AbstractActivated carbon was prepared from sugarcane bagasse with phosphoric acid activation by a mechanochemical process. The effects of milling time on adsorption properties and pore structure of activated carbon were evaluated. The results showed that phosphoric acid activation was assisted by the mechanochemical process, which can reduce the processing time and improve the adsorption performance of the prepared activated carbon. The iodine number, the methylene blue adsorption value, and the specific surface area of the prepared activated carbons were improved from 647.94 mg/g, 150 mg/g and 1075.21 m2/g to 889.37 mg/g, 177 mg/g, and 1254.52 m2/g, respectively. Compared with conventional phosphoric acid activation, the activated carbon produced by the mechanochemical process achieved the advantages of shorter processing time, greater adsorption capacity, and higher adsorbed amounts of iodine, methylene blue, and nitrogen.