摘要本课题首先以水合肼、硝酸胍、乙酰丙酮为起始原料,分别经过胺化反应、成环反应和氧化脱氢反应合成重要前体3,6-双(3,5-二甲基吡唑)-s-四嗪(BT),并对其合成工艺条件进行了优化,得到了较佳的反应条件。其次以3,6-双(3,5-二甲基吡唑)-s-四嗪为前体合成最终产物3,6-二肼基-s-四嗪(BHT),并对其合成工艺条件进行了优化,得到了较佳的反应条件。最后,利用DSC对其热稳定性进行研究。64149
以BHT为前体进行重氮化反应合成叠氮杂环化合物3,6-二(叠氮基)-1,2,4,5 –四嗪(DiAT)。并通过13C核磁共振验证其叠氮-四唑的互变异构和四唑转型的特性。
毕业论文关键词 高氮含能化合物 3, 6-二肼基-1, 2, 4, 5-四嗪 DSC 热稳定性
毕业设计说明书(论文)外文摘要
Title Studies on the Synthesis and Stability of BHT
Abstract In this paper, 3, 6-bis(3,5-dimethylpyrazol-1-yl)-s-tetrazine(BT) which is an important precursor of s-tetrazine type high-nitrogen compounds was synthesized with guanidine nitrate, hydrazine hydrate and acetylacetone as the raw materials. The
synthesis process was optimized and the optimum conditions were obtained. 3,6-di(hydrazino)-1,2,4,5-tetrazine(BHT) was then synthesized from hydrazine hydrate and 3,6-bis(3,5-dimethylpyrazol-1-yl)-s-tetrazine(BT) . The synthesis process was optimized and the optimum conditions were obtained. Finally, DSC was used to study the thermal stability of BHT.
3,6-diazido-1,2,4,5-tetrazine(DiAT) was synthesized from BHT by diazotization.The azido-tetrazolo tautomerization and tetrazolo transformation of 3,6-diazido -1,2, 4, 5 - tetrazine (DiAT) were investigated by the 13CNMR study.
Keywords high-nitrogen compounds 3,6-di(hydrazino)-1,2,4,5-tetrazine differential scanning calorimetry thermal stability
1 绪论 1
1.1 HiNC研究背景 1
1.2 四嗪类HiNC研究进展 2
1.3 研究内容 5
2 实验部分 7
2.1 实验条件 7
2.1.1 实验药品与试剂 7
2.1.2 实验仪器 7
2.1.3 仪器分析 8
2.2 三胺基硝酸胍(TAGN)的合成 11
2.2.1 合成路线 11
2.2.2 反应历程 11
2.2.3 合成步骤 11
2.2.4 工艺优化 12
2.2.5 小结 13
2.3 3,6-双(3,5-二甲基吡唑)-1,2-二氢-s-四嗪(BDT)的合成 13
2.3.1 合成路线 13
2.3.2 反应历程 14
2.3.3 合成步骤 14
2.3.4 工艺优化 14
2.3.4 小结 16
2.3.5 表征 16
2.4 3,6-双(3,5-二甲基吡唑)-s-四嗪(BT)的合成 16
2.4.1 合成路线 BHT的合成及热稳定性研究:http://www.youerw.com/huaxue/lunwen_71114.html