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A novel spray-assisted carbonation microreaction method for the synthesis of mesoporous silica microspheres is reported.The synthetic process comprises the preparation of a silica sol via a carbonation reaction,rapid gelation at high temperature,and subsequent rapid solvent evaporation by spray drying.The carbonation microreaction was conducted in a membrane dispersion microreactor,in the presence of sodium silicate and carbon dioxide reactants.The as-synthesized silica microspheres exhibit a uniform mesostructure,excellent dispersity,and a narrow particle size distribution,with average diameters of 1-2 μm,Brunauer-Emmett-Teller surface areas of 300-1149m2/g,and total pore volumes of 0.21-1.82 cm3/g.Relatively low concentrations of the silicate species and well-controlled silica condensation rates are responsible for the formation of the observed spherical morphology.The synthetic process is of significant practical importance as a result of using low-cost raw materials,and because of the excellent controllability and process stability displayed.Furthermore,this rapid and flexible method may be extended to the synthesis of various silica materials and their composites.