亚铜盐催化碱性水解法合成氟代苯酚及其工艺优化  

The synthesis and process optimization of fluorinated phenol by cuprous salt catalyzed alkaline hydrolysis

作　　者：窦杰[1] 杨俊伟[1] 李程碑[1] 杭磊[1] 李浩[1] 陈国珍[1] 

机构地区：[1]陕西省石油化工研究设计院,陕西西安710054

出　　处：《应用化工》2017年第2期152-156,共5页Applied Chemical Industry

基　　金：陕西省科技统筹创新工程计划项目(2015KTZDGY07-06);陕西省延长石油(集团)有限责任公司科技示范中试项目(ycsy2014sfzs-A-1)

摘　　要：1-卤代氟苯在亚铜盐催化下发生碱性水解反应,生成氟代苯酚,以单因素结合正交实验,对合成工艺进行优化。结果表明,合成五氟苯酚的最佳工艺条件为:全氟苯93.0 g(0.5 mol),Raney Ni 5.0 g,Cu2O 7.5 g,90%工业KOH 65.0 g,水200 g,环丁砜60.0 g,转速500 r/min,120℃反应8 h,收率达到80.0%。经过非均相反应、脱色、除氟、分子精馏等工艺,五氟苯酚达到质量标准:含量≥99.8%,单杂含量≤0.1%,掉氟物≤0.01%,水分≤100 mg/kg,溶剂残留≤100 mg/kg,符合液晶中间体和医药中间体的质量要求。mFluorinated phenol was synthesized from 1 -halogenated fluorobenzene as raw material by cuprous salt catalyzed alkaline hydrolysis reaction,and technological condition was obtained with single factor experiments and orthogonal design. The result showed that the best process conditions of pentafluoro- phenol for 93.0 g（0 -5 mol） hexafluorobenzene,5.0 g Raney Ni,7.5 g Cu2O ,6 5 .0 g 90% . KOH,200 g H2O,60.0 g sulfolane,stirring rate is 500 r/min and reaction temperature is 120 °C for 8 h,the yield of product reached 80.0%. The researches on production process and inspection methods have found that through heterogeneous reaction, decoloring, defluorinating and molecular distillation agents, the pentafluorophenol achieved to such quality specification; product content ≥99 . 8% , single impurity ≤ 0 . 1% ,defluorinated impurity ≤0. 01% , water content≤100 mg/kg, solvent residual≤100 mg/kg, which is in conformity with the quality specification of liquid crystal intermediates and pharmaceutical intermediates.

关 键 词：氟代苯酚 亚铜盐催化碱性水解 工艺优化 检测方法 质量标准 

分 类 号：TQ564.3[化学工程—炸药化工]