Preparation, Crystal Structure, and Thermal Analysis of Carbohydrazide Trinitrophloroglucinolate  

作　　者：LIU Zhen-hua ZHANG Tong-lai HU Xiao-chun ZHANG Jian-guo YANG Li QIAO Xiao-jing 

机构地区：[1]State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, P. R. China [2]Department 3rd, Institute of Chemical Defense, Beijing 102205, P. R. China

出　　处：《Chemical Research in Chinese Universities》2008年第6期683-687,共5页高等学校化学研究（英文版）

基　　金：Supported by the National Natural Science Foundation of China(No.10776002); China Academy of Engineering Physics

摘　　要：A new compound （CHZ）（HTNPG）·0.5H2O was synthesized by mixing carbohydrazide（CHZ） and trinitrophloroglucinol（TNPG） and characterized by elemental analysis and Fourier transform infrared （FTIR） spectrum. Its crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to triclinic system, P1 space group, with a=0.45578（9） nm, b=1.0142（2） nm, c=1.3041（3） nm, α=86.53（3）°, β=99.56（3）°, γ=81.94（3）°, V= 0.5958（2） nm^3, Z=2, Dc=2.008 g/cm^3, R1=0.0476, and wR2=0.1139. The compound is a di-substituted salt of TNPG, which consists of a cation （CHZ）^2＋ and an anion （HTNPG）^2-. The thermal analysis of the compound was studied by means of differential scanning calorimetry（DSC） and thermogravimetry-derivative thermogravimetry（TG-DTG）. Under nitrogen atmosphere at a heating rate of 10 ℃/min, the thermal decomposition of the compound contained one endothermic process of dehydrating stage and two intense exothermic decomposition processes in a temperature range of 140--232 ℃ on the DSC trace. The decomposition products of the title compound are nearly gaseous products. The existing complicated hydrogen bond networks and electrostatic attraction between （CHZ）^2＋ and （HTNPG）^2- enhance the thermal stability of the title compound.A new compound （CHZ）（HTNPG）·0.5H2O was synthesized by mixing carbohydrazide（CHZ） and trinitrophloroglucinol（TNPG） and characterized by elemental analysis and Fourier transform infrared （FTIR） spectrum. Its crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to triclinic system, P1 space group, with a=0.45578（9） nm, b=1.0142（2） nm, c=1.3041（3） nm, α=86.53（3）°, β=99.56（3）°, γ=81.94（3）°, V= 0.5958（2） nm^3, Z=2, Dc=2.008 g/cm^3, R1=0.0476, and wR2=0.1139. The compound is a di-substituted salt of TNPG, which consists of a cation （CHZ）^2＋ and an anion （HTNPG）^2-. The thermal analysis of the compound was studied by means of differential scanning calorimetry（DSC） and thermogravimetry-derivative thermogravimetry（TG-DTG）. Under nitrogen atmosphere at a heating rate of 10 ℃/min, the thermal decomposition of the compound contained one endothermic process of dehydrating stage and two intense exothermic decomposition processes in a temperature range of 140--232 ℃ on the DSC trace. The decomposition products of the title compound are nearly gaseous products. The existing complicated hydrogen bond networks and electrostatic attraction between （CHZ）^2＋ and （HTNPG）^2- enhance the thermal stability of the title compound.

关 键 词：Trinitrophloroglucinol CARBOHYDRAZIDE Carbohydrazide trinitrophloroglucinolate 

分 类 号：O7[理学—晶体学]