Advance oxidation process was employed as a pretreat- ment 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 characteris- tics of polymeric matrices. Crosslinked poly(4-vinylpyridine) of 2 and 25% and poly( D -glucosamine) were tested as sup- ports 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 adsorp- tion capacity of 90 mg g 2 1 . Afterward, poly(4-vinylpyridine) 2%, Cu(II) achieved 64% of phenol conversion, which repre- sents a favorable result for the oxidation of phenol as the model of industrial wastewater pretreatments.