制备Ti/SnO2+Sb2O4/PbO2电极,电极的组分及其价态由XRD和XPS表征;该电极可将2,2-二羟甲基丙醛直接电合成2,2-二羟甲基丙酸.应用高效液相色谱分析原料和产物,电化学方法研究电合成影响因素,包括:2,2-二羟甲基丙醛浓度、溶液pH值、反应温度和氧化电位等.在优化条件下(pH=1,C醛=0.10 mol.L-1,t=15℃,E=1.8 V)电合成2,2-二羟甲基丙酸的转化率为58%,选择性36%,电流效率28%.本法为该产物的合成提供了一种新的途径.
The Ti/SnO2+Sb2O4/PbO2 electrode was prepared.The structure phase and valent state were characterized by means of XRD and XPS.The 2,2-dimethylolpropionic acid was synthesized on the Ti/SnO2+Sb2O4/PbO2 anode by direct electro-oxidation of 2,2-dimethylolpropionaldehyde.The product and crude material were analyzed by HPLC,the effects of the concentration of 2,2-dimethylolpropionaldehyde,pH,potential and reaction temperature were studied.The results showed that the optimum conditions were anode potential 1.8 V,pH=1,reaction temperature 15℃ and 2,2-dimethylolpropionaldehyde concentration 0.10mol/L.Under the optimum conditions,the selectivity of 36%,the current efficiency of 28% and the conversion of 58% were reached.The reported method provides a new route for the synthesis of 2,2-dimethylol propionic acid.
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