The potential of fly ash procured form coal-fired thermal power plants was studied as a heterogeneous catalyst in the oxidation of aqueous sodium sulfide solutions with hydrogen peroxide in the temperature range of 303-323 K. The effects of various parameters (source of fly ash, fly ash loading, initial concentrations of sodium sulfide and hydrogen peroxide, electrolyte and deactivation of catalytic effect of fly ash) were studied. For an initial sodium sulfide and hydrogen peroxide concentration of 26.98 x 10-2 kmol m-3 and 24.28 x 10-2 kmol m-3 respectively, only 4% (w/v) fly ash loading intensified the rate of oxidation by a factor of 4.52 over that without fly ash at 303 K. The deactivation of the catalytic effect of fly ash was found to be less than 20% even after six repeated uses. The kinetics of aqueous phase decomposition of hydrogen peroxide was also studied in the presence of fly ash in alkaline medium.The potential of fly ash procured form coal-fired thermal power plants was studied as a heterogeneous catalyst in the oxidation of aqueous sodium sulfide solutions with hydrogen peroxide in the temperature range of 303-323 K. The effects of various parameters (source of fly ash, fly ash loading, initial concentrations of sodium sulfide and hydrogen peroxide, electrolyte and deactivation of catalytic effect of fly ash) were studied. For an initial sodium sulfide and hydrogen peroxide concentration of 26.98 × 10-2 kmol m-3 and 24.28 × 10-2 kmol m-3 respectively, only 4% (w/v) fly ash loading intensified the rate of oxidation by a factor of 4.52 over that without fly ash at 303 K. The deactivation of the catalytic effect of fly ash was found to be less than 20% even after six repeated uses. The kinetics of aqueous phase decomposition of hydrogen peroxide was also studied in the presence of fly ash in alkaline medium.