Alumina-pillared montmorillonite (Al-PILC) has been used as the host material for the immobilization of copper-tetra decachlorophthalocyanine (Cu-Cl14Pc) Complex using ultrasonic technique. Thermogravimetric (TG)/DTG analysis, BET surface area, XRD, FT-IR and UV-VIS spectroscopic techniques have been used to characterize samples containing different concentrations of copper (0.104-0.152 wt.%) in Al-PILC. The studies reveal that Cu-Cl14Pc is present in the porous structure of Al-PILC and that the immobilized samples prepared by ultrasonication contain better-dispersed Cu-Cl14Pc compared to the sample prepared by normal agitation method. The catalytic activity for the hydroxylation of phenol to catechol and hydroquinone using the immobilized Cu-Cl14Pc and H2O2 is reported. The immobilized copper is the active center in the hydroxylation. The method of preparation and dispersion Of Cu-Cl14Pc influence the catalytic activity. (C) 2002 Elsevier Science B.V. All rights reserved.