Abstract: The natural gas adsorbents were prepared with highsulfur petroleum coke as feed, potassium hydroxide as activation agent and sodium dodecylbenzene sulfonate (SDBS) as surfactant. Their pore texture and pore size distribution were measured and the activation mechanism was suggested. The results showed that the surfactant SDBS during preactivation process can enhance the homogeneity of mixed material, which is then evidently favorable for the activation of highsulfur petroleum coke. The micropore volume of the adsorbents GSR3 and GSR4, prepared under the optimal condition, were 1.0985cm3·g－1and 1.3193cm3·g－1, respectively; and the main pore size distribution was between 0.9nm and 1.5nm. Under 25℃ and the CH4 charging/discharging pressure of 3.5MPa and 0.1MPa, the CH4 mass uptake and effective desorption volume of the adsorbents GSR3 and GSR4 can be up to 0.139 and 0.145, and 111, and 115, respectively. Therefore, the highsulfur petroleum coke based adsorbents are much close to lowsulfur petroleum coke based adsorbents in quality.