Nano-MoO3 was prepared by ultrasonic method with sodium molybdate as raw material. The nano-MoO3 was studied by infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray powder diffractometer, scanning electron microscope and energy spectrum. The maximum adsorption capacity of nano-MoO3 of methylene blue is 535.78 mg/g, and its adsorption type is chemical adsorption, mainly the complex bond between sulfur in methylene blue and molybdenum. According to the adsorption thermodynamics and thermodynamic study, the adsorption model conforms to the Langmuir isothermal adsorption model and quasi-first-order kinetic model, respectively.