Organically modified metal alkoxides were prepared from reactions between metal alkoicides and 1-benzoylcyclohexanol (BCHOH) and 3-pentenoic acid (PAH) in alcohol at room temperature by sol-gel process. Then poly-GPTS was prepared by polymerization of GPTS with (KOBu)-Bu-t at 50 degrees C. After these stages, new hybrid materials Poly-GPTS/M(CL)(x)(O)/OH (M = Ti, Zr, Al, CL = 1-benzoylcycloheacanolate (BCHO) and 3-pentenoate (PA), GPTS = 3-glycidyloxypropyltrimethoxysilane) were prepared from hydrolysis of mixtures of poly-GPTS and organically modified metal alkoxides in 1:1 mol ratio. The hydrolysis reactions were carried out with 0.1 molar HCl in 50 mL of alcohol. The characterizations of the hybrid materials were performed by a combination of elemental analysis, thermogravimetric measurements, and spectroscopic methods. After hydrolysis, it was seen that some of the BCHO ligands were removed from the hybrid materials under the studied conditions. To see the activity of hybrid materials as adsorbents, they were used for removal of lead ion from aqueous solution. This study showed that they were very good adsorbents for industrial usage.