Polymer adsorbents have been prepared by post-polymerization crosslinking of the swollen chloromethylated gel-type and macroreticular copolymers of styrene and divinylbenzene. Their morphology has been studied in the dry state by nitrogen adsorption/desorption method and in the swollen state by inverse steric exclusion chromatography. Their sorption properties were tested for the separation of furfural from aqueous solutions. Obtained data were compared with properties of conventional commercial polymer adsorbents Amberlite XAD-2 and XAD-4. At low concentrations of the sorbate in the surrounding solution the highly microporous post-crosslinked materials are much more efficient adsorbents than the conventional commercial polymers. However, their sorption capacity is restricted by limited pore volume and at higher equilibrium concentrations the high surface area macroporous polymers like Amberlite XAD-4 can be more efficient adsorbents.