Methacrylyloxypropyl modified inorganic/organic hybrid mesoporous materials have been synthesized via an HCl catalyzed sol gel process in the presence of citric acid (CA) as a nonsurfactant template, which involves a combination of 3 (trimethoxysilyl)propyl methacrylate (MSMA) and tetraethoxysilane (TEOS) as precursor species.The CA nonsurfactant is removed by extraction with water, resulting in inorganic/organic hybrid mesoporous materials with high surface area (e.g. 900?m 2·g -1 ) and large pore volume (e.g. 0 55?cm 3·g -1 ).The surface area, pore volume and pore diameter increase slightly with increasing the content of CA.The products were characterized by XRD, N 2 adsorption desorption and FT IR.