Abstract: The highly active Ti/nano-TiO₂-Pt modified electrode was prepared by using the method of electrochemistry synthesis and electro-deposition. The cyclic voltammetry was adopted to study and compare the electrochemical properties of the TiO₂/nano membrane electrode, single Pt electrode, Ti/nano-TiO₂-Pt modified electrode in H₂SO₄ solution.The electro-catalysis properties of Ti/nano-TiO₂-Pt modified was also studied in the process of Mn²⁺ oxidized to Mn³⁺. Results showed that Ti/nano-Pt modified electrode had high catalystic activity to Mn²⁺ and oxidation beak potential of Mn²⁺ was 1.28 V(vs. SCE), which is 0.12 V of negative-transfering as compared with that of single Pt electrode.The oxygen-releasing potential was 1.4 V,about 0.08 V higher than that of single Pt electrode. The electro-catalysis properties of Ti/nano-TiO₂-Pt modified electrode were better than those of single Pt electrode and Ti/nano electrode, while the efficiency of non-homogenous electrolysis oxidation was over 90%. The Mn³⁺ propared by electrolysis could oxidize glycerol to glyceraldehyde,and the yield was 96%.