Polymer-supported macrocyclic polythioethers (7a, b, and 8) were prepared from chloromethylated polystyrene resins (6) and 14- or 20-membered a hydroxyl group containing polythioethers (3a, b, and 5), which were synthesized by the reaction of the corresponding dithiols with 1,3-dichloro-2-propanol (2). The polymer-supported polythioethers were found to be highly efficient adsorbents of Ag(I), moderately effective for Cu(II), but less effective for Cd(II). For Ag(I) the binding ability of 7a is almost independent of the morphology of the polymer support, whereas for Cu(II) the binding ability depends on the morphology. Adsorbed Ag(I) or Cu(II) were removed by treatment with an ammonia solution from the polymer-supported macrocyclic polythioethers, which can be re-used without a significant decrease in binding ability.