四甲基乙烯合成频哪酮的研究  

The Synthesis of Pinacolone by Tetramethylethylene

作　　者：张正东 焦蒙蒙 Zhang Zhengdong;Jiao Mengmeng(Yancheng PureTech Carbon Co.,Ltd.,Jiaugsu Yancheng 224300;Southeast University,Jiangsu Nanjing 211189)

机构地区：[1]盐城普鲁泰克炭素有限公司,江苏盐城224300 [2]东南大学化学化工学院,江苏南京211189

出　　处：《化工时刊》2019年第6期9-12,共4页Chemical Industry Times

摘　　要：以四甲基乙烯为原料,设计使用环氧化试剂过硫酸氢钾复合盐(Oxone)和一种固体酸催化剂全氟磺酸树脂(Nafion-H)合成频哪酮。通过实验对影响其收率的关键因素进一步优化,实验结果表明:第一步的最佳工艺条件是过硫酸氢钾复合盐与烯烃的物料配比为1.3∶1,反应时间为1h,磁子的转速为1800rpm,溶液的pH为6.7,室温下反应,最佳收率为96.1%;第二步的工艺条件是催化剂与四甲基环氧乙烷的比例是200∶1(mg/g),室温下反应,收率为90.3%,总收率为86.8%。并且通过红外光谱和核磁氢谱对产品结构进行了表征。Pinacolone which was prepared from tetramethylethylene was characterized by FTIR and NMR.The process is divided into two steps, which include the use of epoxidizing agents potassium peroxodisulfate complex salt and solid acid catalyst perfluorosulfonic acid resin. In this paper, the conditions of this technology were optimized,the best process conditions of the first step: the ratio of potassium persulfate compound salt to olefin is 1.3 ∶ 1, The reaction time was 1 h, and the rotational speed of the magnet 1800rpm,and the pH of the solution 6.7 , the experiment is conducted at room temperature, The best yield was 96.1%;The process conditions of second step of the process conditions: the ratio of catalyst to tetramethyloxirane was 20 ∶ 1 (mg/mmol), reaction at 10-15℃, The yield was 90.3%, The overall yield was 86.8%.

关 键 词：频哪酮 新工艺 绿色 环氧化反应 高效液相色谱分析 

分 类 号：TQ224.4[化学工程—有机化工]