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作 者:王友兵[1] 王伯周[1] 叶志虎[1] 尚雁[1] 卿辉[1] 李亚南[1]
出 处:《含能材料》2011年第2期142-146,共5页Chinese Journal of Energetic Materials
摘 要:以乙醇为溶剂,苦基氯与氨水反应得到了2,4,6-三硝基苯胺(TNA),再与4-氨基-1,2,4-三氮唑(ATA)经氢的亲核取代(VNS)反应生成了1,3,5-三氨基-2,4,6-三硝基苯(TATB),总收率大于95.7%。采用红外光谱、核磁、质谱以及元素分析等表征了TNA和TATB。研究了甲醇钠、ATA、反应时间对TATB收率的影响,优化了VNS反应条件,其最佳工艺条件为:mTNA mATAmNaOCH3=1614,反应温度70℃,反应时间2h。采用无机酸溶液猝灭反应过程的方法直接合成了超细TATB,平均粒径D50为0.151μm,并对其粒径分布和晶体进行了分析。2,4,6-trinitroaniline(TNA) was synthesized by trinitro-chlorobenzene and aqueous ammonia in alcohol,and then reacted with 4-amino-1,2,4-triazole(ATA) to generate 1,3,5-triamino-2,4,6-trinitrobenzene(TATB) by VNS(Vicarious nucleophilic substitution) reaction with total yield of 95.7%.The structures of TNA and TATB were characterized by FTIR,NMR,MS and elementary analysis.Effects of CH3ONa,ATA and the reaction time were investigated on the overall yield of TATB.The optimized conditions of VNS reaction were: the mass ratio of TNA,ATA and NaOCH3 is 1:6:14,reaction temperature is 70 ℃,and time is 2 hours.The ultra fine TATB with average particle diameter D50 of 0.151 μm was obtained using aqueous mineral acid solutions to quench the reaction.The particle-size and crystal were analyzed.
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