N,N-二正丁基间氨基苯酚的合成工艺优化  

Optimization of synthesis process of N,N-dibutyl-m-aminophenol

作　　者：袁晋亭 蔺黎明 高令峰 张书廷[1] Yuan Jinting;Lin Liming;Gao Lingfeng;Zhang Shuting(School of Environmental Science and Engineering,Tianjin University,Tianjin 300072,China;Shandong Ruikang Fine Chemical Co.,Ltd.,Weifang 262700,Shandong,China)

机构地区：[1]天津大学环境科学与工程学院,天津300072 [2]山东瑞康精化有限公司,山东潍坊262700

出　　处：《精细化工》2020年第2期397-402,共6页Fine Chemicals

摘　　要：以间氨基苯酚和氯代正丁烷为原料,水为溶剂,设计了制备N,N-二正丁基间氨基苯酚的工艺路线。优化后得到的反应条件为:n(间氨基苯酚)∶n(氯代正丁烷)∶n(碘化亚铜)=1∶2∶0.06,反应温度为105~110℃,反应压力为0.2~0.5 MPa,pH为6.5~6.8,反应时间为6.0~6.5 h,N,N-二正丁基间氨基苯酚收率达到96.7%,产品液相色谱纯度≥99%。该工艺通过缓冲溶液反应体系设计,并结合反应压力控制,实现蒸馏后N,N-二正丁基间氨基苯酚的选择性达98.5%,有效抑制了氮单烷基化和酚羟基烷基化两种副产物的生成。The preparation of N,N-dibutyl-m-aminophenol from m-aminophenol and n-chlorobutane using water as solvent was optimized.The results showed that the optimized conditions for the synthesis of N,N-dibutyl-m-aminophenol were the following:n(m-aminophenol)∶n(n-chlorobutane)∶n(CuI)=1∶2∶0.06,reaction time of 6.0~6.5 h,reaction temperature of 105~110℃and reaction pressure of 0.2~0.5 MPa.Under these conditions,the yield of the N,N-dibutyl-m-aminophenol was up to 96.7%and the purity that was determined by liquid chromatography was above 99%.By the fine control of the reaction pressure and the pH of reaction solution,the selectivity of 98.5%was achieved.In this work,the formation of the two side-products including 3-(butylamino)phenol and 3-butoxy-N,N-dibutylaniline was effectively inhibited via the control of the reaction pressure and the p H value of reaction solution.This optimized synthesis process provides a new idea for the fabrication of N,N-di-n-butyl m-aminophenol.

关 键 词：N N-二正丁基间氨基苯酚 热敏染料 控压 控pH 特种染料与颜料 

分 类 号：TQ610.42[化学工程—精细化工]