The biomass of mangosteen shells was utilized as a raw material to prepare activated carbon based on mangosteen shells through a two-step process of mixed alkali carbonization and activation. This study aimed to investigate the efficacy of the activated carbon in removing methylene blue. The optimum preparation conditions for the study are KOH : NaOH : MSC = 1 : 1 : 1 with a particle size of 80 mesh. The activated carbon exhibits a BET specific surface area of 1432.699 m2/g and a Langmuir maximum specific surface area of 2066.130 m2/g. It demonstrates excellent adsorption performance for methylene blue, with a maximum adsorption amount of 985.5 mg/g. Characterization of the activated carbon is conducted using various techniques including Scanning Electron Microscope, X-ray Diffraction Instrument (XRD), Raman Spectrometry (RMS), Fourier IR Spectrometry (FT-IR), XPS, and BET theory. The adsorption results were consistent with the Freundlich model and the pseudo-first-order kinetic model, indicating that the carbon material exhibits multilayer physical adsorption characteristics for methylene blue. The prepared material offers a large specific surface area, good environmental economics, and excellent adsorption performance, making it a promising choice for adsorption material preparation compared to other biomass activated carbons.