Abstract: Using sucrose and sepiolite as experimental raw materials, a new sucrose carbide/sepiolite composite material was prepared by hydrothermal carbonization method, and the composite material was dried by freeze vacuum drying method. The composite samples were characterized by XRD, IR, SEM and BET, and methylene blue was selected as adsorbate to investigate its adsorption properties. The preparation technical conditions of the composite were optimized by the single factor experiment and the response surface methodology. The results showed that the optimum preparation conditions were as follows. Sucrose carbide could be successfully loaded on the surface of sepiolite to prepare sucrose carbide/sepiolite composite. The optimum adsorption capacity of methylene blue is 42.983 mg/g (composite) with the mass ratio of sucrose to sepiolite of 3.5:1.0, the carbonization time of 8 h, and the carbonization temperature of 220 ℃. The order of the influence of the factors on the adsorption properties of methylene blue was: mass ratio of sucrose to sepiolite > carbonization time > carbonization temperature. It could be found that the adsorption effect of composite materials on methylene blue was superior to the values reported in the existing literature.