采用相转移催化法精制粗间二硝基苯

摘要

采用相转移催化法对租间二硝基苯进行醚化处理,将其中的邻、对位异构体转化为对应的硝基苯醚,考察了不同烷氧基化试剂及季铵盐、反应条件、聚乙二醇和季铵盐与聚乙二醇两者复配对间二硝基苯精制反应的影响.结果表明,以甲醇为烷氧基化试剂,四丁基溴化铵为催化剂时,醚化效果较好.在粗间二硝基苯、甲醇、NaOH(质量分数40%)和四丁基溴化铵的质量比为1:0.5:0.09:0.05,反应温度78℃和反应时间为40min的条件下进行粗间二硝基苯精制,最终得到的间二硝基苯纯度可达到99.5%以上.%The crude m-dinitrobenzene was purified by phase transfer catalysis to transfer the P-dinitrobenzene and o-dinitrobenzene into nitrodiphenyl ether. The effects of oxyalkylation reagent, catalyst and reaction conditions on the purification of crude m-dinitrobenzene were investigated. The results showed that tetrabutyl ammonium bromide exhibited better activity with methanol as oxyalkylation reagent. The purity of m-dinitrobenzene reached above 99.5% under the conditions of the mass fraction of crude m-dinitrobenzene, methanol, NaOH and tetrabutyl ammonium bromide 1:0.5:0.09:0.05, reaction temperature 78 ℃ and reaction time 40 min.