The solid silica sulfuric acid was used to heterogeneous sulfonation of polystyrene waste dissolved in organic solvent. After sulfonation, small suspended particles of polystyrene derivatives were easily separated from much bigger particles of silica sulfuric acid by filtration and from solvent mostly by decantation and additionally by evaporation. The characteristics of adsorption of heavy metal cations on resins from polystyrene were compared with that of commercial resins. It was proved that synthesized resins are effective cation exchangers. The advantage of obtained resins was their high rate of metal removal.