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作 者:刘建武[1,2] 严生虎 张跃[2] Liu Jianwu;Yan Shenghu;Zhang Yue(School of Pharmaceutical and Life Sciences, Changzhou University, Changzhou 213164, Jiangsu, China;Continuous Flow Engineering Laboratory of National Petroleum and Chemical Industry, Changzhou 213164, Jiangsu, China)
机构地区:[1]常州大学制药与生命科学学院,江苏常州213164 [2]石油和化工行业连续流技术工程实验室,江苏常州213164
出 处:《精细石油化工》2020年第6期42-47,共6页Speciality Petrochemicals
基 金:江苏省产学研前瞻性联合研究项目(BY2014037-19)。
摘 要:以环己酮为底物,过氧化氢为氧化剂,1,4-二氧六环为溶剂,SO^2-4/Sn-MCM-41为催化剂,经Baeyer-Villiger反应生成ε-己内酯。通过水热合成法和浸渍法制得SO^2-4/Sn-MCM-41分子筛改性催化剂,采用XRD、FT-IR和BET等手段对催化剂结构进行表征。实验考察了反应条件对氧化反应的影响,结果表明:在70%过氧化氢为氧化剂、SO^2-4/Sn-MCM-41(n(Si)/n(Sn)=50)为催化剂、n(催化剂)∶n(环己酮)=0.5∶1、氧酮比2.5∶1、n(溶剂)∶n(环己酮)=8∶1、70℃下反应3 h条件下,环己酮转化率达74.4%,ε-己内酯收率达52.1%。ε-Caprolactone was synthesized by Baeyer-Villiger reaction in a solution consisting of 1,4-dioxane,SO^2-4/Sn-MCM-41 over catalyst,with cyclohexanone as substrate,and hydrogen peroxide as oxidant.SO^2-4/Sn-MCM-41 modified molecular sieve catalyst was prepared by hydrothermal synthesis and impregnation,which was characterized by XRD,FT-IR and BET.The effects of factors on the oxidation were investigated,including catalyst,solvent amount,catalyst amount,ratio of oxygen to ketone,temperature and time.The results showed that under conditions of 70%hydrogen peroxide as oxidant,SO^2-4/Sn-MCM-41(n(Si)/n(Sn)=50)over catalyst,n(catalyst)∶n(cyclohexanone)=0.5∶1,ratio of oxygen to ketone at 2.5,n(solvent)∶n(cyclohexanone)=8∶1,temperature 70℃,and time 3 h,the conversion of cyclohexanone was 74.4%,and the yield ofε-caprolactone reached 52.1%.
关 键 词:环己酮 过氧化氢 Ε-己内酯 Baeyer-Villiger
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