Abstract: A kind of carbonaceous nanometer pore adsorbent was produced from petroleum coke by a composite activation process. The pore width of the adsorbent among 1 nm～2 nm is over 90%. Under the condition of 25 ℃，3.5 MPa，the volume and mass adsorption of methane on the adsorbent are over 120 V/V and 14.0% respectively. Adsorption isotherm shows that the adsorption type belongs to theⅠadsorption, and in according with micropore filling theory; Adsorption isobar shows that low temperature favors the adsorption; the water contained in the adsorbents is harmful to the increase of the adsorption capacity.