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Casein (CS) and graphene oxide (GO) were employed for the fabrication of a casein/graphene oxide (CS/GO) aerogel by vacuum freeze drying. Fourier transform infrared spectroscopy, scanning electron microscopy, surface area and micropore analysis (BET), and thermogravimetric analysis were used to characterize the specific surface area, structure, thermal stability, and morphology of the CS/GO aerogel. The influence of experimental parameters such as the GO mass fraction in the aerogel, metering of the adsorbent, pH, contact time, and temperature on the adsorption capacity of the CS/GO aerogel on methylene blue (MB) was also investigated. According to Langmuir isotherm determination, the maximum removal rate of MB from the CS/GO aerogel was 437.29 mg/g when the temperature was 293 K and pH was 8. Through kinetic and thermodynamic studies, it is found that adsorption follows a pseudo-second-order reaction model and is also an exothermic and spontaneous process.