In this paper, a novel process using the combination of a microreactor and a stirred-tank reactor for the controlled preparation of silica materials with a large-pore-volume and narrow-pore-diameter distribution was presented. At the precipitation stage, the gelation time was controlled to within 50 ms by improving the mixing performance in the microreactor. After further mixing and acidizing in a stirred-tank reactor, silica with a pore volume of 1.96 mL/g and a specific surface area of 476.1 m2/g was prepared. The primary particle size was 10 nm, and the variance of the logarithmic pore diameter was approximately 0.20, which indicated that the pore-diameter distribution was narrow and uniform particles were in favor of accumulating uniform pores. At the drying stage, with the addition of poly­(vinyl alcohol) to a silica slurry, the process conditions were optimized, and silica with a larger pore volume of 2.13 mL/g was prepared.

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