The （SCZ）（TNPG）.2H2O prepared by mixing semicarbazide （SCZ） and trinitrophloroglucinol （TNPG） was characterized by elemental analysis and IR measurement, and its crystal structure was determined by X-ray singl...The （SCZ）（TNPG）.2H2O prepared by mixing semicarbazide （SCZ） and trinitrophloroglucinol （TNPG） was characterized by elemental analysis and IR measurement, and its crystal structure was determined by X-ray single-crystal diffraction analysis. The crystal belongs to triclinic,space group P1, （NH2CONHNH3）^＋（C6H2N3O9）^-·2H2O, Mr = 372.23, a = 0.68853（14）, b =0.93966（19）, c = 1.1925（2） nm, α = 67.48（3）, β = 77.56（3）, γ = 78.93（3）°, V = 0.6908（2） nm^3, Z = 2,Dc = 1.789 g/cm^3, Mr = 373.23, F（000） = 384, S = 0.999 and μ（MoKa） = 0.172 mm^-1. The final R and wR are 0.0394 and 0.1057 for 1724 observed reflections with I 〉 2σ（I）. It is concluded that （SCZ）（TNPG） 2H2O is an ionic compound composed of a cation SCZ^＋, an anion TNPG- and two water molecules. The TNPG anion and SCZ^＋ cation are bonded together by electrostatic attraction and hydrogen bonds, and the compound structure is stable. The thermal decomposition of （SCZ）（TNPG） 2H2O was studied by using TG-DTG and DSC techniques with a heating rate of 10 ℃/min, showing the compound contains one endothermic process of dehydrating stage and two intensive exothermic decomposition stages. The enthalpy of exothermic decomposition reaction is 452.31 kJ/mol.展开更多
A novel energetic compound 3-（3,5-dimethylpyrazol-1-yl）-6-semicarbazide-1,2,4,5-tetrazine（DSTZ） was prepared and characterized by elemental analysis and Fourier transform infrared（FTIR） spectroscopy.The crystal ...A novel energetic compound 3-（3,5-dimethylpyrazol-1-yl）-6-semicarbazide-1,2,4,5-tetrazine（DSTZ） was prepared and characterized by elemental analysis and Fourier transform infrared（FTIR） spectroscopy.The crystal structure was determined by X-ray single crystal diffraction technology.The crystal belongs to the monoclinic system with a P2 1 /c space group,a=0.9942（7） nm,b=0.5067（3） nm,c=1.1830（8） nm,β=109.616°,Z=2 and D c =1.475 g/cm 3.With extensive hydrogen bonds,the molecules were linked together to form a three-dimensional herringbone-like pattern.Thermal analysis of the compound was carried out via differential scanning calorimetry（DSC） and thermogravimetric-derivative thermogravimetry（TG-DTG）.Under a nitrogen atmosphere at a heating rate of 10 K/min,DSTZ decomposed directly in a range of 493―513 K.Only one intense exothermic process was observed and the decomposition products were all gaseous products.Conventional sensitivity properties were determined,showing that the title complex was insensitive to friction,impact and flame.展开更多
A new coordination complex [Cu（IMI）4]（PA）2 had been synthesized with imidazole（IMI） as ligands and picrate（PA-） groups as outer anions,and characterized by Fourier transform infrared（FTIR） spectrum and eleme...A new coordination complex [Cu（IMI）4]（PA）2 had been synthesized with imidazole（IMI） as ligands and picrate（PA-） groups as outer anions,and characterized by Fourier transform infrared（FTIR） spectrum and elemental analysis.Its crystal structure was determined by single crystal X-ray diffraction（XRD） analysis.The crystallographic data show that the crystal belongs to monoclinic,C2/c space group,a=2.542（5） nm,b=0.91773（18） nm,c=1.3778（3） nm,β=107.854（3）° and Z=4.Furthermore,the central copper（II） ion is coordinated by four N atoms from four imidazole ligands.All the molecular units are linked into a zigzag pattern along a-axis by the hydrogen bonds,and extended to the distance regularly.Thermal decomposition mechanisms were determined based on differential scanning calorimetry（DSC） and thermogravimetry-differential thermogravimetry（TG-DTG） analysis,and kinetic parameters of the first exothermic process were studied using Kissinger＇s and Ozawa-Doyle＇s method,respectively.Sensitivity tests show that the title complex has low sensitivity to external stimulus,but it has a higher energy of combustion of 14.2 kJ/g due to which it may be used as the additives of energetic materials to improve the explosive performance.展开更多
The title compound （C12H15NO13S, Mr = 413.31） was synthesized by the nitration of napthalene-1,4-dicarboxylate acid in mixed nitric and sulfuric acids. It crystallizes in monoclinic, space group P2 1/c with a = 8.10...The title compound （C12H15NO13S, Mr = 413.31） was synthesized by the nitration of napthalene-1,4-dicarboxylate acid in mixed nitric and sulfuric acids. It crystallizes in monoclinic, space group P2 1/c with a = 8.100（1）, b = 24.369（3）, c = 8.634（1） A, β = 105.380（2）°, V = 1643.1（4） A^3, Z = 4, Dc = 1.671 g/cm^3, F（000） = 856, μ（MoKa） = 0.273 mm^- 1, T = 294（2） K, the final R = 0.0400 and wR = 0.1021 for 2866 observed reflections with I 〉 2σ（I）. In this crystal there exist a number of H-bonds which link the molecules to form a three-dimensional infinite network structure. The thermal decomposition of the title compound was investigated by using TG-DTG and DSC techniques.展开更多
