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A superfine zeolite-Y(FAZ) was synthesized by alkali fusion of coal fly ash followed by hydrothermal treatment. The synthesized zeolite was characterized using X-ray powder diffraction (XRD), infrared spectra (IR) and scanning electron microscope (SEM). A modified fly ash zeolite (FAZ-Fe3+ ) was obtained after the treatment of FAZ with3.0mol/L concentration FeCl3 solution, and it was used for the removal of fluoride ions from aqueous solutions. The results indicated that FAZ-Fe3+ had a higher adsorption capacity for fluoride removal than the unmodified fly ash zeolite (FAZ). When the concentration of fluoride ions was 10mg/L, the adsorption equilibrium time was about 4.5 h for both FAZ-Fe3+ and FAZ, whereas the adsorption capacity was 0.74mg/g for FAZ-Fe3+ and 0.56 mg/g for FAZ, respectively. The kinetic of fluoride sorption onto FAZ-Fe3+ was well-fitted with the pseudo-second-order model. The adsorption isotherms could be described by Freundlich model. Which may indicate that the the mechanism of fluoride sorption onto FAZ-Fe3+ probably was chemisorption onto a heterogeneous material.