Coal fly ash has been used to synthesize X-type zeolite by alkali fusion followed by hydrothermal treatment. The synthesized fly ash based zeolite (FAZ) has been characterized by various analytical techniques. Copper(II), Nickel(II) and Zinc(II) complexes of N,N 1 -ethylenebis (salicylamide) encapsulated in the supercages of FAZ have been prepared by flexible ligand method and characterized by Fourier Transform infra red spectroscopy (FTIR), X-ray diffraction (XRD) analysis, Scanning electron microscopy (SEM), Atomic absorption spectrometry (AAS), Ultra Violet – Visible spectroscopy and Thermo gravimetric analysis (TGA). These complexes have been found to catalyze the liquid phase hydroxylation of phenol with hydrogen peroxide to yield catechol. It appears to be the first report of catalysis of metal complex encapsulated in fly ash based zeolite.