The activated coke (ACoke) was used as the adsorbent to remove the complex organic matter from the printing and dyeing wastewater. The change of organic matter species and concentrations before and after absorption was studied. Physicochemical properties of ACoke and its influence on adsorption characteristics were investigated. The results showed that the content of organics (aromatic hydrocarbons and alkane derivatives) decreased from 89.1% to 30.5% after absorption by ACoke. The content of organic matter only decreased from 89.1% to 87.7% after absorption by activated carbon (AC). Types and contents of surface functional groups of ACoke were similar to those of AC, and contributed indistinctively to the adsorption characteristics. The abundant mesoporous structure had a significant influence on the adsorption characteristics of ACoke. The specific surface area of mesoporous structure of ACoke was 114.111 m2/g, which accounted for 28.6% of its total specific surface area and was 2.7 times that of AC.