多孔氧化物微球的制备与表征
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摘要
自从1992年，Mobil公司发明了以超分子模板法合成介孔氧化硅分子筛M41S以来，越来越多的研究者以超分子模板法合成具有不同组成，新型孔道结构以及具有特殊性质的多孔材料。本文选择具有单分散高比表面积的二氧化硅为研究对象，利用化学方法将氧化物如氧化钛和氧化铝包覆在二氧化硅微球的表面，形成具有单分散、高比表面积、且有“核—壳”结构的氧化物复合微球，旨在研究这种新型复合微球的制备方法，并研究“壳层”材料对微孔二氧化硅微球的宏观粒径、形貌、微观孔结构及性能的影响。
本论文工作主要分为五个部分：第一部分以1-烷基胺(alkylamine)为模板剂，通过正硅酸乙酯(TEOS)的水解-缩聚反应，制备出单分散的多孔二氧化硅微球。通过改变1-烷基胺的碳链长度，二氧化硅的颗粒大小、形貌和孔结构都受到明显地影响。随着1-烷基胺的碳链长度的增加，其孔尺寸、孔隙率和孔体积增加，相反比表面积减小。相比之下，用十二胺为模板剂比十六胺和十八胺可得到质量更好的二氧化硅微球，它的最佳合成条件如下：正硅酸乙酯浓度范围为0.11-0.18mol L~(-1)；十二胺浓度为0.016-0.24mol L~(-1)；水解反应温度为15℃左右。随着试样焙烧温度的升高，其比表面积、孔容逐渐增大，而平均孔径变得越来越小。小角X射线衍射(XRD)和高分辨透射电镜(HRTEM)的结果证明用此种方法合成的二氧化硅微球具有无序的微孔结构。
第二部分以前一部分介绍的单分散高比表面积的SiO_2为核，利用静电吸附沉积法在SiO_2微球的表面均匀涂覆TiO_2胶体颗粒，合成具有单分散且高比表面积的SiO_2／TiO_2复合微球。SiO_2／TiO_2复合微球的分散性和形貌与悬浮液的pH值有关，要使TiO_2胶粒均匀涂覆在SiO_2微球的表面，悬浮液的最佳pH范围为3.0～5.0。合成的SiO_2／TiO_2复合微球在600℃煅烧后的比表面积和孔体积分别为960m~2g~(-1)和0.48mLg~(-1)。
第三部分采用单分散高比表面积的SiO_2为核，钛酸丁酯(TTBT)在羟甲基纤维素(HPC)为表面脂化剂和多孔模板剂的作用下水解，合成以微孔SiO_2为核、介孔二氧化钛为壳的具有“核—壳”结构的SiO_2／TiO_2复合微球。复合微球的大小和形貌与混合溶液中HPC的添加量有关。当调控HPC的浓度为3.2mmolL~(-1)时，可得到分散性良好且TiO_2涂层均匀的SiO_2／TiO_2复合微球。经900℃热处理后的SiO_2／TiO_2复合微球中即含有锐钛矿相又含有金红石相。这种“核-
The development of mesoporous silica materials by researchers of Mobil Corporation in 1992 stimulated explosive research on the preparation of porous materials through templates approaches. In this thesis, we focused on the preparation of monodispersed SiO_2 microspheres with high specific surface area, and then oxide particles deposited on the surface of the as-prepared SiO_2 microspheres by two main chemical methods to obtain monodispersed oxide composite microspheres with core/shell structures. The effects of experimental conditions and methods on particle size, morphology and microstructure of composite microspheres were investigated and discussed as main tasks in this paper.
This thesis was divided into five major parts. The first part reported the synthesis of monodispersed microporous silica microspheres by hydrolysis and condensation of tetraethoxysilane (TEOS) using alkylamine as template. The results showed that the alkyl chain length of 1-alkylamine obviously influenced the morphologies and sizes of SiO_2 particles. With increasing the alkyl chain length of 1-alkylamine, the pore volume and average pore size increased, however, surface area decreased. The quality of the silica microspheres synthesized using hexadecylamine and octadecylamine as templates were inferior to that of the silica microspheres synthesized using dodecylamine as a template. The optimal synthesis conditions were as follows: [TEOS] = 0.11-0.18 mol L~(-1), [DDA] = 0.016-0.24 mol L~(-1) and hydrolysis temperature = 15°C. The small angle XRD and HRTEM results confirmed that the prepared SiO_2 microspheres had disordered pore structures
In part 2, monodispersed porous SiO_2/TiO_2 composite microspheres with high specific surface areas were prepared by depositing titania colloid particles on the surface of monodispersed microporous silica microspheres using a simple electrostatic attraction strategy. Uniform titania coatings could be deposited on the surface of silica microspheres by adjusting the pH value of the reaction solution to a optimal pH value ranges of about 3-5. The specific surface area and pore volume of the SiO_2/TiO_2 composite microspheres calcined at 600°C were 960 m~2g~(-1) and 0.48 mLg~(-1), respectively.
