Preparation of a novel adsorbent, mainly composed of Si(Al, Fe)Ca mixed hydrous oxides, from a mixture of coal fly ash and quicklime (CaO) was attempted. Coal fly ash was mixed with NaOH powder and heated to 600°C for 6 h in an electric furnace, and after cooling to room temperature, the produced fused coal ash was mixed with quicklime. The mixture was then stirred in distilled water at room temperature for one day to prepare the adsorbent. With increase in CaO addition to the fused fly ash, the adsorbent changed from an amorphous material to a mixture of calcite [CaCO 3 ] and amorphous phases, then a mixture of calcite and hydrocalumite [Ca 4 Al 2 O 8 (CO 3 )•11H 2 O], and finally that of calcite, hydrocalumite, and portlandite [Ca(OH) 2 ]. The removal ability of the adsorbent for NH 4 + is almost the same and that for Pb 2+ and PO 4 3¹ increases with increasing CaO addition. The removal of NH 4 + , PO 4 3¹ , and Pb 2+ depends on the pH of the solution. The adsorbent containing hydrocalumite without portlandite indicates good ability for multifunctional removal in neutral solution and fixation. Fly ash contents, Si and Al, in the adsorbent contribute to NH 4 + removal by ion exchange of SiAl amorphous gels, PO 4 3¹ removal by synthesis of hydrocalumite to form hydroxyapatite, and Pb 2+ removal by formation of PbSi 2 O 5 •1.6H 2 O. The kinetics of the removal of NH 4 + , PO 4 3¹ , and Pb 2+ using this adsorbent follows the pseudo-second-order kinetics model rather than the pseudo-first-order kinetics model, and the removal of Pb 2+ is faster than that of NH 4 + and PO 4 3¹ . These results indicate that a novel adsorbent with removal abilities for NH 4 + , Pb 2+ , and PO 4 3¹ can be prepared from coal fly ash and quicklime, and suggests a new recycling method for industrial wastes.