二次催化溶胶-凝胶法制备多孔硅胶微球

doi:10.3724/SP.J.1077.2011.01090

无机材料学报 ›› 2011, Vol. 26 ›› Issue (10): 1090-1094.DOI: 10.3724/SP.J.1077.2011.01090 CSTR: 32189.14.SP.J.1077.2011.01090

二次催化溶胶-凝胶法制备多孔硅胶微球

赵贝贝¹, 许婵婵², 唐涛^1,3, 李彤³, 张维冰^3,4, 王风云¹

(1. 南京理工大学工业化学研究所, 南京210094; 2. 胜利石油管理局钻井工艺研究院, 东营 257017; 3. 大连依利特分析仪器有限公司, 大连116023; 4. 华东理工大学化学与分子工程学院, 上海 200237)

收稿日期:2010-11-25 修回日期:2011-01-17 出版日期:2011-10-20 网络出版日期:2011-09-20
作者简介:赵贝贝(1985-), 女, 博士研究生. E-mail: gentlebeibei@163.com
基金资助:
江苏省科技支撑计划项目(BE2010731); 大连市科学技术基金(2009J22DW015)

Preparation of SiO₂ Microspheres by Two-step Catalytic Sol-Gel Method

ZHAO Bei-Bei¹, XU Chan-Chan², TANG Tao^1,3, LI Tong³, ZHANG Wei-Bing^3,4, WANG Feng-Yun¹

(1. Institute of Industrial Chemistry, Nanjing University of Science and Technology, Nanjing 210094, China; 2. Research Institute of Drilling Technology, Shengli Petroleum Administration of Sinopec, Dongying 257017, China; 3. Dalian Elite Analytical Instruments Co., Ltd., Dalian 116023, China; 4. School of Chemistry and Molecular Engineering, East China University of Science and Technology, Shanghai 200237, China)

Received:2010-11-25 Revised:2011-01-17 Published:2011-10-20 Online:2011-09-20
Supported by:
Science and Technology Support Project of Jiangsu Province (BE2010731); Dalian Science and Technology Foundation (2009J22DW015)

摘要/Abstract

摘要： 以四乙氧基硅烷(TEOS)为原料, N,N-二甲基甲酰氨(DMF)为模板, 采用二次催化的溶胶-凝胶法制得微米级多孔性硅胶微球. 考察了一次催化水解缩聚过程中水量、乙醇量, 二次催化反应过程中电解质浓度、搅拌速度对微球粒径的影响, 并采用扫描电子显微镜(SEM)、激光粒度分布仪、比表面及孔径分析仪、显微镜-图像颗粒分析系统进行表征. 结果表明, 制得硅胶微球球形规则且无团聚现象, 平均粒径(D50)为8.9μm, 粒径呈典型高斯分布, 比表面积546.67m²/g, 孔体积0.7142m³/g, 孔径主要分布在2~8nm之间, 分布范围窄; 硅胶微球粒径大小随一次催化过程中水量、乙醇量及二次催化过程中电解质浓度增加而增大, 随乳状液形成过程中搅拌速度加快而减小.

关键词: 硅胶微球, 二次催化, 溶胶-凝胶法

Abstract: Micrometer SiO₂ microspheres were prepared by two-step catalytic Sol-Gel method with tetraethoxysilane (TEOS) as starting material and N,N-Dimethylformamide (DMF) as template. The effects of some factors on the diameter and particle size distribution of the SiO₂ microspheres were discussed, such as H₂O quantity and ethanol quantity during the first catalytic process, the electrolyte concentration and stirring speed during the secondary catalytic process. SiO₂microspheres were characterized by SEM, Zetasizer, BET measurements and microscope-particle image analysis system. Results show that SiO2 microspheres are mostly regular-ball with no particle agglomeration. The mean particle size (D50) is 8.9μm, and the particle size distribution follows typical Gaussian distribution. The specific surface area is 546.67m²/g, and pore volume is 0.7142m³/g, with a narrow pore size varied from 2nm to 8nm. Also the particle size increases with water quantity, ethanol quantity and NaCl concentration increaing, but decreases with stirring speed acceleration.

Key words: SiO₂microspheres, two-step catalysis, Sol-Gel method

中图分类号:

TQ127

赵贝贝, 许婵婵, 唐涛, 李彤, 张维冰, 王风云. 二次催化溶胶-凝胶法制备多孔硅胶微球[J]. 无机材料学报, 2011, 26(10): 1090-1094.

ZHAO Bei-Bei, XU Chan-Chan, TANG Tao, LI Tong, ZHANG Wei-Bing, WANG Feng-Yun. Preparation of SiO₂ Microspheres by Two-step Catalytic Sol-Gel Method[J]. Journal of Inorganic Materials, 2011, 26(10): 1090-1094.

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二次催化溶胶-凝胶法制备多孔硅胶微球

Preparation of SiO₂ Microspheres by Two-step Catalytic Sol-Gel Method

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二次催化溶胶-凝胶法制备多孔硅胶微球

Preparation of SiO2 Microspheres by Two-step Catalytic Sol-Gel Method

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Preparation of SiO₂ Microspheres by Two-step Catalytic Sol-Gel Method