ZnMoO4 powder was synthesized by coprecipitation method using Zn(NO3)2·6H2O and (NH4)6Mo7O24·4H2O as main materials. Phase composition, microstructure of the synthesized samples were characterized by XRD, SEM, and so on. Antibacterial performance of the synthesized samples with different treatment temperatures were studied through Escherichia coli as the killing object. The results show that precursor mainly consists of non-crystalline with a small amount of ZnMoO4, Zn2Mo3O8, Zn(OH)2 and MoO3; the precursor is transferred into ZnMoO4 when heat treated at 400 ℃ to 600 ℃ for 30 min. With the increase of heat treatment temperature, the crystal structure of ZnMoO4 is gradually improved, so antibacterial performance of ZnMoO4 is increased. When the heat treatment temperature is 600 ℃, ZnMoO4 with good crystallization can be obtained, and particle size of ZnMoO4 is granular and flake-like with average size of 1.5 μm. The as-synthesized ZnMoO4 owns better antibacterial performance. Among them, antibacterial performance of ZnMoO4 synthesized by heat treatment of 600 ℃ is the best, and its antibacterial rate arrives at 99.2% after 24 h antibacterial test. When 5% ZnMoO4 powder is added into commercial coating slurry, antibacterial rate of the coating reaches 95.7%, which has good application prospects.