4,6-二硝基苯并氧化呋咱的制备、晶体结构及热分解机理

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

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P2 1 ,a =0 740 8( 2 )nm ,b =0 6185 ( 1)nm ,c =0 9796( 2 )nm ,β =10 7 99( 2 )° ,V =0 42 69( 16)nm3 ,Z =2 ,Dc=1 75 9g·cm-3 ,F( 0 0 0 ) =2 2 8,μ(MoKα) =0 161mm-1 ,R1 =0 0 483 ,wR2 =0 12 40 ,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 5K·min-1 的升温条件下 ,其熔点为 173℃ ,在 2 0 6～ 2 46℃之间发生剧烈分解反应 ,至 42

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 single crystal diffraction, elemental analysis and IR measurement. The crystal is monoclinic, space group P 2 1 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) nm 3, Z =2, D c=1 759 g·cm -3 , F (000)=22...