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有机化学
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有机化学 ›› 2004, Vol. 24 ›› Issue (2): 205-209. 上一篇    下一篇

研究论文

4,6-二硝基苯并氧化呋咱的制备、晶体结构及热分解机理

苗艳玲a, 张同来*,a, 乔小晶a, 张建国a, 郁开北b   

  1. a北京理工大学爆炸灾害预防控制国家重点实验室 北京 100081
    b中国科学院成都有机化学研究所分析测试中心 成都 640041
  • 收稿日期:2003-03-25 修回日期:2003-06-18 接受日期:2003-08-29 发布日期:2022-09-20

Preparation, Crystal Structure and Thermal Decomposition Mechanisms of 4,6-Dinitrobenzofuroxan

MIAO, Yan-Linga, ZHANG, Tong-Lai*,a, QIAO, Xiao-Jinga, ZHANG, Jian-Guoa, YU, Kai-Beib   

  1. aState Key Laboratory of Prevention and Control of Explosion Disasters,Beijing Institute of Technology, Beijing 100081
    bInstrumentation Analysis and Research Center, Chengdu Branch, Chinese Academy of Sciences, Chengdu 640041
  • Received:2003-03-25 Revised:2003-06-18 Accepted:2003-08-29 Published:2022-09-20
  • Contact: * E-mail: ztlbit@public.bta.net.cn

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通过2,4,6-三硝基叠氮苯(TNAB)在冰醋酸中的关环反应,制备了4,6-二硝基苯并氧化呋咱(DNBF)、并培养出了DNBF的单晶.利用X射线单晶衍射、元素分析和红外光谱对其进行了结构表征.测试结果表明:DNBF晶体属单斜晶系,空间群为P21, a=0.7408(2) nm, b=0.6185(1) nm, c=0.9796(2) nm, β=107.99(2)°,V=0.4269(16) nm3, Z=2, Dc=1.759 g·cm-3, F(000)=228, μ(Mo Kα)=0.161 mm-1, R1=0.0483, wR2=0.1240, DNBF分子呈平面构型,其晶体为层状晶体.用TG-DTG和DSC研究了DNBF的热分解过程,在5 K·min-1的升温条件下,其熔点为173 ℃,在206～246 ℃之间发生剧烈分解反应,至429 ℃分解完全.

关键词: 4,6-二硝基苯并氧化呋咱, 制备, 晶体结构, 热分解机理

4,6-Dinitrobenzofuroxan (DNBF) was prepared by heating 1-azido-2,4,6-trinitrobenzene (TNAB) in acetic acid at 100 ℃, and the single crystal of DNBF was cultivated. The crystal was characterized by using X-ray singlecrystal diffraction, elemental analysis and IR measurement. The crystal is monoclinic, space group P21 with crystal parameters as: a=0.7408(2) nm,b=0.6185(1) nm, c=0.9796(2) nm, β=107.99(2)°, V=0.4269(16)nm3, Z=2, Dc=1.759 g·cm-3, F(000)=228, μ(Mo Kα)=0.161 mm-1, R1=0.0483, wR2=0.1240. The obtained results indicate that DNBF is a kind of planar molecules, and its crystal is packed layer bylayer like graphite. The thermal decomposition process of DNBF was studied by using TG-DTG and DSC techniques with a heating rate of 5 K·min-1. The results show that DNBF melts at 173 ℃, produces an intense thermolysis between 206and 246 ℃, and decomposes completely up to 429 ℃.

Key words: 4,6-dinitrobenzofuroxan, preparation, crystal structure, thermal decomposition mechanism