用微反应器连续合成吡啶-N-氧化物工艺

Continuous Synthesis Process of Pyridine-N-oxide in Micro-channel Reactor

以吡啶为原料,在微反应器[1]中,研究连续合成吡啶-N-氧化物工艺.考查了氧化剂浓度、反应温度、反应物料摩尔比、原料进料停留时间对反应的影响,并优化了工艺.结果表明:最佳工艺条件为30%双氧水作氧化剂,吡啶:双氧水:乙酸的摩尔比为1:5:8,反应温度70℃,反应物料停留时间为41s,产物吡啶-N-氧化物粗品收率为96.6%.产物经质谱和^1HNMR表征.

Using pyridine as raw materials to synthesis of pyridine-N-oxide in the micro-reactor for continuous process. Oxidant concentration, reaction temperature, reaction material mole ratio, residence time of raw material in reactor is investigated and optimize the process conditions further. Results show that in the optimum technological conditions of 30% hydrogen peroxide as oxidant, pyridine : hydrogen peroxide : acetic acid =1:5:8, reaction temperature 70℃,raw material feeding residence time of 41 s, the coarse product yield of pyridine-N-oxide is 96.6%. Products is characterized by mass spectrometry and ^1HNMR.