单分散大粒径介孔二氧化硅微球的制备及表征

硅酸盐通报 ›› 2022, Vol. 41 ›› Issue (9): 3288-3295.

单分散大粒径介孔二氧化硅微球的制备及表征

关彤, 靳钊, 邵华锋, 孙金芮

青岛科技大学高分子科学与工程学院,青岛 266000

收稿日期:2022-05-02 修回日期:2022-06-13 出版日期:2022-09-15 发布日期:2022-09-27
通讯作者: 靳钊,博士,副教授。E-mail:jinzhao@qust.edu.cn
作者简介:关彤(1998—),女,硕士研究生。主要从事功能材料的研究。E-mail:905113572@qq.com
基金资助:
山东省自然科学基金(ZR2019MB072)

Preparation and Characterization of Monodisperse Mesoporous Silicon Dioxide Microspheres with Large Particle Size

GUAN Tong, JIN Zhao, SHAO Huafeng, SUN Jinrui

School of Polymer Science and Engineering, Qingdao University of Science and Technology, Qingdao 266000, China

Received:2022-05-02 Revised:2022-06-13 Online:2022-09-15 Published:2022-09-27

摘要/Abstract

摘要： 以正硅酸四乙酯(TEOS)为硅源、N,N-二甲基甲酰胺(DMF)为乳化致孔剂,采用酸催化法得到部分缩合的聚硅酸乙酯(PES),再经碱进一步催化得到介孔二氧化硅微球。分析了酸催化剂用量、旋蒸温度对PES粘度及聚合程度的影响以及PES粘度对二氧化硅微球粒径的影响,并研究了氨水用量、乳化致孔剂种类、乳化致孔剂用量以及搅拌速度和后处理方式对二氧化硅微球性质的影响。利用扫描电子显微镜、旋转粘度计、氮吹吸附仪、傅里叶变换红外光谱仪等对所得微球进行表征。结果表明,所制备的介孔二氧化硅微球球形完整,粒径分布均匀,纯度高,微球平均孔径为10.164 4 nm,孔体积为1.023 023 cm³/g,比表面积为396.528 1 m²/g。

关键词: 二氧化硅微球, 大粒径, 介孔, 溶胶-凝胶法, 粘度, 纳微结构

Abstract: Using tetraethyl orthosilicate (TEOS) as silicon source and N,N-dimethylformamide (DMF) as emulsified porogen, partially condensed poly(ethoxy)siloxane (PES) was obtained by acid-catalyzed method. PES was further catalyzed by alkali to obtain mesoporous silicon dioxide microspheres. The effects of the amount of acid catalyst, spin temperature on the viscosity and degree of polymerisation of PES and the effect of PES viscosity on the particle size of silicon dioxide microspheres were investigated. The effects of the amount of ammonia water, the type of emulsified porogen, the amount of emulsified porogen, the stirring speed and the post-treatment method on the properties of silicon dioxide microspheres were also studied. The microspheres were characterized by scanning electron microscopy, rotational viscometer, nitrogen blow adsorption and Fourier infrared spectroscopy. The results show that the prepared mesoporous silicon dioxide microspheres are spherically intact, with uniform particle size distribution and high purity. The average pore size of microspheres is 10.164 4 nm, the pore volume is 1.023 023 cm³/g and the specific surface area is 396.528 1 m²/g.

Key words: silicon dioxide microsphere, large particle size, mesoporous, sol-gel method, viscosity, nano microstructure

中图分类号:

TB34

关彤, 靳钊, 邵华锋, 孙金芮. 单分散大粒径介孔二氧化硅微球的制备及表征[J]. 硅酸盐通报, 2022, 41(9): 3288-3295.

GUAN Tong, JIN Zhao, SHAO Huafeng, SUN Jinrui. Preparation and Characterization of Monodisperse Mesoporous Silicon Dioxide Microspheres with Large Particle Size[J]. BULLETIN OF THE CHINESE CERAMIC SOCIETY, 2022, 41(9): 3288-3295.

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