碳化法制备微米级球形多孔二氧化硅

Preparation of micron-sized spherical porous silica by carbonization method

曹永杰，刘伟，陈爱平，姜海波，李春忠

（华东理工大学 a. 材料科学与工程学院；b. 超细材料制备与应用教育部重点实验室，上海 200237）

DOI:10.13732/j.issn.1008-5548.2022.02.015

收稿日期： 2021-05-18，修回日期：2021-06-22，在线出版时间：2022-02-18。

基金项目：国家自然科学基金项目，编号：21838003，91834301；上海市优秀学术带头人计划项目，编号：19XD1401400；中央高校基本科研业务费专项资金资助项目，编号：222201718002。

第一作者简介：曹永杰(1995—)，男，硕士研究生，研究方向为球形二氧化硅的制备及其应用。E-mail：2577232406@qq.com。

通信作者简介：姜海波(1972—)，男，博士，副研究员，硕士生导师，研究方向为新型纳米材料合成、结构调控和过程放大等。E-mail：jianghaibo@ecust.edu.cn。

摘要：使用自制混合反应器，利用环保型气体二氧化碳和廉价型硅源水玻璃，经过碳化、老化、喷雾干燥阶段制备微米级球形多孔二氧化硅；并利用激光粒度仪、扫描电子显微镜、透射电子显微镜等对其进行表征。结果表明：微米级球形多孔二氧化硅的球形规整，分散性良好，粒径分布窄；其孔容为0.42～1.53 cm3/g，比表面积为97.4～375.4 m3/g，为介孔结构；粒径为8.44～28.58 μm，具有光滑的表面。喷雾干燥阶段形成球形多孔二氧化硅，较小的硅酸钠浓度及较慢的缩合反应是球形形成的基础。该法有助于规模化绿色生产球形二氧化硅及其进一步的功能化研究。

关键词： 碳化法；反应器；微米级二氧化硅；球化

Abstract:Micron-sized spherical porous silica was prepared through the stages of carbonization,aging,and spray drying,using environment-friendly gas carbon dioxide and cheap silicon source water glass by self-made mixed reactor,and characterized by laser particle size analyzer,scanning electron microscope,and transmission electron microscope.The results show that the prepared porous silica microspheres have regular spheres,good dispersibility and narrow particle size distribution.The pore volume is 0.42-1.53 cm3/g,the specific surface area is 97.4-375.4 m3/g,and the structure is mesoporous.The particles size is 8.44-28.58 μm,and the surface is smooth.The spherical porous silica is formed in the spray drying stage,and the lower sodium silicate concentration and slower condensation reaction are the basis for the spherical formation.The method is helpful for large-scale green production of spherical silica and its further functionalization research.

Keywords:carbonization method；reactor；micron-sized silica；spheroidization

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