Facile preparation of hollow amino-functionalized organosilica microspheres by a template-free method
Facile preparation of hollow amino-functionalized organosilica microspheres by a template-free method
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无模板法简便制备空心氨基功能化有机硅微球
DOI：
10.1039/c2jm33220e
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发表时间：
2012-01-01
影响因子：
--
通讯作者：
Xu, Jian
中科院分区：
文献类型：
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作者：
Yang, Xiaoli;Zhao, Ning;Xu, Jian
基于3-氨丙基三乙氧基硅烷（APTES）和四乙氧基硅烷（TEOS）在水溶液体系中的水解和缩合反应，在没有额外模板剂和催化剂的情况下，开发了一种简单的方法来制备中空的氨基官能化有机二氧化硅微球。通过扫描电子显微镜、透射电子显微镜和N2吸附-脱附测量对所得中空杂化有机硅微球进行了表征。傅里叶变换红外光谱、固体核磁共振谱、X射线光电子能谱和热重分析的结果表明合成的空心微球的组成和表面氨基的存在。提出了一种自模板和自催化的中空微球的形成机制：质子化的APTES既作为反应的催化剂，又作为疏水前体液滴的稳定剂，而液滴本身作为软模板，前体的消耗导致中空结构的形成。通过调节前驱体的组成、搅拌速度和反应温度可以控制有机硅微球的形貌和粒径分布。杂化有机硅微球的壳层上有一个开孔的大空腔和表面上的反应性氨基基团，这预示着许多潜在的应用。介绍了微球作为吸附剂和相变微胶囊的应用实例。
A facile method was developed to fabricate hollow amino-functionalized organosilica microspheres based on the hydrolysis and condensation of 3-aminopropyltriethoxysilane (APTES) and tetraethoxysilane (TEOS) in an aqueous system without an additional template and catalyst. The hollow hybrid organosilica microspheres obtained have been characterized by scanning electron microscopy, transmission electron microscopy, and N2 adsorption–desorption measurements. The results of Fourier transform infrared spectroscopy, solid-state NMR spectroscopy, X-ray photoelectron spectroscopy and thermogravimetric analysis displayed the composition of the synthesized hollow microspheres and the presence of amino groups on the surface. A self-templated and self-catalyzed mechanism for the formation of the hollow microspheres is proposed: the protonated APTES acts as both a catalyst for the reaction and a stabilizer for the hydrophobic precursor droplets, while the droplets themselves act as soft templates, and the consumption of the precursors leads to the formation of a hollow structure. The morphology and the size distribution of the organosilica microspheres can be controlled by tuning the composition of the precursors, and the stirring speed, as well as the reaction temperature. The large cavity with an open hole on the shell and the reactive amino groups on the surface of the hybrid organosilica microspheres promise many potential applications. Examples of employing the microspheres as adsorbents and phase change microcapsules have been presented.