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化学学报
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化学学报 ›› 2009, Vol. 67 ›› Issue (8): 729-734. 上一篇    下一篇

研究论文

三氨基胍三硝基间苯二酚盐的制备、晶体结构及热分解

齐书元a 张同来*,a 敖国军b 张建国a 杨 利a

  

  1. (a北京理工大学 爆炸科学与技术国家重点实验室 北京 100081)
    (b华东微电子技术研究所 合肥 230022)

  • 投稿日期:2008-08-11 修回日期:2008-11-03 发布日期:2009-04-28
  • 通讯作者: 张同来

Synthesis, Crystal Structure and Thermal Analysis of (TAGH)(HTNR)

Qi, Shuyuan a Zhang, Tonglai *,a Ao, Guojun b Zhang, Jianguo a Yang, Li a   

  1. (a State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081)
    (b East China Research Institute of Microelectronics, Hefei 230022)
  • Received:2008-08-11 Revised:2008-11-03 Published:2009-04-28

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利用三氨基胍和斯蒂芬酸制备得到了三氨基胍三硝基间苯二酚盐, 培养出了可用于X射线衍射的单晶. 利用元素分析、红外光谱、差示扫描量热法(DSC)、热重-微分热重法(TG-DTG)和X射线单晶衍射等方法对标题化合物的组成和结构进行了表征. 晶体属于三斜晶系, 空间群为P-1, 晶胞参数a＝0.75554(15) nm, b＝0.90816(18) nm, c＝1.0264(2) nm, α＝101.61(3)°, β＝91.96(3)°, γ＝107.74(3)°, V＝0.6536(2) nm3; Dc＝1.775 g/cm3; Z＝2; F(000)＝360, μ＝0.160 mm－1, R1＝0.0479, ωR2＝0.0998. 晶体结构分析结果表明, 该化合物分子式为C7N9O7H11, 是由[C(N2H3)3]＋和(C6N3O8H2)－结合成的离子化合物, 分子中含有大量的氢键, 结构较为稳定. 热分析结果表明, 在10 K/min的升温速率下, 标题化合物的热分解过程由1个吸热峰和3个放热峰组成, 分解产物大部分为气相产物, 剩余残渣量在1%左右.

关键词: 三氨基胍, 三硝基间苯二酚, 晶体结构, 热分析

A new energetic compound (TAGH)(HTNR) (TAG: triaminoguanidine, H2TNR: 2,4,6-trinitroresorcinol) was synthesized by reacting triaminoguanidine with 2,4,6-trinitroresorcinol (Styphnic acid) in aqueous solution under nitrogen atmosphere. Single crystals suitable for X-ray measurement were obtained. The title compound was characterized by elemental analysis, Fourier transform infrared (FTIR) spectra, differential scanning calorimetry (DSC), thermal gravimetry-differential thermal gravimetry (TG-DTG) and single crystal X-ray diffraction analysis. The crystal belongs to a triclinic system with P-1 space group and cell parameters of a＝0.75554(15) nm, b＝0.90816(18) nm, c＝1.0264(2) nm, α＝101.61(3)°, β＝91.96(3)°, γ＝107.74(3)°, V＝0.6536(2) nm3, Dc＝1.775 g/cm3, Z＝2, F(000)＝360, μ＝0.160 mm－1, R1＝0.0479, and ωR2＝0.0998. The results show that the title compound C7N9O7H11 formed by [C(N2H3)3]＋ and (C6N3O8H2)－ belongs to an ionic compound. There are a lot of intramolecular and intermolecular hydrogen bonds existing in the title compound, which make the title compound stable. Under nitrogen atmosphere with a heating rate of 10 K/min, the thermal decomposition of the title compound displayed one endothermic decomposition process and three exothermic processes with released gas as the main products and only 1% leavings.

Key words: triaminoguanidine, 2,4,6-trinitroresorcinol, crystal structure, thermal analysis