固体酸H_2SO_4-SiO_2催化制备9,9-双(4-羟苯基)芴的应用研究

A Solid Acid H_2SO_4-SiO_2 Technology of Catalytic Preparation of 9,9-Bis(4-hydroxyphenyl) fluorine

以9-芴酮和苯酚为原料,首次采用固体酸H_2SO_4-SiO_2(简称:固体酸)为催化剂合成9,9-双(4-羟苯基)芴(简称:双酚芴).用熔点、IR和1H-NMR对双酚芴的结构进行了表征.对反应温度、原料摩尔比、催化剂用量进行了优化.结果显示当温度45℃,反应时间3.5 h,原料摩尔比n(9-芴酮)∶n(苯酚)=1∶6,固体酸催化剂的量占原料总质量8%,助催化剂β-巯基丙酸的量占原料总质量0.5%时,双酚芴的产率为96.05%,纯度为99.7%,苯酚的回收率为90%.

Starting materials with fluorenone and phenol, for the first time using a solid acid catalyst H2SO4-SiO2 （ abbreviation： solid acid ） synthesizes 9, 9-bis （ 4-hydroxyphenyl ） fluorene （abbreviations： bisphenolfluorene）. The structure of bisphenolfluorene has been verified by melting pointIR and 1H-NMR. The reaction temperature,mole ratio and the amount of catalyst are optimized. The result indicates that when the temperature is 45 ℃ ,reaction time is 3.5 hours,the mole ratio of 9- fluorenone/phenol is 1 to 6, the quality of the solid acid catalyst accounting for the total material is 8% ,the quality of co-catalyst β-mercaptop-ropionic acidcatalyst accounting for the total material is 0. 5% ,and the bisphenolfluorene is 96. 05% yield and 99. 7% purity ,recovery of phenol is 90%.