Abstract: The magnetic nano-activated carbon was prepared by co-precipitation after refining activated carbon by rolling vibration mill. The research process included characterizing the magnetic nano-activated carbon,studying effects of the adsorption time,initial concentration of adsorbent and pH value on the adsorption of magnetic nano-activated carbon for methylene blue and phenol,fitting adsorption kinetics models and adsorption isotherm models,and researching the regeneration capacity preliminarily. The results were as follows: the adsorption time had a great influence on the adsorption rate of phenol; when the initial concentration of methylene blue was more than 100 mg·L^-1 and phenol was less than 10 mg·L^-1,it had a greater influence on the adsorption rate; the adsorption rate of methylene blue increased with the increase of pH value,and the adsorption rate of phenol had a peak value（ 76. 1%） at pH 6. 0; the adsorption processes of methylene blue and phenol were in accord with the pseudo-second-order kinetics and the Langmuir equation; the adsorption rate of methylene blue on magnetic nano-activated carbon was mainly controlled by the intraparticle diffusion process; the adsorption rate of phenol on magnetic nano-activated carbon was mainly controlled by the surface adsorption and liquid film diffusion; the magnetic properties of magnetic nano-activated carbon were excellent,and magnetic separation method combined with other regeneration methods could be used for regeneration. Magnetic nano-activated carbon is an economical and efficient new activated carbon,which has a great application prospect in wastewater treatment.