摘要
以甲醇钠和混二硝基苯为原料研究了甲氧基化反应,将其中的邻、对二硝基苯转化为对应的硝基苯醚,从而得到高纯度间二硝基苯。并讨论了甲醇、甲醇钠加入量对粗间二硝基苯进行醚化反应收率的影响,确定了最优的工艺条件。实验结果表明:粗间二硝基苯和甲醇质量比为1∶0.3,邻、对二硝基苯与甲醇钠的物质的量的比为1∶1.05,反应时间50 min,反应温度76℃时,邻、对二硝基苯的转化率高达99.8%,间二硝基苯的纯度在99.8%以上。
In this paper,the methoxidation reaction was studied using sodium methanol and mixed dinitrobenzene as raw materials to convert the o-,p-dinitrobenzene into the corresponding nitro phenyl ether,thereby obtaining high purity m-dinitrobenzene.The effect of the amount of methanol and sodium methoxide on the yield of etherification reaction of crude dinitrobenzene was discussed.Thus,the optimum process conditions were determined.The experimental results show that when the mass ratio of crude dinitrobenzene to methanol is 1∶0.3,the molar ratio of o-,p-dinitrobenzene and sodium methoxide is 1∶1.05,the reaction time is 50 min,and the reaction temperature is 76℃,the conversion rate of dinitrobenzene is as high as 99.8%,and the purity of m-dinitrobenzene is above 99.8%.
作者
丁军委
刘孟潇
李鑫
赵文婷
李晓珂
DING Junwei;LIU Mengxiao;LI Xin;ZHAO Wenting;LI Xiaoke(College of Chemical Engineering,Qingdao University of Science and Technology,Qingdao 266042,China)
出处
《青岛科技大学学报（自然科学版）》
CAS
2021年第3期13-16,21,共5页
Journal of Qingdao University of Science and Technology:Natural Science Edition
基金
山东省重点研发计划项目(2019GSF109055)。
关键词
二硝基苯
甲醇钠
硝基苯甲醚
甲氧基化
dinitrobenzene
sodium methoxide
nitroanisole
methoxylation
