β-cyclodextrin microsphere was prepared,and then was bonded to chitosan.XRD、IR、SEM and surface area determinator were used to characterize the structure and micro-morphology.Raw materials were compared with polymer in adsorbing methyl orange through changing stirring time,temperature,pH value and methyl orange concentration.It was proved that the adsorption of chitosan bonded β-cyclodextrin microsphere was better than that of chitosan and β-cyclodextrin microsphere.In addition,the adsorption of polymer increased with temperature and pH value,the maximum adsorption is 20 mg/g.The process of adsorption fitted Freundlich adsorption model well,moreover,the adsorption was an unspontaneously endothermic process.