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Dually crosslinked graphene oxide reinforced alginate/polyvinyl alcohol (PVA) double network (DN) hydrogels were prepared via a facile freeze/thaw method followed by soaking in a Ca2+ solution. The morphology and structure of the hydrogels were systematically examined by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA). The effects of pH, dosage of hydrogel, adsorption time, and temperature on the adsorptive property of DN hydrogels towards methylene blue (MB) were also studied. Results indicated that the hydrogels exhibited typical 3D porous structures and had an efficient adsorption effect towards MB due to strong interactions between DN hydrogels and MB molecules. The adsorption isotherm was found to coincide with the Langmuir model with a monolayer adsorption. The highest adsorption capacity of DN hydrogels for MB was examined as 480.76 mg·g−1.

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