The activated carbon prepared from cotton stalk with ZnCl(2) as activation was investigated under microwave radiation. Effects on the yield and adsorption capacities of activated carbon were evaluated then, such as, microwave power, microwave radiation time and the impregnation ratio of ZnCl(2). It indicated that the optimum conditions were as follows: microwave power of 560 W, microwave radiation time of 9 min and the impregnation ratio of ZnCl(2) was 1.6g/g. Iodine number, amount of methylene blue adsorption and the yield of activated carbon prepared under optimum conditions were 972.92 mg/g, 193.50mg/g and 37.92%, respectively. Laboratory prepared activated carbons were characterized by pH(ZPC), SEM, FT-IR, S(BET) and pore structural parameters. Then they were used as adsorbent for the removal of methylene blue from aqueous solutions under varying conditions of initial concentration, carbon dosage and pH. It indicated that Langmuir isotherm was fitter than Freundlich isotherm and Temkin isotherm.