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The present study describes the preparation of CaCO₃-loaded cellulose aerogel and evaluation of its adsorptive removal of Congo Red (CR) from aqueous solution. The CaCO₃-cellulose aerogel was produced via in situ precipitation of CaCO₃ into as-prepared cellulose aerogel, which was prepared by freeze-drying a crosslinked cellulose solution that was dissolved using a NaOH/urea solution. The particles that formed in the aerogel were confirmed to be calcite CaCO₃. Adsorption studies illustrated that the CR uptake by the aerogel was dependent on the dye concentration and temperature. Incorporation of CaCO₃ into the cellulose aerogel significantly enhanced the adsorption capacity of the aerogel toward CR. The maximum adsorption capacity of the CaCO₃-cellulose aerogel was approximately 75.81 mg/g.