Scalable Preparation of Sub-Millimeter Double-Shelled Al₂O₃ Hollow Spheres and Their Rapid Separation from Wastewater after Adsorption of Congo Red

Abstract

Porous double-shelled ceramic hollow spheres (PDSs) have attracted extensive attention due to their high specific surface areas and multifunctional designs. When used in wastewater treatment, millimeter or sub-millimeter spheres can be quickly separated from water by commercial sieves. However, the simple, scalable, and low-cost preparation of sub-millimeter PDSs in the solid phase remains a challenge. Herein, porous PDSs were facilely fabricated via a spheronization process utilizing pseudoboehmite powders and wet gelatin spheres as templates, which broke through the difficulty of preparing PDSs by one-step solid-state synthesis. Treating pseudoboehmite powder with nitric acid can improve the compressive strength of the PDSs. By controlling the rolling time and gelatin concentration of gelatin microspheres, the integrity, shell thickness, and double-shelled spacing of the gelatin microspheres were tuned. When the rolling time was 8–12 min, and the gelatin concentration in gelatin spheres was 250 g/L, and PDSs with a complete double-shelled structure, good mechanical property, and high specific surface area (327.5–509.6 m2/g) were obtained at 600 °C. The adsorption capacities of the PDSs for 100 mg/L Congo red solution (70.7 mg/g) were larger than those of single-shelled hollow spheres (49 mg/g), and larger diameters (608–862 μm) of the PDSs allow them to be rapidly separated from solution by a commercial sieve. This paper provides a facile and scalable method for the preparation of sub-millimeter PDSs and demonstrates their excellent adsorption capacity for Congo red solution.