Coking coal, the raw material of a coke plant, was applied to the adsorption of coking wastewater. In this study, coking coal was directly treated with sulfuric acid to improve its surface properties and adsorption ability. Acid treatment was carried out at various concentrations, by varying from 0.001 to 1 mol/L. The samples were characterized by ash content analysis, scanning electron microscope (SEM), N2 adsorption-desorption analysis, Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), wettability analysis, and zeta potential analysis. These results demonstrated that H+ could react with inorganic minerals, which resulted in a significant variation of the chemical composition and the structure of coal surface. Furthermore, both the ash content and the surface content of O = C-O, C = O and C-O groups declined gradually as the concentration of sulfuric acid increased, while the surface area and pore volume of micropore, the lipophilic and hydrophobic properties, and zeta potential magnitude increased, resulting in enhanced hydrophobic and Van der Waals' forces between the fine coal and organic pollutants. Characterization modification showed a better performance in adsorption, the removal rate enhanced from 23% to 42% after treated by 1 mol/L sulfuric acid. It was concluded that the acid activation modified the lipophilic and hydrophobic properties, the surface charge properties, surface area and pore volume, the content of oxygen functional groups, all of which could be potentially useful in wastewater adsorption.