Titanium oxide coatings(TiO2/Ti) were formed on the titanium surface by micro-arc oxidation(MAO) in Na3PO4 solution.Using the TiO2/Ti as anod electrode, the titanium as counter electrode.Coated activated carbon(TiO2/AC) that prepared by sol-gel dipcoating method ,and activated carbon mixture as particle electrode,combining with the UV lamp and regulated power supply make up the three-dimensional electrode photoelectrocatalysis system. The photoelectrocatalysis system use Na2SO4 aqueous solution as supporting electrolyte.The photoelectrocatalytic ability of titanium oxide coatings were evaluated by photoelectrocatalytic degradation of methylthionine chloride aqueous solution.The experiment demonstrate that there was photoelectrocatalytic degradation of single TiO2/Ti film or only adsorbtion, the photoelectrocatalysis of three-dimensional electrode with particle electrode have the synergistic effect,which can improve the degradation of methylene blue aqueous solution.The influence of some factors was studied,including initial solution,cell voltage, electrolyte concentration and some other factors.When the methylthionine chloride concentration of 5mg/L, cell voltage of 8V, electrolyte concentration of 0.04M. The three-dimensional electrode photoelectrocatalysis degradation of methylene blue compare to traditional two-dimensional plate electrodes which without particle electrode increase 40.36% after 3 hours photoelectrocatalysis.