The present invention relates to a copper-iron-carbon aerogel electrode preparation method. According to the method, resorcinol, formaldehyde, water, sodium carbonate, iron acetylacetonate and copper acetate monohydrate are uniformly mixed in a reaction container according to a certain ratio, a polymerization reaction is performed for a certain time at a certain temperature to prepare a wet gel, the wet gel is dried, programming heating and cooling is performed to prepare the copper-iron-carbon aerogel electrode, and the prepared copper-iron-carbon aerogel electrode is activated sequentially through CO2 and N2 so as to be used as the cathode in the degradation pool to degrade organic pollutants such as dimethyl phthalate and the like. Compared to the method in the prior art, the method of the present invention has advantages of simple preparation process, high activity, low treatment cost for degradation of organic pollutants such as DMP and the like, simple treatment process, flexible degradation, and the like.