Synthesis of mesoporous silica microspheres by a spray-assisted carbonation microreaction method--颗粒学报PARTICUOLOGY

Han, C., Hu, Y., Wang, K., & Luo, G. (2020). Synthesis of mesoporous silica microspheres by a spray-assisted carbonation microreaction method. Particuology, 50, 173-180. https://doi.org/10.1016/j.partic.2019.06.003

Synthesis of mesoporous silica microspheres by a spray-assisted carbonation microreaction method

Chunli Han, Yunpeng Hu, Kai Wang, Guangsheng Luo ^*

The State Key Laboratory of Chemical Engineering, Department of Chemical Engineering, Tsinghua University, Beijing 100084, China

10.1016/j.partic.2019.06.003

Volume 50, June 2020, Pages 173-180

Received 12 May 2019, Revised 12 June 2019, Accepted 17 June 2019, Available online 5 August 2019, Version of Record 7 April 2020.

E-mail: gsluo@tsinghua.edu.cn

Highlights

• Spray-assisted carbonation method to prepare silica microspheres is first reported.

• Synthetic process includes the preparation of a silica sol, gelation, and spray drying.

• Carbonation reaction was conducted in a microreactor with Na2SiO3 as the silica source.

• Mesoporous silica microspheres exhibit excellent dispersity, with diameters of 1–2 μm.

• This method can be extended to prepare various silica materials and related composites.

Abstract

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 300–1149 m²/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.

Graphical abstract

Keywords

Silica microspheres; Mesoporous; Carbonation method; Spray drying; Microreaction

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