The azo dyes new coccine (NCC) were successfully removed through the adsorption onto PVBTAC-modified α-Al2O3 particles. The optimal conditions of both the surface modification by PVBTAC adsorption and the NCC adsorption were thoroughly investigated. Formerly, polycations PVBTAC were adsorbed onto the nanosized α-Al2O3 particles at p H 8, NaCl 100 mM, with a contact time of 2 h, and initial concentration of 1000 ppm to modify the α-Al2O3 surface. Latterly, the NCC adsorptive removal was conducted at p H 8, NaCl 10 mM, α-Al2O3 adsorbent dosage of 3 mg mL−1, and a contact time of 45 min. Interestingly, the optimal p H of 8 potentially applies to treat real wastewater as the environmental p H range is often about 7–8. High removal efficiency and adsorption capacity of the NCC azo dyes were, respectively, found to be approximately 95% and 3.17 mg g−1 with an initial NCC concentration of 10 ppm. The NCC adsorption on the modified α-Al2O3 particles was well fitted with a Freundlich model isotherm. A pseudo-second kinetic was more suitable for the NCC adsorption on the PVBTAC-modified α-Al2O3 surface than a pseudo-first kinetic. The NCC adsorptive removal kinetic was also affirmed by the FT-IR spectra, based especially on the changes of functional group stretch vibrations of −SO3− group in the NCC molecules and −N+(CH3)3 group in the PVBTAC molecules. The high reusability of the α-Al2O3 particles was proved to be higher than 50% after four generation times.
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