N_2O_5/发烟硫酸体系一步法合成1-甲基-3,4,5-三硝基吡唑  

One Step Synthesis of MTNP with N_2O_5/Oleum System

作　　者：吴霏[1] 李永祥[1] 郝彩丽[1] 薛梅[1] 王建龙[1] 曹端林[1] 

机构地区：[1]中北大学化工与环境学院,山西太原030051

出　　处：《含能材料》2016年第6期618-620,共3页Chinese Journal of Energetic Materials

摘　　要：以1-甲基吡唑(1-MP)为原料,N_2O_5-发烟硫酸体系作为硝化剂,一步法硝化合成1-甲基-3,4,5-三硝基吡唑(MTNP),并采用红外光谱、核磁共振、元素分析和质谱表征了其结构。研究了N_2O_5质量分数、1-MP与N_2O_5摩尔比、反应温度和时间对MTNP产率的影响,并确定了最佳反应条件为:N_2O_5质量分数20%,n(1-MP)∶n(N_2O_5)=1∶5,温度为165℃,反应时间1.5 h,该条件下MTNP收率达60.32%。1 -Methyl-3,4,5-trinitropyrazole （MTNP） was synthesized by one-step method using 1 -methylprazole（1 -MP） as raw materials and N2O5-oleum（20% ） as nitrating agent. Its structure was characterized by IR, NMR, elemental analysis and MS. In addition, the influences of the mass fraction of N2O5, molar ratio of 1-MP and N2O5, reaction temperature and time on MTNP yield were studied. The optimum reaction conditions were obtained as. mass fraction of N2O5 20%, n（1-MP） ： n（N2O5）= 1 ： 5, reaction temperature 165 ℃ and reaction time 1.5 h, respectively. Under such conditions, the yield of MTNP can reach up to 60.32%.

关 键 词：1-甲基-3  4 5-三硝基吡唑(MTNP) N2O5 硝化 20%发烟硫酸 

分 类 号：O626[理学—有机化学] TQ560.1[理学—化学]