摘要
以甲酰胺与乙二醛为原料,碱性条件下缩合制备了中间体1,4-二甲酰基-2,3,5,6-四羟基哌嗪(DFTHP);在杂多酸/纯硝酸体系中将DFTHP缩合、硝化制备了4,10-二硝基-2,6,8,12-四氧杂-4,10-二氮杂四环十二烷(TEX)。通过红外光谱、核磁共振光谱等对其进行了结构表征,研究了TEX的最佳制备工艺,探讨了反应机理。结果表明,H3[P(W3O10)4]为最佳的杂多酸催化剂,最佳工艺条件为:质量比m(DFTHP)/m(urea)=1∶0.25,H3[P(W3O10)4]用量1 g,控制加料温度为50℃,反应温度65℃,反应时间40 min,TEX的产率为44.7%。
The intermediate 1,4-formaldehyde-2, 3, 5, 6-tetrahydroxy-piperazine （DFTHP） was prepared by the reaction of for- mamide and glyoxal condensed in alkaline condition, then it was condensed and nitrified in the system of heteropolyacid/pure nitric acid to obtain 4, 1 0-dinitro-2,6,8,12-tetraoxa-4,10-diaza-tetracyclo dodecane （ TEX）. TEX was characterized by infrared spectroscopy and nuclear magnetic resonance spectroscopy, and the mechanism of the reaction was also discussed. H3 [ P（W3 O10 ）4 ] was proved to be the favorable heteropolyacid catalyst, the optimum processing conditions were determined as： mass ratio m（DFTHP）/m（urea）=1 ： 0.25, the dosage of H3EP（W3O10）4] 1 g, adding the reactants at 50℃,reaction temperature 65 ℃ and reaction time 40 min. with the yield of TEX 44.7%.
出处
《含能材料》
EI
CAS
CSCD
北大核心
2015年第2期125-129,共5页
Chinese Journal of Energetic Materials
基金
国家自然科学基金资助(51374131)
关键词
杂多酸
1
4-二甲酰基-2
3
5
6-四羟基哌嗪
4
10-二硝基-2
6
8
12-四氧杂-4
10-二氮杂四环十二烷
机理
heteropolyacid, I ,4-formaldehyde-2, 3, 5, 6-tetrahydroxy-piperazine
4,10-dinitro-2,6,8,12-tetraoxa-4,10-diaza-tetracyclo dodecane
mechanism
