火工品
火工品
화공품
INITIATORS & PYROTECHNICS
2014年
4期
43-46
,共4页
MTII%微波合成%含能材料
MTII%微波閤成%含能材料
MTII%미파합성%함능재료
MTII%Microwave synthesis%Energetic materials
在微波加热条件下,以N-甲基咪唑为原料,用I2/HIO3的酸性溶液碘化合成1-甲基-2,4,5-三碘基咪唑(MTII)。采用红外光谱、元素分析和高效液相色谱等方法对合成产物MTII进行了结构表征和纯度分析,讨论了反应温度、反应时间、碘、碘酸用量对碘代反应的影响。结果表明,碘代反应的最佳反应条件为:反应温度80℃,反应时间60min,n (I2):n (HIO3)∶n (C4H6N2)=2∶3∶1,高效液相色谱分析表明MTII纯度大于98%。
在微波加熱條件下,以N-甲基咪唑為原料,用I2/HIO3的痠性溶液碘化閤成1-甲基-2,4,5-三碘基咪唑(MTII)。採用紅外光譜、元素分析和高效液相色譜等方法對閤成產物MTII進行瞭結構錶徵和純度分析,討論瞭反應溫度、反應時間、碘、碘痠用量對碘代反應的影響。結果錶明,碘代反應的最佳反應條件為:反應溫度80℃,反應時間60min,n (I2):n (HIO3)∶n (C4H6N2)=2∶3∶1,高效液相色譜分析錶明MTII純度大于98%。
재미파가열조건하,이N-갑기미서위원료,용I2/HIO3적산성용액전화합성1-갑기-2,4,5-삼전기미서(MTII)。채용홍외광보、원소분석화고효액상색보등방법대합성산물MTII진행료결구표정화순도분석,토론료반응온도、반응시간、전、전산용량대전대반응적영향。결과표명,전대반응적최가반응조건위:반응온도80℃,반응시간60min,n (I2):n (HIO3)∶n (C4H6N2)=2∶3∶1,고효액상색보분석표명MTII순도대우98%。
2,4,5-triiodo-1-methylimidazole was synthesized using N-methylimidazole as starting material via iodination of I 2/HIO 3 acidic solution under microwave irradiation. The infrared spectra analysis, elemental analysis and high performance liquid chromatography(HPLC) were adopted for product characterization and purity determination. The effects of reaction time, reaction temperature, the quality of iodine and iodic acid on the iodo-reaction results were studied. The results showed that the optimum parameters of iodination process are reaction time of 60min,reaction temperature of 80℃,n(iodine):n(iodic acid):n(N-methylimidazole)=2:3:1. HPLC analysis showed the purity of MTII was over 98%.