Hierarchically porous SiO2/C hollow microspheres (HPSCHMs) were synthesized by a hydrothermal and NaOH-etching combined route. The adsorption performance of the prepared HPSCHMs was investigated to remove Congo Red (CR) in aqueous solution. The results show that the synthesized composite possesses a hollow microspherical structure with hierarchical pores and a diameter of about 100–200 nm, and its surface area is up to 1154 m2 g−1. This material exhibits a remarkable adsorption performance for CR in solution, and its maximum adsorption amount for CR can reach up to 2512 mg g−1. It shows faster adsorption and much higher adsorption capacity than the commercial AC and γ-Al2O3 samples under the same conditions. The studies of the kinetics and thermodynamics indicate that the adsorption of CR on the PHSCHM sample obeys the pseudo-second order model well and belongs to physisorption. The adsorption activation energy is about 7.72 kJ mol−1. In view of the hierarchically meso–macroporous structure, large surface area and pore volume, the HPSCHM material could be a promising adsorbent for removal of pollutants, and it could also be used as a catalyst support.
