Chitosan/cellulose acetate multimicrospheres (CCAM) were prepared by the method of W/O/W emulsion with no toxic reagents and had the size interval of 200--280µm. It was investigated as an ideal alternative to enhancement the adsorption of water-soluble dyes from wastewater. The correlation coefficients of adsorption isotherm showed that the Freundlich model was comparable to the Langmuir model. The 1/n was lower than 1.0, indicating that malachite green was favorably adsorbed by CCAM. Furthermore, the amount of malachite green absorbed steeply increased with increasing time and reached plateau values within 2 h and increased with increasing of initial concentration of malachite green from 5 to 25 mg/g.