Partial Photoelectrocatalytic Oxidation of 3‐Methylpiridine in Green Conditions by Nanotube/Nanowire Ti/TiO2 Plates Prepared in Aqueous, Glycerol, or Ethylene Glycol Medium

Abstract Nanotube/nanowire structured TiO 2 samples on Ti plates were prepared by anodic oxidation in aqueous, glycerol or ethylene glycol medium under different experimental conditions and characterized by XRD, SEM‐EDX, electrochemical methods (photocurrent profiles and electrochemical impedance spectroscopy). The nanostructured TiO 2 was built on relatively large Ti plates, and consequently, in some preparation conditions, different morphologic properties were observed in the underside and upside zones of the electrodes, especially in ethylene glycol medium. The electrodes were tested for selective photoelectrocatalytic oxidation of 3‐methylpyridine to 3‐pyridinemethanol, 3‐pyridinemethanal and vitamin B 3 in water under UVA irradiation. The best performance was found with the electrode prepared in ethylene glycol/water/NH 4 F (98/2/0.3 w/w) medium at 36 V potential for 3 h, while the worst was that prepared in aqueous medium which showed the shortest nanostructure length. Unlike photoelectrocatalysis and photocatalysis, no aromatic alcohol/carbonyl products were obtained in electrocatalytic and photolytic experiments. The selectivity values of the products were similar for the various electrodes, while the morphology of the nanotubes/nanowires and their quantity which affects the total active surface area were essential for the substrate conversion. The results also show that the photocurrent intensity, XRD peak intensity, and electrical conductivity are correlated with photoelectrocatalytic activity of the Ti/TiO 2 electrodes.