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The graphite/vanadium oxide composites were prepared by a carbothermal reduction method using V2O5 as the raw material and graphite powder as the reducing agent. The Methylene blue was used as a simulated pollutant, the adsorption properties of the prepared samples in different reduction conditions were systematically evaluated, and the samples prepared at the reduction temperature of 650 ℃, reduction time of 60 min and graphite ratio of 18.03% were selected for characterization and as the target adsorbent. The microstructure and surface morphology were characterized by X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, Raman spectroscopy, high-resolution transmission electronic microscope and BET microporous analysis. The characterization results showed that the phase of the samples consisted of graphite, VO2 and a small amount of V6O13, the vanadium oxides were dispersed on the lamellar graphite surface in the form of lumps, strips and radiations, the particle sizes of the samples ranged from a few microns to tens of microns. The BET specific surface area box pore volumes of the graphite/vanadium oxide were 6.84 m2/g and 0.02 cm3/g, respectively, and most of the pore sizes were distributed in the mesoporous and macroporous regions. The adsorption experiments results showed that the graphite/vanadium oxide had good adsorption performance on methylene blue in the pH range of 3-8, and the equilibrium adsorption amounts were above 200 mg ? g-1. The adsorption process was in accordance with the Langmuir isotherm and quasi-secondary kinetic equations.