The invention discloses a preparation method and application of an iron-copper composite catalyst. The preparation method includes the following steps that 1, ferrous sulfate is dissolved in a mixed solution of ethyl alcohol and deionized water, urea is added, and the mixture is stirred to be dissolved; 2, the material obtained in the step 1 is subjected to magnetic stirring and refluxing in an oil bath, the material is centrifugally washed after being naturally cooled, precipitate is obtained, and the precipitate is dried; 3, the material obtained in the step 2 is calcined, and a first component is obtained after natural cooling is completed; 4, copper nitrate is completely dissolved in a mixed solution of ethyl alcohol and ethylene glycol; 5, the first component is added into the material obtained in the step 4, the first component is completely dispersed through ultrasonic treatment, then the mixture reacts for 3-7 h at the temperature of 115-165 DEG C, the mixture is centrifugally washed after being naturally cooled, and precipitate is obtained; 6, the precipitate obtained in the step 5 is dried under the vacuum condition, and the iron-copper composite catalyst is obtained. The adding amount of the prepared iron-copper composite catalyst and the adding amount of persulfate are both small, therefore, cost is reduced, and the catalyst can be separated and reused after being precipitated.