A novel inorganic-organic hybrid with modified palygorskite (MPGS) and acrylamide was prepared with a heterogeneous redox initiator system composed of a reductive agent (MPGS) together with an oxidant (Ce4+). The MPGS-polyacrylamide (PAM) hybrids were characterized by X-ray diffraction, H-1-NMR, Fourier transform infrared spectroscopy, conductometry, viscometry, and size exclusion chromatography. The MPGS-PAM hybrid could be a starlike and ionic bond hybrid. The ionization behavior of the MPGS-PAM hybrid in deionized water depended strongly on its coil dimension and the palygorskite content in the hybrid. The flocculation performance of the MPGS-PAM hybrid in a kaolin suspension was also related to its intrinsic viscosity and the palygorskite content and was better than that of PAM, except for that of the MPGS-PAM hybrid with a high palygorskite content. (c) 2006 Wiley Periodicals, Inc.