三氨基胍三硝基间苯二酚盐的制备、晶体结构及热分解

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

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=1.775g/cm3;Z=2;F(000)=360,μ=0.160mm-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10K/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.

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） nm^3, Dc=1.775 g/cm^3, 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.