氧气液相催化氧化孔雀绿隐色体的环境友好工艺研究

Study of Environmentally-friendly Technology of Catalytic Oxidation of Peacock Green Leuco with Oxygen in Liquid Phase

研究了催化剂种类及用量、循环氧化剂四氯苯醌的用量、溶剂、底物初始浓度、醋酸用量、反应温度和反应时间对氧气液相氧化孔雀绿隐色体的影响。发现在乙醇介质中以金属络合物为催化剂、氧气为氧化剂、催化剂用量为底物质量的 3 %、四氯苯醌用量为底物质量的 0 91%、隐色体初始浓度为 3 3mol/L、醋酸用量与溶剂总量的体积比为 1∶6、于 5 0℃下反应 10h ,可以获得76 72 %的产品收率。工艺过程由于使用了价廉易得、无污染的氧气为氧化剂 ,因而对环境友好。氧化产物的结构经过核磁共振谱得以确认。

The effects of catalyst, chloronil which was used as circulating oxidizing agent, solvent, initial concentration of the substrate, acetic acid, reaction temperature and reaction time on the oxidation of Peacock Green leuco with oxygen in liquid phase were studied. It was found that 76.72% yield could be obtained with metal complex as catalyst in alcohol medium under following conditions. The amount of catalyst was 3 percent of the substrate (W/W), the amount of chlononil was 0.91 percent of the substrate (W/W), the initial concentration of leuco was 3.3 mol/L, the ratio of acetic acid to the total amount of solvent was 1:6(V/V), the reaction time was 10 h and the reaction temperature was 50°C. The structure of oxidized product was confirmed by 1HNMR.