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A new modified zeolite (HTiZFA) was achieved by dually supporting hexadecyltrimethylammonium (HDTMA) and hydrous titania onto synthetic zeolite from coal fly ash via coating HDTMA and Ti(SO4)2 solution respectively, which has an increased adsorption activity for anion X‐3B dye from aqueous solution. HTiZFA with the optimum removal efficiency was obtained at the coating concentration of 13 mmol/L HDTMA, 20.8 mmol/L Ti(SO4)2, and 2 g/L dosage of zeolite. X‐ray fluorescence, X‐ray diffraction (XRD), scanning electron microscope‐energy dispersive, Fourier transform infrared, Brunauer Emmett Teller (BET), and zeta potential analysis are used to characterize the samples (HTiZFA). In XRD spectrum, no typical peak representing anatase TiO2 crystal suggested that hydrous titania which was impregnated on HTiZFA existed as an amorphous phase. The specific surface area of HTiZFA (32.73–37.71 m2/g) did not alter a lot compared with that of ZFA, but the surface charge of HTiZFA (pH = 8.55) shifted to positive greatly, which caused a considerable enhancement in X‐3B adsorption. It was found that X‐3B sorption on HTiZFA was almost independent on initial pH because the removal rate maintained above 96% in a wide pH range of 3.0–11.0. An increasing qe with an upward temperature confirmed versatile attractive interactions and endothermic sorption nature, and a good ability was observed after several adsorption/desorption circulations. HTiZFA is expected to be a multifunctional adsorbent for treating higher concentration anionic pollutants that cannot be removed by commonly modified products efficiently.

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