四相相转移催化氧化芴制备芴酮  

Preparation of Fluorenone by Four-Phase Phase Transfer Catalytic Oxidation of Fluorene

作　　者：闫俊[1] 于丽梅[1] 张文珠[1] 高占先[1] 

机构地区：[1]大连理工大学化学学院,辽宁大连116024

出　　处：《精细化工》2014年第9期1173-1176,共4页Fine Chemicals

摘　　要：该文利用气-质联用仪确证了芴中杂质的结构和含量。反应物和产物的物料衡算揭示:在以二甲苯和水为溶剂,氢氧化钠为催化剂、季铵盐为相转移剂、空气为氧化剂氧化悬浮于二甲苯中的芴制备芴酮的反应中,芴的转化率为100%;芴100%的转化成芴酮和水,无其他副产物;反应前后原料芴中的杂质数目没有变化,每个杂质的物质的量也保持相等。用纯芴在相同的条件进行氧化反应,芴的转化率为100%,得到纯度100%的芴酮,验证了前述结果。从反应液中分离出芴酮后,溶剂、催化剂、相转移剂、水均可循环使用。同时讨论了反应的机理。In this article, GC-MS was used to confirm the structure and content of the impurities in fluorene. The material balance of each component of reactants and products reveals that, in the preparation of fluorenone by the oxidation of solid fluorene reaction with xylene using Na0H as catalyst and quaternary ammonium salt as the phase transfer agent and air as oxidant, the conversion yield of fluorene is 100%, and the product yield of fluorenone and water is 100% with no other by-products. Meanwhile, there was no change in the number of the impurities in fluorene during the reaction, and the moles of each component also remained the same. The results were verified by the oxidation reaction of pure fluorene under the same conditions. After fluorenone was isolated from the reaction, the solvents, catalysts, and phase transfer reagent can be recycled. Meanwhile, the reaction mechanism was also discussed.

关 键 词：芴 悬浮溶液 氧化反应 芴酮 相转移催化反应 绿色化学 精细化工中间体 

分 类 号：TQ426.94[化学工程]