Al-grafted mesoporous silica zeolite materials known as Al-MCM-41 were prepared with supercritical CO2 as the media. The X-ray diffraction（XRD） patterns and N2 adsorption/desorption isotherms indicate that Al-modified MCM-41 materials keep silica MCM-41 pore diameter of about 2.7 nm and the excellent structural ordering very well. The gel permeation chromatography（GPC） and1H NMR show that the polymerization of ε-caprolactone went well with butanol. It was demonstrated that compared with conventional Al-MCM-41 materials, the aluminosilicate mesoporous zeolite prepared with the aid of supercritical CO2 is a novel useful catalyst for the polymerization of ε-caprolactone.
