-1,5-二氨基四唑的合成工艺改进与热性能

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英文篇名：Synthesis process improvement and thermal properties of N~1-(2,2,2-trinitroethyl)-1,5-diamino-1H-tetrazole 作者：高福磊 ; 汪营磊 ; 赵宝东 ; 陆婷婷 ; 陈斌 ; 刘卫孝 英文作者：GAO Fu-lei;WANG Ying-lei;ZHAO Bao-dong;LU Ting-ting;CHEN Bin;LIU Wei-xiao;Xi'an Modern Chemistry Research Institute; 关键词：四唑 ; 2 ; 2 ; 2-三硝基乙醇 ; 合成 ; 热性能 英文关键词：tetrazole;;trinitroethanol;;synthesis;;thermal property 中文刊名：GXHX 英文刊名：Journal of Chemical Engineering of Chinese Universities 机构：西安近代化学研究所; 出版日期：2019-06-15 出版单位：高校化学工程学报 年：2019 期：v.33 基金：国家自然科学基金(21875185) 语种：中文; 页：GXHX201903019 页数：5 CN：03 ISSN：33-1141/TQ 分类号：154-158

摘要

改进了含能化合物N~1-(2,2,2-三硝基乙基)-1,5-二氨基四唑(TTD)的合成工艺。以二氨基胍盐酸盐为原料,经重氮化反应合成出1,5-二氨基四唑(DAT),然后与2,2,2-三硝基乙醇(TNE)发生曼尼希缩合反应得到TTD,并采用红外光谱、核磁共振、元素分析等鉴定了其结构;优化了缩合反应条件,确定适宜反应条件为:选用物料DAT与TNE的质量比1:2.0,反应介质水/乙醇的质量比1:0.3,温度30℃,时间1 h。利用差示扫描量热法(DSC)、热失重法(TG)对TTD进行了热分解研究,并结合Kissinger法和Ozawa法及相关方程计算了TTD的热动力学参数、热爆炸临界温度,得到TTD的活化能和指前因子分别为:73.65 kJ·mol~(-1),21.15 s~(-1);并计算得到热爆炸临界温度为401.34 K。
        An improved synthetic process was developed for N~1-(2,2,2-trinitroethyl)-1,5-diamino-1 H-tetrazole(TTD). TTD was prepared via diazotization and mannich condensation using diaminoguanidinium and trinitroethanol(TNE) as raw materials, and its structure was identified by IR, ~1HNMR and elemental analysis. The optimized reaction condition of TTD was found as: the mass ratio of TTD to TNE = 1:2.0, the mass ratio of water to ethanol = 1:0.3, reaction temperature = 30 ℃ and reaction time = 1 h. The thermal decomposition properties of TTD were studied by thermogravimetry(TG) and differential scanning calorimetry(DSC). Its thermal decomposition kinetic parameters and thermodynamic parameters were calculated by Kissinger and Ozawa methods. The activation energy of TTD was 73.65 kJ·mol~(-1), the pre-exponential factor was 21.15 s~(-1) and the critical temperatures of thermal explosion(T_p) was 401.34 K.

引文

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