CHINESE JOURNAL OF ENERGETIC MATERIALS
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1-氨基-3-甲基-1,2,3-三唑硝酸盐的合成与表征
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作者单位:

南京理工大学,南京理工大学,南京理工大学

作者简介:

李琳(1986-),女,硕士研究生,研究方向为含能离子盐的合成。

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Synthesis and Characterization of 1-Amino-3-methyl-1,2,3-triazolium Nitrate
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Nanjing University of Science and Technology,Nanjing University of Science and Technology,Nanjing University of Science and Technology

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    摘要:

    以乙二醛和水合肼为起始原料,经加成-消除、环化甲基化、置换反应得到1-氨基-3-甲基-1, 2, 3-三唑硝酸盐(1-AMTN),总收率71.8%(以乙二醛计),采用核磁(NMR)、红外(IR)、质谱(MS)和元素分析对产物进行了表征。预测了1-AMTN的性能:密度为1.63 g·cm-3,生成焓84 kJ·mol-1,爆速8115 m·s-1。研究了溶剂、温度、物料比对产物得率的影响,确定了环化甲基化的最佳反应条件:溶剂为乙腈,反应温度20 ℃,乙二腙与碘甲烷的物料比1:5,环化甲基化收率为86.7%。对活性二氧化锰进行了回收利用并对其机理进行了探讨。

    Abstract:

    1-Amino-3-methyl-1, 2, 3-triazolium nitrate(1-AMTN) was synthesized using glyoxal and hydrazine hydrate as starting materials in three steps, i.e. addition-elimination, cyclization, methylation and replacement reaction. The overall yield is 71.8%(based on glyoxal). The structure of products was confirmed by IR, MS, NMR and elemental analysis. The properties of 1-AMTN were estimated: density 1.63 g·cm-3, enthalpy of formation 84 kJ·mol-1 and detonation velocity 8115 m·s-1. The key factors of cyclization and methylation were studied and the optimal reaction conditions were confirmed: medium acetonitrile, 20 ℃, and the ratio of glyoxal bishydrazone and methyl Iodide 1:5. The overall yield of cyclization and methylation is 86.7%. In addition, actived manganese oxide was recycled and its mechanism was also discussed.

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引用本文

李琳,叶志文,吕春绪.1-氨基-3-甲基-1,2,3-三唑硝酸盐的合成与表征[J].含能材料, 2012, 20(1):9-12. DOI:10.3969/j. issn.1006-9941.2012.01.003.
LI Lin, YE Zhi-wen, Lü Chun-xu. Synthesis and Characterization of 1-Amino-3-methyl-1,2,3-triazolium Nitrate[J]. Chinese Journal of Energetic Materials, 2012, 20(1):9-12. DOI:10.3969/j. issn.1006-9941.2012.01.003.

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历史
  • 收稿日期: 2011-03-17
  • 最后修改日期: 2011-05-10
  • 录用日期: 2011-05-19
  • 在线发布日期: 2012-02-23
  • 出版日期: