芴液相催化氧化制取9-芴酮

Catalysts for Liquid-Oxidation of Fluorene to 9- Fluorenone

9-芴酮是重要的精细化工中间体,具有非常高的经济价值,主要由芴催化氧化制得。建立了芴液相氧化反应产物的气相色谱分析方法,解决了反应产物主要组分的定性和定量分析问题。以固体碱为催化剂,考察了催化剂种类、催化剂用量、溶剂种类、氧气流量、温度、反应时间和搅拌速率等因素对反应的影响,并进行了催化剂回收再利用实验。实验结果表明:NaOH是一种高性能、非均相催化剂,在适宜的条件下(催化剂与芴质量比为0.06∶1、溶剂用量为30mL、氧气流量为12mL/min、反应温度为40℃、反应时间为4h、搅拌速率为300r/min),芴的转化率在99%以上,9-芴酮收率在95%以上。

9-Fluorenone,as an important fine chemical intermediate of very high economical value,is mainly prepared by catalytic oxidation of fluorene. The gas chromatography analysis method for reaction products was established,and the main components in the reaction products were analyzed qualitatively and quantitatively. With solid base as catalyst,type of catalysts,amount of catalyst,type of solvents,oxygen flow rate,temperature,reaction time and stirring speed which had effects on the reaction were experimentally determined. At the same time,the experiments on recycling and reusing catalyst were carried out. The results show catalyst of Na OH is a type of high-powered heterogeneous catalyst. Under optimal experimental conditions: m( catalyst) ∶ m( fluorene) = 0. 06∶ 1,solvent of 30 m L,oxygen flow rate of12 m L / min,reaction temperature of 40 ℃,reaction time of 4 h,stirring speed of 300 r / min,the conversion of fluorene and yield of 9-fluorenone can reach above 99% and 95%,respectively.