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作 者:刘亚静[1] 莫洪昌[1] 丁峰[1] 张丽洁[1] 高福磊[1] 姬月萍[1]
出 处:《含能材料》2014年第6期732-735,共4页Chinese Journal of Energetic Materials
基 金:总装预研项目资助(51328050505)
摘 要:以丙三醇为原料,经酯化、叠氮化两步反应,合成了三叠氮三乙酸甘油酯( TAA)。总收率为84.1%。用红外光谱、核磁共振、元素分析表征了中间体和目标化合物的结构。探讨了酯化反应和叠氮化反应的影响因素。结果表明,叠氮化反应的最佳条件为:NaN3摩尔加入量为理论值的1.10倍,混合溶剂中水占总体积的5%~25%,反应时间为10 h。TAA的收率为95.0%,纯度不小于96.8%。Triazidotriacetin( TAA)was synthesized via esterification and azidonation using propanetriol as raw material. The over-all yield was 84. 1%. The structures of intermediates and target compound were characterized by IR,NMR and elemental analysis. The factors affecting esterification and azidonation reactions were discussed. Results show that the optimum conditions of azidona-tion reaction are determined as:the dosage of NaN3 is 1.10 times of theoretical value,i. e. nexp ∶ ntheo=1.10(molar ratio),the dosage of water is 5% ~25% of the total volume of acetone-water mixed solvent,and the reaction time is 10 h. The yield of TAA is 95. 0% and its purity more than 96. 8%.
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