Preparation and porous properties of materials prepared by selective leaching of phlogopite

Abstract

Porous silica products obtained by selective leaching of phlogopite using an acid solution were investigated by XRD, MAS NMR, SEM, TEM, DTA/TG, and N₂ and Ar gas adsorptions. The phlogopite powder was leached by a nitric acid solution at various concentrations (0.01–10 M) at 5–150°C for 10 min–480 h. Selective leaching of the phlogopite powder became extensive when the concentration of nitric acid was >1 M. Only SiO₂ remained after the treatment, the other components (MgO, Al₂O₃, K₂O and Fe₂O₃) being selectively leached from the product. At higher leaching temperatures, the leaching rate became faster and the resulting maximum specific surface area of the porous silica product became larger at each leaching temperature. The porous silica products were found by SEM and TEM, to maintain their original platy particle shape even after the selective leaching. The ²⁹Si MAS NMR spectra of the products, however, revealed that the linkage structure of SiO₄ tetrahedra converted to a framework type from a layered type in the original phlogopite. The porous silica product with the maximum specific surface area (532 m²/g) was obtained by leaching in a nitric acid solution with concentration of 5 M at 90°C for 15 min. The pore-size distribution of the porous silica product was bimodal with micropores of ∼0.7 nm and mesopores of ∼4 nm. The pore size of the products changed from 0.7 nm to 4 nm and further to 6 nm with increased leaching time. The present results are discussed in relation to those reported for phlogopite by other workers.