The invention relates to a preparation method of a Ti/FeMoO4 electrode. The preparation method comprises the following steps: S1, preprocessing a porous titanium substrate; S2, preparing Ti/Fe(OH)F: dissolving a ferrous salt, a soluble fluoride, a micromolecular template and hydrazine in water according to a molar ratio of 1:(2.0-3.5):(4-8):(5-10), performing uniform stirring, transferring the obtained mixed solution into a reaction kettle, adding the pretreated porous titanium obtained in step S1, performing stirring for 20 min by using a mechanical stirrer, transferring the obtained mixtureinto an oven having a certain temperature of T1, performing a reaction for 3-7 h, taking out the obtained titanium sheet after cooling, washing the titanium sheet with water, and carrying out vacuum drying for 2 h; and S3, preparing Ti/FeMoO4: weighing a certain amount of Na2MoO4.2H2O, dissolving the Na2MoO4.2H2O in water, transferring the Ti/Fe (OH) F prepared in step S2 and the obtained Na2MoO4solution into the reaction kettle, performing stirring for 10 min by using the mechanical stirrer, sealing the reaction kettle, placing the reaction kettle in a drying box, performing a reaction at acertain temperature of T2 for a certain time, cooling the obtained reaction product to room temperature, taking out the obtained porous titanium, and carrying out vacuum drying for 2 h to obtain the Ti/FeMoO4 electrode. The electrode prepared in the invention has a multistage structure, the preparation method is green and simple, and the electrode has a good decontamination effect when used as a cathode for treating organic wastewater.