A novel polymer/clay composite sorbent based on acrylamide/maleic acid, starch and clay such as kaolin was synthesized with free radical solution polymerization by using ammonium persulfate/N,N,N ,Ntetramethylethylenediamine as redox initiating pair in the presence of poly(ethylene glycol)diacrylate as a crosslinker. Surface morphology was characterized by the scanning electron microscopy technique. FT-IR analysis was used to identify the presence of different repeating units in the semi-interpenetrating polymer networks (semi-IPNs). Some swelling and diffusion characteristics were calculated for different semi-IPNs and hydrogels prepared under various formulations. The hydrogels were used in experiments on sorption of water-soluble cationic dye such as toluidine blue. Sorption of toluidine blue into the polymeric systems was studied by the batch sorption technique at 25 • C. Water uptake and dye sorption properties of the crosslinked polymeric systems were investigated as a function of chemical composition of the hydrogels.