The invention discloses a method for utilizing a heterogeneous catalyst to efficiently activate persulfate so as to treat organic wastewater, belonging to the technical field of water pollution control. According to the method, nano Fe0, nano FeOxHy (y=2x-3 or 3y=6x-8) and FeOxHy@Fe0 (FeOxHy@Fe0, y=2x-3 or 3y=6x-8) nano composite materials are used as a heterogeneous catalyst, so that persulfate is activated to produce sulfate free radicals having strong oxidizing property, thereby removing nondegradable organic substances in wastewater. Besides, due to the characteristics of high specific area, high catalytic activity and the like, the solid-phase nano catalyst can efficiently and persistently activate the persulfate to be subjected to heterogeneous activation. The method is applicable to treatment of various organic wastewater, has the advantages of high efficiency, favorable persistence, convenient operation process and environment friendliness, and can efficiently remove toxic and harmful pollutants in the wastewater in a wider pH value range, thus providing broad prospects for treatment of toxic, harmful and nonbiodegradable organic wastewater.