CHINESE JOURNAL OF ENERGETIC MATERIALS
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2-甲基-4,5-二硝基三唑-1-氧化物的合成与表征
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(西安近代化学研究, 陕西 西安 710065)

作者简介:

杨威(1983-),男,硕士,工程师,主要从事含能材料及功能材料合成研究。e-mail: ywei-2002@163.com

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总装备部预先研究项目(513051202)


Synthesis and Characterization of 2-Methyl-4,5-dinitro-1,2,3-triazole-1-oxide
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(Xi′an Modern Chemistry Research Institute, Xi′an 710065, China)

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    摘要:

    以乙二醛、甲基肼和盐酸羟胺为起始原料, 经缩合、肟化, 生成的中间体不经分离直接加入硫酸铜-吡啶-水体系, 缩合环化得到2-甲基三唑-1-氧化物(MTO)。并用硝硫混酸硝化合成出2-甲基-4, 5-二硝基三唑-1-氧化物(DNMTO), 由文献报道的4步反应缩减为2步, 总收率16%, 纯度99%。对采用红外光谱、核磁、质谱以及元素分析等对MTO和DNMTO进行了结构表征。确定了缩合环化反应与硝化反应最佳反应条件为100 ℃, 反应0.5 h。在B3LYP/aug-cc-pVDZ基组水平上对DNMTO的结构进行了优化, 获得稳定的几何构型、键级, 并得出温度对热力学性能影响的关系式。结果表明:热能、热容、熵均随温度的升高而增大。

    Abstract:

    With glyoxal, methylhydrazine and hydroxylamine hydrochloride as starting materials, 2-methyl-4, 5-dinitro-1, 2, 3-triazole-1-oxide(DNMTO) was synthesized by the process of condensation, oxime, cyclization and nitration with yield of 16% and purity of 99%, and title compound and its intermediate were characterized by IR, 1H NMR and elemental analysis. Compared with the four-step reaction in the literature, this approach was reduced to two steps. The optimum conditions for the cyclization and nitration reaction were as follows: reaction temperature was 100 ℃ and reaction time was 0.5 h. The structure of DNMTO was also estimated by a B3LYP method based on aug-cc-pVDZ basis set and the stable geometric configuration and bond order were obtained. The relationships between temperature and thermodynamics properties were confirmed. The results show that all thermal energy, thermal capacity and entropy increase with the increase of temperature.

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引用本文

杨威,尉涛,王晓峰,等.2-甲基-4,5-二硝基三唑-1-氧化物的合成与表征[J].含能材料, 2014, 22(1):12-16. DOI:10.3969/j. issn.1006-9941.2014.01.003.
YANG Wei, YU TAO, WANG Xiao-feng, et al. Synthesis and Characterization of 2-Methyl-4,5-dinitro-1,2,3-triazole-1-oxide[J]. Chinese Journal of Energetic Materials, 2014, 22(1):12-16. DOI:10.3969/j. issn.1006-9941.2014.01.003.

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历史
  • 收稿日期: 2012-10-09
  • 最后修改日期: 2013-04-16
  • 录用日期: 2013-05-02
  • 在线发布日期: 2014-01-23
  • 出版日期: 2014-02-25