| 大粒径介孔氧化硅微球的优化合成及表征 |
| Optimum Synthesis and Characterization of Mesoporous Large-Scale Silica Microspheres |
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| 摘要: 以非离子型嵌段共聚物为模板剂、正硅酸乙酯为硅源，制备了一种比表面积为712 m2·g-1、孔径6.93 nm、孔容1.06 cm3· g-1、粒径10 μm的介孔SBA-15微球，采用扫描电镜考察了各种合成条件对介孔氧化硅微球形貌的影响，对SBA-15介孔微球的合成条件优化和形成机理进行了研究和探讨。结果表明：介孔氧化硅微球的生长可以看作一个由微小溶胶粒子发生渐进聚沉、成长为较大溶胶粒子的过程；共表面活性剂和无机盐的引入对介孔微球的形成具有辅助作用；合成体系的酸度和晶化阶段之前的陈化条件是介孔微球形成的关键所在。在共聚物的盐酸溶液(1 mol·L-1)中，不添加共表面活性剂和无机盐，仅控制陈化条件于35 ℃静置24 h，100 ℃水热处理24 h，可得到大粒径的介孔SBA-15微球。 |
| 关键词: 嵌段共聚物 介孔 SBA-15 微球 水热合成 |
| 基金项目: |
| Abstract: A large-scale mesoporous SBA-15 microsphere was synthesized using nonionic copolymer as template and tetraethyl orthosilicate (TEOS) as silicon source in an acid solution. The microsphere has a surface area of 712 m2·g-1, large pore size of 6.93 nm, pore volume of 1.06 cm3·g-1 and spherical diameter of ~10 μm. The synthesis conditions and formation mechanism of the microspheres were discussed in virtue of scanning electronic microscope. The experimental results showed that the formation of large-scale microspheres could be attributed to association and aggregation of tiny colloid particles, cosurfactant and inorganic salt were in favor of the formation of silica microspheres, the pH of solution and aging conditions (stirring, temperature) directed immediately the formation of mesoporous microspheres. These large-scale mesoporous silica microspheres would be prepared by an optimum procedure, in which the copolymer and TEOS were sequentially dissolved in 1 mol·L-1 HCl solution without cosurfactant and inorganic salts, the solution was kept under static state for 24 h at 35 ℃ and then treated hydrothermally for 24 h at 100 ℃ to obtain the spherical solids. |
| Keywords: copolymer mesoporous SBA-15 microspheres hydrothermal synthesis |
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| 梁 栋,王 琰,白亚东,李瑞丰.大粒径介孔氧化硅微球的优化合成及表征[J].无机化学学报,2010,26(6):1031-1038. |
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