3,6-二肼基-1,2,4,5-四嗪的合成与表征

摘要以水合肼、硝酸铵和硝酸胍为基本原料，经四步反应生成最终产物DHT。其中，第一步以水合肼和硝酸胍为原料经过胺化反应制得了三氨基硝酸胍(TAGN)；第二步以TAGN和乙酰丙酮为原料经过成环反应制得了3,6-对(3,5-二甲基吡唑)-1,2-二氢-1,2,4,5-四嗪(BDT)并进行了核磁与红外表征；第三步反应以BDT、亚硝酸钠和冰乙酸为原料经过氧化过程制得了3,6-对(3,5-二甲基吡唑)- 1,2,4,5-四嗪(BT)并对其进行了核磁与红外表征。最终BT和水合肼在乙腈介质中反应得到目标产物DHT并进行了核磁与红外表征。30060
为了探究DHT的最佳合成条件，本论文对每步反应的投料比例、反应时间、反应温度、催化剂的用量等实验条件进行了系统的探讨，经过大量的实验，对实验条件进行了优化，最终得到最优实验条件。
关键词：3,6-对(3,5-二甲基吡唑)-1,2,4,5-四嗪(BT) 3,6-二肼基-1,2,4,5-四嗪含能材料
毕业论文设计说明书外文摘要
Title
Synthesis and Characterization of 3,6-Dihydrazino -1,2,4,5 -tetrazine
Abstract
3,6-Dihydrazino-1,2,4,5-tetrazine is synthesized by Hydrazine hydrate, Ammonium nitrate and Guanidine nitrate by a four-step reaction. The main product of the first step is Triaminoguanidine nitrate(TAGN)，which is synthesized by hydrazine hydrate and guanidine nitrate through amination reaction. The second product is 3,6-bis(3，5-dimethyl pyrazole)-1,2-Dihydrogen-1，2，4，5-tetrazine(BDT), which is synthesized by TAGN and acetyl acetone through cyclization reaction and characterized the product through IR and 1HNMR. The main product of the third step is 3,6-bis(3，5-dimethyl pyrazole)-1，2，4，5-tetrazine(BT),which is synthesized by BDT sodium nitrite and glacial acetic acid through oxidation Reaction and characterized the product through IR and 1HNMR. Finally, the final product 3,6-Dihydrazino-1,2,4,5-tetrazine is synthesized by BT and Hydrazine hydrate and characterized it through IR and 1HNMR.
On the other hand, in order to find out the best Synthesis Conditions of DHT. The article discussed the experiment conditions such as molar ratio of reactants, reaction time, temperature and the amount of catalyst. By Systematic experiment, the best condition of each step was found.
Keywords 3,6-bis(3,5-dimethylpyrazole)-1,2,4,5-tetrazine 3,6-Dihydrazino-1,2,4,5-tetrazine Energetic materials
目   次
1 绪论    1
1.1 四嗪类含能材料的研究进展    1
1.2 3,6-二肼基-1,2,4,5-四嗪的性质及合成方法    3
1.2.1 盐酸三氨基胍法    3
1.2.2 三氨基硝酸胍法    4
1.3 本课题的工作计划    5
1.3.1 3,6-二肼基-1,2,4,5-四嗪(DHT)的合成与工艺优化    5
1.3.2 TAGN、BDT、BT、DHT的表征    5
2 三氨基硝酸胍(TAGN)的制备与工艺优化    6
2.1 实验药品及实验仪器    6
2.1.1 实验药品    6
2.1.2 实验仪器    6
2.2 实验步骤:    7
2.3 结果与讨论    7
2.3.1 硝酸胍与水合肼投料比对产率的影响    7
2.3.2 反应时间对三氨基硝酸胍产率的影响    8
2.3.3 催化剂对三氨基硝酸胍产率的影响    9
3 3,6-对(3,5-二甲基吡唑)-1,2-二氢-1,2,4,5-四嗪的制取与工艺条件的优化    10
3.1 实验步骤    10
3.2 结果与讨论    10
3.2.1 三氨基硝酸胍与乙酰丙酮投料比对收率的影响    10
3.2.2 反应时间对BDT产率的影响    11
3.3 BDT的图谱表征    12
4 3,6-对(3,5-二甲基吡唑)- 1,2,4,5-四嗪(BT)的制取与工艺条件的优化    14 3,6-二肼基-1,2,4,5-四嗪的合成与表征:http://www.751com.cn/huaxue/lunwen_25580.html