The present study is aimed at investigations on the catalytic activity for total oxidation of volatile organic compounds (VOCs), such as toluene, acetone, n-hexane and dichlorobenzene onto zeolite-like materials synthesized from coal fly ash (FA) directed to development of an economically efficient approach for degradation of VOCs. Fly ash zeolites (FAZ) were prepared by alkaline conversion of FA collected from Thermal Power Plants supplied with lignite coal from "Maritza-East" basin in Bulgaria. Different synthesis procedures double stage fusion-hydrothermal activation, fusion-atmospheric crystallization and atmospheric aging were applied. The synthesis products were identified by X-ray diffraction, and were assigned to zeolite Na-X. Scanning electron microscopy images reveal submicron dimensions of the composing crystallites. Nitrogen adsorption/desorption measurements reveal a mixed micro-mesoporous structure and specific surface area between 116 and 396 m(2)/g for the obtained FAZ. Relationships between surface properties, iron content and the catalytic activity of FAZ were investigated and discussed. Copper-modified fly ash zeolites (Cu-FAZ) were prepared by incipient wetness impregnation technique with copper acetylacetonate. The loading of 5 wt. % copper on the zeolite samples was achieved. The catalytic activity of FAZ and Cu-FAZ in the total oxidation of model VOCs mixture containing n-hexane, acetone, toluene, 1,2 dichlorobenzene was evaluated.