The activator, nanometer titanium dioxide-loaded active carbon was prepared by adsorption-roasting method. A novel electric catalysis system was introduced to treat dyestuff wastewater. The importance of each factor was tested by orthogonal experiment. The experiment results indicated that the electrochemical oxidation process could efficiently remove and degrade organic pollutants. The removal efficiency could be attributed to the oxidation of electrogenerated H₂O₂, hydroxyl radicals generated in electro-fenton process. Furthermore, salicylic acid had been used as a probe to display the generation of the hydroxyl radical.