常压催化加氢合成3-氟-4-氨基苯酚新技术

Preparation of 3-Fluoro-4-aminophenol by Catalytic Hydrogenation at Atmospheric Pressure

用浸渍法制得0.2%铁元素改性的Ti O2为载体的负载5%Pd催化剂,用于3-氟-4-硝基苯酚常压催化加氢合成3-氟-4-氨基苯酚,用熔点、元素分析、IR和1H NMR对它的结构表征为目标产物;确定优化工艺条件为:0.1mol硝基物,0.26g催化剂,60mL无水乙醇作溶剂,反应温度为40°C,0.1MPa下加氢反应3h,产率为98.6%,产物的纯度达99.2%。

The catalyst of 5% palladium supported on TiO2 modified by 2% Fe was prepared by impregnation method for synthesizing 3-fluoro-4-aminophenol from 3-fluoro-4-nitrophenol by catalytic hydrogenation at ambient pressure. The product was idenlified by IR and ^1H NMR, melting point test, and elemental analysis. The optimum reaction conditions were as follows. 0.1 mol 3-fluoro-4-nitrophenol, 0.26 g catalyst, 60 mL anhydrous alcohol as solvent, reaction temperature of 40 ℃ and reaction pressure of 0.1 MPa and reaction time of 3 h. The yield was 98.6%, and the purity of the product reached 99.2%.