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The effective separation of dimethyl carbonate (DMC) from its methanol mixture through simple, inexpensive and low energy-input method is a promising and challenging field in the process of organic synthesis. Herein, a reversible adsorption strategy through the assistance of superbase and CO₂ for DMC/methanol separation at ambient condition was described. The process was demonstrated effectively via the excellent CO₂ adsorption efficiency. Notably, the protocol was also suitable to other alcohol (i.e., monohydric alcohol, dihydric alcohol, trihydric alcohol) mixtures. The study provided guidance for potential separation of DMC/alcohol mixture in the scale-up production.