Abstract: MoO3 was recovered from waste MoSi2 after oxidation reaction by thermal evaporation method, and Fe2(MoO4)3 material was prepared from recovered MoO3 and Fe2O3 by reaction sintering method. The time and temperature of complete oxidation of MoSi2 and the microstructure, linear shrinkage, volume density, spectral properties of prepared Fe2(MoO4)3 material were studied. The results show that, waste MoSi2 powder can be oxidized completely after calcination at 500 ℃ for more than 150 minutes. In the reaction sintering of MoO3 and Fe2O3, with increasing temperature, the reaction sintering is more complete, Fe2(MoO4)3 material has more voids, the linear shrinkage increases and the volume density decreases. Fluorescence spectrum analysis shows that, the photogenerated electron-hole pairs of Fe2(MoO4)3 and MoO3 composite material is more difficult to be recombined than pure Fe2(MoO4)3 which means composite material has higher photocatalytic activity. Using methylene blue as dye, pure Fe2(MoO4)3 has good adsorption performance, while Fe2(MoO4)3 and MoO3 composite show excellent photocatalytic performance, and the mixture of Fe2(MoO4)3 and MoO3 composite has best photocatalytic degradation cycle stability.