Advance oxidation process was employed as a pretreatment of industrial wastewater. For this purpose, the use of heavy metals as a catalyst is necessary but also complicated because homogeneous catalysts are difficult to recover after reaction process. The heterogenization of Cu(II) ions was proposed by taking advantage of the adsorptive characteristics of polymeric matrices. Crosslinked poly(4-vinylpyridine) of 2 and 25% and poly(D-glucosamine) were tested as supports of copper. Adsorption was employed to heterogenize Cu(II) by considering the influences of pH and temperature on the process. The catalysts were evaluated by their metal content, catalytic behavior for the oxidation of phenol and leaching degree after reaction. Poly(4-vinylpyridine) 2% was the best material for Cu(II) immobilization with an adsorption capacity of 90 mg g 21 . Afterward, poly(4-vinylpyridine) 2%, Cu(II) achieved 64% of phenol conversion, which represents a favorable result for the oxidation of phenol as the model of industrial wastewater pretreatments.