Using straw and urea as raw materials, biochar (BC) and g-C3N4 were prepared by oxygen-free pyrolysis at 300°C and 550°C. BC/g-C3N4 was prepared by loading different amounts of g-C3N4 onto the surface of biochar and characterized by SEM and FT-IR. The adsorption effect on methylene blue (MB) was investigated from the aspects of dosage and pH. The studies of adsorption equilibrium isotherms and the kinetic and the thermodynamic parameters on the BC/g-C3N4 adsorbents are discussed. The results showed that BC/g-C3N4 0.16 g/L with a doping ratio of 1 : 3 was added to the MB solution with an initial concentration of 50 mg/L and pH=11. The adsorption rate and adsorption amount were 96.72% and 302.25 mg/g, respectively. The adsorption process included surface adsorption and intraparticle diffusion, which conformed to the pseudo-second-order kinetic model and Langmuir-Freundlich model. Thermodynamic parameters (ΔG0<0, ΔH0>0, and ΔS0>0) showed that the adsorption reaction is spontaneous, which positively correlated with temperature.