CHINESE JOURNAL OF ENERGETIC MATERIALS
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二硝基脲含能离子盐的合成及表征
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李亚妮(1982-),女,助理工程师,主要从事催化合成研究。e-mail: nizi0217@163.com

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国防973项目资助(613740202)


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

    Abstract:

    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 diacidic 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.

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李亚妮,杨建明,余秦伟,等.二硝基脲含能离子盐的合成及表征[J].含能材料, 2011, 19(3):247-251. DOI:10.3969/j. issn.1006-9941.2011.03.002.
LI Ya-ni, YANG Jian-ming, YU Qin-wei, et al. Preparation and Characterization of Energetic Ionic Salts of N, N-Dinitrourea[J]. Chinese Journal of Energetic Materials, 2011, 19(3):247-251. DOI:10.3969/j. issn.1006-9941.2011.03.002.

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历史
  • 收稿日期: 2010-03-22
  • 最后修改日期: 2010-08-08
  • 录用日期: 2010-06-13
  • 在线发布日期: 2012-02-22
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