Acrylamide has been polymerized between the layers of kaolinite by heat treatment. Acrylamide monomer was first intercalated by the displacement reaction between a kaolinite-N-methylformamide (NMF) intercaJation compound and a 10% acrylamide aqueous solution. The resulting intercalation compound showed a basal spacing of 11.3 A. Infrared (IR) spectroscopy and '3C nuclear magnetic resonance spectroscopy with cross polarization and magic angle spinning ('3C CP/MAS-NMR) indicated the replacement of NMF by acrylamide. IR spectroscopy also showed the formation of hydrogen bonds with the hydroxyls of kaolinite. When the kaolinite-acrylamide intercalation compound was heated at 300"C for 1 hr, the basal spacing increased to 11.4 A, and IR and '3C CP/MAS-NMR showed the disappearance of C----C bonds, indicating the polymerization of acrylamide. The heat-treated kaolinite- acrylamide intercalation compound was resistant to 30 min-washing with water, whereas the untreated kaolinite-acrylamide intercalation compound collapsed after the same treatment, an observation consis- tent with acrylamide polymerization between the layers of kaolinite. IR spectroscopy revealed that poly- acrylamide was hydrogen bonded to kaolinite, but in a manner different from the hydrogen bonding of acrylarnide.