In part 3, SiO_2/TiO_2 composite microspheres with microporous core/mesoporous
本论文工作主要分为五个部分：第一部分以1-烷基胺(alkylamine)为模板剂，通过正硅酸乙酯(TEOS)的水解-缩聚反应，制备出单分散的多孔二氧化硅微球。通过改变1-烷基胺的碳链长度，二氧化硅的颗粒大小、形貌和孔结构都受到明显地影响。随着1-烷基胺的碳链长度的增加，其孔尺寸、孔隙率和孔体积增加，相反比表面积减小。相比之下，用十二胺为模板剂比十六胺和十八胺可得到质量更好的二氧化硅微球，它的最佳合成条件如下：正硅酸乙酯浓度范围为0.11-0.18mol L~(-1)；十二胺浓度为0.016-0.24mol L~(-1)；水解反应温度为15℃左右。随着试样焙烧温度的升高，其比表面积、孔容逐渐增大，而平均孔径变得越来越小。小角X射线衍射(XRD)和高分辨透射电镜(HRTEM)的结果证明用此种方法合成的二氧化硅微球具有无序的微孔结构。
第二部分以前一部分介绍的单分散高比表面积的SiO_2为核，利用静电吸附沉积法在SiO_2微球的表面均匀涂覆TiO_2胶体颗粒，合成具有单分散且高比表面积的SiO_2／TiO_2复合微球。SiO_2／TiO_2复合微球的分散性和形貌与悬浮液的pH值有关，要使TiO_2胶粒均匀涂覆在SiO_2微球的表面，悬浮液的最佳pH范围为3.0～5.0。合成的SiO_2／TiO_2复合微球在600℃煅烧后的比表面积和孔体积分别为960m~2g~(-1)和0.48mLg~(-1)。
第三部分采用单分散高比表面积的SiO_2为核，钛酸丁酯(TTBT)在羟甲基纤维素(HPC)为表面脂化剂和多孔模板剂的作用下水解，合成以微孔SiO_2为核、介孔二氧化钛为壳的具有“核—壳”结构的SiO_2／TiO_2复合微球。复合微球的大小和形貌与混合溶液中HPC的添加量有关。当调控HPC的浓度为3.2mmolL~(-1)时，可得到分散性良好且TiO_2涂层均匀的SiO_2／TiO_2复合微球。经900℃热处理后的SiO_2／TiO_2复合微球中即含有锐钛矿相又含有金红石相。这种“核-
The development of mesoporous silica materials by researchers of Mobil Corporation in 1992 stimulated explosive research on the preparation of porous materials through templates approaches. In this thesis, we focused on the preparation of monodispersed SiO_2 microspheres with high specific surface area, and then oxide particles deposited on the surface of the as-prepared SiO_2 microspheres by two main chemical methods to obtain monodispersed oxide composite microspheres with core/shell structures. The effects of experimental conditions and methods on particle size, morphology and microstructure of composite microspheres were investigated and discussed as main tasks in this paper.
This thesis was divided into five major parts. The first part reported the synthesis of monodispersed microporous silica microspheres by hydrolysis and condensation of tetraethoxysilane (TEOS) using alkylamine as template. The results showed that the alkyl chain length of 1-alkylamine obviously influenced the morphologies and sizes of SiO_2 particles. With increasing the alkyl chain length of 1-alkylamine, the pore volume and average pore size increased, however, surface area decreased. The quality of the silica microspheres synthesized using hexadecylamine and octadecylamine as templates were inferior to that of the silica microspheres synthesized using dodecylamine as a template. The optimal synthesis conditions were as follows: [TEOS] = 0.11-0.18 mol L~(-1), [DDA] = 0.016-0.24 mol L~(-1) and hydrolysis temperature = 15°C. The small angle XRD and HRTEM results confirmed that the prepared SiO_2 microspheres had disordered pore structures
In part 2, monodispersed porous SiO_2/TiO_2 composite microspheres with high specific surface areas were prepared by depositing titania colloid particles on the surface of monodispersed microporous silica microspheres using a simple electrostatic attraction strategy. Uniform titania coatings could be deposited on the surface of silica microspheres by adjusting the pH value of the reaction solution to a optimal pH value ranges of about 3-5. The specific surface area and pore volume of the SiO_2/TiO_2 composite microspheres calcined at 600°C were 960 m~2g~(-1) and 0.48 mLg~(-1), respectively.
In part 3, SiO_2/TiO_2 composite microspheres with microporous core/mesoporous
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