间二氯苯合成间氯苯甲醚的工艺研究  

Research on synthesis of m-chloroanisole from 1,3- dichlorobenzene

作　　者：曹明珍 徐徐[1,2] 鲍名凯[1] 王石发[1,2] 

机构地区：[1]南京林业大学化学工程学院,江苏南京210037 [2]江苏生物质绿色燃料和化学品重点实验室,江苏南京210037

出　　处：《南京林业大学学报（自然科学版）》2015年第5期150-154,共5页Journal of Nanjing Forestry University：Natural Sciences Edition

基　　金：国家林业公益性行业科研专项项目(201104015);国家自然科学基金项目(31170538)

摘　　要：以间二氯苯和甲醇钠为原料,对间氯苯甲醚合成的新工艺进行了研究;通过单因素实验考察了溶剂种类及用量、间二氯苯与甲醇钠的摩尔比、反应温度、反应时间对间二氯苯转化率和间氯苯甲醚得率的影响,并采用正交实验法对反应条件进行了优化。确定了适宜的合成工艺条件为:以N,N-二甲基甲酰胺(DMF)作溶剂,溶剂用量为75 m L/mol,n(间二氯苯):n(甲醇钠)=1∶1.2,反应温度为120℃,反应时间6 h。在此工艺条件下,间二氯苯的转化率为94.8%,间氯苯甲醚的得率为91.0%。采用FT-IR和GC-MS分析技术对间氯苯甲醚进行了表征。A new preparation process for m-chloroanisole was explored from 1,3-dichlorobenzene and sodium methoxide.The effects of types of solvent and their dosage,mole ratio of 1,3-dichlorobenzene to sodium methoxide,reaction temperature and reaction time on the conversion rate of 1,3-dichlorobenzene and yield of m-chloroanisole was examined. The optimum synthesis conditions were obtained by orthogonal test as follows： N,N-dimethyl-formamide（ DMF） was used as solvent,and solvent dosage was 75 m L / mol; the molar ratio of 1,3-dichlorobenzene to sodium methoxide was 1 ∶ 1. 2;reaction temperature was 120 ℃ and reaction time was 6 h. Under this optimum conditions,the conversion rate of 1,3-dichlorobenzene was 94. 8% and the yield of 1,3-chloroanisole was 91. 0%. The structure of the m-chloroanisole was analyzed by FT-IR and GC-MS.

关 键 词：间二氯苯 甲醇钠 甲氧基化反应 间氯苯甲醚 

分 类 号：TQ612.1[化学工程—精细化工]