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CeVO4-V2O3 composites were prepared by simple hydrothermal method, and the effects of ethylene glycol(EG) on the products were studied by XRD, N2 adsorption–desorption, SEM, EDS, XPS, PL and UV-vis spectra. The characterization reveals a slight decrease in surface area and a slight enhancement of visible light absorption in the final sample, while the crystalline phase, morphology and separation efficiency of the collective carriers are severely affected by the EG. At the same time, the photocatalytic effect of CeVO4-V2O3 composites was evaluated by the degradation rate of methylene blue (MB) under simulated visible light. The sample for 10 mL EG obtained the highest efficiency of 96.9%, while the one for 15 mL EG showed the lowest efficiency of 67.5% within 300 min. The trapping experiments and ESR experiment showed that the contribution of active species to the photocatalytic degradation of MB was ∙OH > h+ > ∙O2− in descending order, and a possible degradation mechanism was proposed.