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含能材料  2015 

千克级LLM-105合成和三氟乙酸回收技术

DOI: 10.11943/j.issn.1006-9941.2015.01.006

Keywords: 应用化学 三氟乙酸 回收利用 氧化 LLM-105

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Abstract:

研究了氧化2, 6-二氨基-3, 5-二硝基吡嗪(ANPZ)合成2, 6-二氨基-3, 5-二硝基吡嗪-1-氧化物(LLM-105)的千克级工艺。LLM-105收率为98.3%, 纯度96.4%。降低了三氟乙酸(TFA)用量。采用红外、元素、核磁、质谱表征了LLM-105的结构。采用中和、酸化、蒸馏的方法, 研究了TFA母液回收的千克级工艺, 回收率为85.4%, 纯度99.7%。回收TFA用于ANPZ氧化反应, LLM-105收率为97.8%。探讨了影响氧化反应的因素。最佳工艺参数为: m(ANPZ):V(H2O2)=1:1.8, m(ANPZ):V(TFA) =1:5, 反应温度25~30 ℃, 反应时间14 h; 回收TFA的最佳工艺参数为,质量比m(TFA):V(H2SO4)=1:1.0

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