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. ...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.展开更多
基金This work was supported by the National Natural Science Foundation of China (20471008) and the Foundation of BIT-UBF-200302B01
文摘The （SCZ）（TNPG）.2H2O prepared by mixing semicarbazide （SCZ） and trinitrophloroglucinol （TNPG） was characterized by elemental analysis and IR measurement, and its crystal structure was determined by X-ray single-crystal diffraction analysis. The crystal belongs to triclinic,space group P1, （NH2CONHNH3）^＋（C6H2N3O9）^-·2H2O, Mr = 372.23, a = 0.68853（14）, b =0.93966（19）, c = 1.1925（2） nm, α = 67.48（3）, β = 77.56（3）, γ = 78.93（3）°, V = 0.6908（2） nm^3, Z = 2,Dc = 1.789 g/cm^3, Mr = 373.23, F（000） = 384, S = 0.999 and μ（MoKa） = 0.172 mm^-1. The final R and wR are 0.0394 and 0.1057 for 1724 observed reflections with I 〉 2σ（I）. It is concluded that （SCZ）（TNPG） 2H2O is an ionic compound composed of a cation SCZ^＋, an anion TNPG- and two water molecules. The TNPG anion and SCZ^＋ cation are bonded together by electrostatic attraction and hydrogen bonds, and the compound structure is stable. The thermal decomposition of （SCZ）（TNPG） 2H2O was studied by using TG-DTG and DSC techniques with a heating rate of 10 ℃/min, showing the compound contains one endothermic process of dehydrating stage and two intensive exothermic decomposition stages. The enthalpy of exothermic decomposition reaction is 452.31 kJ/mol.
基金Supported by the National Natural Science Foundation of China(No.20471008)the Program of the Ministry of Education of China for New Century Excellent Talents in Universities(No.NCET-09-0051)
文摘A novel energetic compound 3-（3,5-dimethylpyrazol-1-yl）-6-semicarbazide-1,2,4,5-tetrazine（DSTZ） was prepared and characterized by elemental analysis and Fourier transform infrared（FTIR） spectroscopy.The crystal structure was determined by X-ray single crystal diffraction technology.The crystal belongs to the monoclinic system with a P2 1 /c space group,a=0.9942（7） nm,b=0.5067（3） nm,c=1.1830（8） nm,β=109.616°,Z=2 and D c =1.475 g/cm 3.With extensive hydrogen bonds,the molecules were linked together to form a three-dimensional herringbone-like pattern.Thermal analysis of the compound was carried out via differential scanning calorimetry（DSC） and thermogravimetric-derivative thermogravimetry（TG-DTG）.Under a nitrogen atmosphere at a heating rate of 10 K/min,DSTZ decomposed directly in a range of 493―513 K.Only one intense exothermic process was observed and the decomposition products were all gaseous products.Conventional sensitivity properties were determined,showing that the title complex was insensitive to friction,impact and flame.
基金Supported by the Project of Science and Technology of Applied Physical Chemistry Laboratory of China(No.9140C3703051105)the Project of State Key Laboratory of Explosion Science and Technology,China(Nos. QNKT12-02,ZDKT10-01b)
文摘A new coordination complex [Cu（IMI）4]（PA）2 had been synthesized with imidazole（IMI） as ligands and picrate（PA-） groups as outer anions,and characterized by Fourier transform infrared（FTIR） spectrum and elemental analysis.Its crystal structure was determined by single crystal X-ray diffraction（XRD） analysis.The crystallographic data show that the crystal belongs to monoclinic,C2/c space group,a=2.542（5） nm,b=0.91773（18） nm,c=1.3778（3） nm,β=107.854（3）° and Z=4.Furthermore,the central copper（II） ion is coordinated by four N atoms from four imidazole ligands.All the molecular units are linked into a zigzag pattern along a-axis by the hydrogen bonds,and extended to the distance regularly.Thermal decomposition mechanisms were determined based on differential scanning calorimetry（DSC） and thermogravimetry-differential thermogravimetry（TG-DTG） analysis,and kinetic parameters of the first exothermic process were studied using Kissinger＇s and Ozawa-Doyle＇s method,respectively.Sensitivity tests show that the title complex has low sensitivity to external stimulus,but it has a higher energy of combustion of 14.2 kJ/g due to which it may be used as the additives of energetic materials to improve the explosive performance.
基金This work was supported by the NNSFC (No. 20471008)
文摘The title compound （C12H15NO13S, Mr = 413.31） was synthesized by the nitration of napthalene-1,4-dicarboxylate acid in mixed nitric and sulfuric acids. It crystallizes in monoclinic, space group P2 1/c with a = 8.100（1）, b = 24.369（3）, c = 8.634（1） A, β = 105.380（2）°, V = 1643.1（4） A^3, Z = 4, Dc = 1.671 g/cm^3, F（000） = 856, μ（MoKa） = 0.273 mm^- 1, T = 294（2） K, the final R = 0.0400 and wR = 0.1021 for 2866 observed reflections with I 〉 2σ（I）. In this crystal there exist a number of H-bonds which link the molecules to form a three-dimensional infinite network structure. The thermal decomposition of the title compound was investigated by using TG-DTG and DSC techniques.
基金Supported by the National Natural Science Foundation of China(No.10776002) China Academy of Engineering Physics
文摘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.
