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Porous rGO/SiO₂ nanocomposites with a “core-shell” structure were prepared as an efficient adsorbent for the liquid-phase adsorption of cationic neutral red (NR) dye. The samples were characterized with powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), thermogravimetric analysis (TG), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and N₂ and water vapor adsorption/desorption methods. The NR removal ability and kinetics of the adsorption process of SiO₂ and the rGO/SiO₂ nanocomposites were investigated at 298 K. The rGO/SiO₂ nanocomposite SG 0.30 showed a superior adsorption of NR dye. In regard to NR at pH 5, we measured a superior adsorption capacity of 66.635 mg/g at an initial NR concentration of 50 mg/L. The experimental adsorption capacity of SG 0.30 was 3.791 times higher than that of SiO₂. Then, we compared the results with similar materials used for NR removal. Moreover, the water adsorption sites provided by the nitrogen- and oxygen-containing groups might be one of the reasons for the increased adsorption of water vapor. The broad range of properties of the rGO/SiO₂ nanocomposite, including its simple synthesis, ability to be mass prepared, and strong adsorption properties, makes it a truly novel adsorbent that can be industrially produced, and shows potential application in the treatment of wastewater-containing dyes.