By mean of heterophase polymerization on the silica gel surface has been made in situ immobilization of poly[4-methacroyloxy-(4 '-carboxy)-azobenzene], poly[4-methacroyloxy-(4 '-carboxy-3-chloro)-azobenzene] and poly[(4-methacroyloxy-(4 '-carboxy-2 '-nitro)azobenzene has been received new organic-mineral composite materials. As a result of a detailed study of the sorption properties of the synthesized materials, it was found that the best sorption properties for toxic metal ions are silica gel, in situ modified by poly[(4-methacroyloxy-(4 '-carboxy-2 '-nitro)azobenzene. In particular, this composite showed a high sorption capacity for the ions Pb (II) and Cu (II).