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含能材料  2013 

HNAB的制备及其热分解动力学

DOI: 10.3969/j.issn.1006-9941.2013.01.002

Keywords: 有机化学,2,2′,4,4′,6,6′-六硝基偶氮苯(HNAB),九水合硝酸铁,热分解动力学

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Abstract:

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1HNMR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2.0g,2,4,6-三硝基氯苯7.6g,甲醇15mL,三乙胺6mL,反应温度45℃,反应时间24h;氧化反应较优工艺为:1,2-二(2,4,6-三硝基苯基)肼2.0g,九水合硝酸铁7.1g,累计研磨8h,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123.48kJ·mol-1,3.965×1011s-1。

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