The present study describes the preparation of CaCO 3 -loaded cellulose aerogel and evaluation of its adsorptive removal of Congo Red (CR) from aqueous solution. The CaCO 3 -cellulose aerogel was produced via in situ precipitation of CaCO 3 into asprepared 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 CaCO 3 . Adsorption studies illustrated that the CR uptake by the aerogel was dependent on the dye concentration and temperature. Incorporation of CaCO 3 into the cellulose aerogel significantly enhanced the adsorption capacity of the aerogel toward CR. The maximum adsorption capacity of the CaCO 3 -cellulose aerogel was approximately 75.81 mg/g.