Flower-like molybdenum disulfide was synthesized from molybdenum trioxide and sulfur by argon protection solid-state method. The structure and morphology of the products were characterized by XRD, SEM and TEM. The effects of raw material ratio, reaction temperature, reaction time and heating rate on the purity of the product were investigated, and molybdenum disulfide with high purity was prepared. The results show that when the molar ratio of MoO3∶S is 1∶7.5, the reaction temperature is 450 ℃ and the reaction time is 4 h, heating rate is 15 ℃/min, the flower-like molybdenum disulfide with purity of 99.4% can be obtained. The flower-like structure is composed of warped thin plate with thickness of about 10 nm. 0.62 nm monolayer MoS2 is observed by TEM. Flower-like molybdenum disulfide has large specific surface area, which has broad application prospects in the fields of energy storage and catalysis.