作　　者： ; ; ; ;

机构地区： 南京理工大学化工学院

出　　处： 《含能材料》 2013年第1期7-11,共5页

摘　　要： 以2,4,6-三硝基氯苯为原料,经亲核取代、九水合硝酸铁研磨氧化制得2,2',4,4',6,6'-六硝基偶氮苯(HNAB)。利用MS,IR和1H NMR对中间体和最终产物的结构进行了表征,并对各反应条件进行了优化。亲核取代反应较优工艺为:硫酸肼2.0 g,2,4,6-三硝基氯苯7.6 g,甲醇15 mL,三乙胺6 mL,反应温度45℃,反应时间24 h;氧化反应较优工艺为:1,2-二(2,4,6-三硝基苯基)肼2.0 g,九水合硝酸铁7.1 g,累计研磨8 h,总收率68.5%。利用DSC和TG研究了HNAB的热行为。由Ozawa法计算得热分解机理为n=1的成核和核生长机理,机理函数为f(α)=(1-α),其活化能和指前因子分别为123.48 kJ·mol-1,3.965×1011s-1。 Hexanitroazobenzene（HNAB） was prepared via nucleo chloride as raw materials. The were optimized. The nucleoph ntermediate and final product were lic substitution reaction conditions philic substitution reaction and characterized by MS, IR and ^1 H oxidation reaction using picryl NMR. The reaction conditions are determined as： hydrazine sulfate 2.0 g, 2,4,6-trinitrochlo- robenzene 7.6 g,methyl alcohol 15 mL,triethylamine 6 mL,reaction time 24 h under 45 cc. The oxidation reaction conditions are determined as： 1,2-bis（2,4,6-trinitrophenyl）hydrazine2.0 g,iron（III） nitrate nonahydrate7.1 g, cumulative grinding8 h. The total yield is 68.5%. Thermal behaviors of HNAB were studied by DSCandTG. The thermal decomposition mechanism of HNAB is classified as random nucleation and growth with n = 1. The activation energy,pre-exponential factor and mechanism function of the thermal decomposition process of HNAB obtained by the Ozawa＇s method are 123.48 kJ ·mol^-1,3. 965 × 10^11 s^-1f（α） = （1 -α） ,respectively.

关 键 词： 有机化学 六硝基偶氮苯 九水合硝酸铁 热分解动力学

领　　域： [兵器科学与技术] [理学] [理学]