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Continuous synthesis of monodisperse silica microspheres over 1 μm size

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Abstract

This study presents a robust and scalable method for synthesizing continuously the silica microspheres via the Stöber method. Owing to the superb mixing accessible with gas-liquid segmented flow in coiled microtube, satisfactory morphology and mono-dispersity of silica spheres was obtained. The continuous method was firstly optimized through investigating the effects of various operation parameters on the morphology, particle size, size distribution and chemical structure of silica spheres. Without the surfactant, the size of silica spheres was limited < 850 nm due to the partial blockage of microchannel when synthesizing larger silica spheres. The addition of surfactant migrated the clogging issue, enabling the reliable synthesis of microspheres with diameters over 1 μm within a four times shorter residence time (30 min). Moreover, the mono-dispersity of silica microspheres could be further improved by increasing the gas/liquid ratio in segmented flow due to the more intensified mixing in liquid segments, as verified in visual flow field investigation.

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Acknowledgements

This work was supported by the Youth Innovation Promotion Association of Chinese Academy of Sciences and the Key Technical Personnel of Chinese Academy of Sciences, the Ministry of Science and Technology of China (grant 2016YFA0602603). The work was also supported by Frontier Scientific Research Project funded by Shell under contract No. PT19253.

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Authors and Affiliations

  1. CAS Key Laboratory of Low-Carbon Conversion Science and Engineering, Shanghai Advanced Research Institute, Chinese Academy of Sciences, Shanghai, 201203, People’s Republic of China

    Shian Fei, Yaheng Zhang, Jie Zhang & Zhiyong Tang

  2. School of Chemical Engineering, University of Chinese Academy of Sciences, Beijing, 100049, People’s Republic of China

    Shian Fei, Yaheng Zhang, Jie Zhang & Zhiyong Tang

  3. School of Chemistry and Material Science, University of Science and Technology of China, Hefei, Anhui, 230026, People’s Republic of China

    Zhiyong Tang

  4. School of Physical Science and Technology, ShanghaiTech University, Shanghai, 201210, People’s Republic of China

    Zhiyong Tang

  5. Department of Science and Technology Development, China National Offshore Oil Corporation, Beijing, 100010, People’s Republic of China

    Qing Wu

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  1. Shian Fei
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  3. Jie Zhang
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Correspondence to Jie Zhang, Zhiyong Tang or Qing Wu.

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Highlights

• Synthesis of monodisperse silica microspheres over 1 μm by gas-liquid segmented flow in microreactor.

• Adding the surfactant solved the clogging problem, and preserved the quality of synthesized silica microspheres.

• Adjusting the gas/liquid flow ratio affected the particle size distribution.

Supplementary Information

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ESM 2

Flow performance when gas/liquid ratio = 1:1. (MP4 1.31 MB)

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Fei, S., Zhang, Y., Zhang, J. et al. Continuous synthesis of monodisperse silica microspheres over 1 μm size. J Flow Chem 11, 831–842 (2021). https://doi.org/10.1007/s41981-021-00157-2

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