含能材料2017，Vol.25Issue(10)：843-847,5.DOI:10.11943/j.issn.1006-9941.2017.10.009
3,3′-二(偕二硝基甲基)-4,4′-偶氮呋咱的合成与热性能
Synthesis and Thermal Properties of 4,4′-Bis(dinitromethyl)-3,3′-azofurazan
黄晓川 1王子俊 1秦明娜 1郭涛 1刘敏 1邱少君1
作者信息
- 1. 西安近代化学研究所,陕西 西安710065
- 折叠
摘要
Abstract
4,4′-Bis(dinitromethyl)-3,3′-azofurazan (4) and potassium 4,4′-bis(dinitromethyl)-3,3′-azofurazanate (3) were syn-thesized from 4,4′-dicyano-3,3′-azofurazan through addition, diazotization and nitration with yield for each step reaction of 93. 3%, 91. 2%, 24. 5% and 63. 1%,respectively. In addition, a new furazan, 4,4′-aminoxim-3,3′-hydrazinefurazan (1), was obtained in the synthesis process of 4 . This synthesis of 1 may proceed first with hydroxylamine addition of 4 ,4′-dicyano-3 ,3′-azo-furazan followed by reduction of excessive hydroxylamine. The intermediates and product were analyzed by1 H NMR,13 C NMR,IR and mass spectrum. The thermal behavior of 1, 3 and 4 were studied by DSC-TG method. The thermal behavior of 1 includes one dehydration endothermal stage and two obvious decomposition stages with mass loss of 5. 1%, 53. 5% and 36. 3%,respectively. The peak temperature of each stage is 83 . 7℃, 241 . 1℃ and 336 . 2℃. The thermal behavior of 3 and 4 include only one obvious decomposition stage. The mass loss and the peak temperature are 86. 6% and 258. 1 ℃, 71. 8%156. 0 ℃, respectively.关键词
偶氮呋咱/二硝基甲基/有机合成/热性能/含能材料Key words
azofurazan/dinitromethy/organic synthesis/thermal behavior/energetic material分类
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黄晓川,王子俊,秦明娜,郭涛,刘敏,邱少君..3,3′-二(偕二硝基甲基)-4,4′-偶氮呋咱的合成与热性能[J].含能材料,2017,25(10):843-847,5.
