聚能富氮化合物5,5-联四唑-1,1-二氧化物二羟铵合成工艺研究

摘要

Dihydroxylammonium 5,5-bistetrazole-1,1-diolate(TKX-50)was synthesized using solution glyoxal (40%w/w in H2O) and hydroxylammonium as starting materials, by five steps, i.e. substitution, chloration, nitrine reaction, ring formation reaction and salt formation reaction.The over yield is 19%.The structure of the product was characterized by IR, elemental analysis and NMR. Meanwhile, the properties of TKX-50 were tested, it showed that the impact sensitivity H 50 is 41cm, and the friction sensitivity is72%. The key factors of reaction temperature, reaction time and holding temperature for yield of BTO were studied, the optimal reaction condition were reaction temperature 0~5℃, reaction time 12h, holding temperature 20~25℃.%以40%乙二醛水溶液和盐酸羟胺为原料，通过取代、氯化、叠氮化、成环、成盐反应制备了5,5-联四唑-1,1-二氧化物二羟铵（TKX-50），总得率为19%。通过元素分析、红外光谱、核磁对其结构进行表征，测定了TKX-50的撞击感度H50为41cm，摩擦感度爆炸百分数为72%。研究了反应温度、反应时间、保温温度对5,5-联四唑-1,1-二氧化物二水合物（BTO）得率的影响，确定了成环的较佳反应条件为：反应温度0~5℃，反应时间12h，保温温度20~25℃。