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最常见的中孔有序硅石和有机硅石的硅醇基含量的定量测定:总硅醇基与可及硅醇基。

Quantification of silanol sites for the most common mesoporous ordered silicas and organosilicas: total versus accessible silanols.

机构信息

COMOC, Center for Ordered Materials, Organometallics and Catalysis, Department of Inorganic and Physical Chemistry, Ghent University, Krijgslaan 281 (S-3), 9000 Ghent, Belgium.

出版信息

Phys Chem Chem Phys. 2013 Jan 14;15(2):642-50. doi: 10.1039/c2cp42811c. Epub 2012 Nov 27.

Abstract

IR and NMR spectroscopy were used to determine the silanol content in the most common mesoporous ordered silicas: MCM-41, MCM-48, SBA-15 and SBA-16. In addition, a spray dried MCM-41 and an ethene bridged PMO are investigated. The results are compared with a commercial chromatographic silica (Nucleosil). The complete distribution of surface and bulk silanols, and of isolated, geminal and vicinal silanols for all these materials is presented. A distinction is made between the total silanol number and the reachable or surface silanol content. The latter is determined by controlled reactions with simple silanes. All mesoporous ordered silicas, and especially the thick walled SBA-type materials and the PMO contain a surprisingly high amount of total silanol sites, albeit that up to 90% of these silanols are buried inside the walls and are not reachable for small silanes.

摘要

采用红外和核磁共振光谱法测定了最常见的介孔有序硅石

MCM-41、MCM-48、SBA-15 和 SBA-16 中的硅醇含量。此外,还研究了喷雾干燥的 MCM-41 和乙烯桥接的 PMO。将结果与商业色谱硅胶(Nucleosil)进行了比较。给出了所有这些材料的表面和体相硅醇以及孤立、偕二和邻位硅醇的完整分布。区分了总硅醇数和可及或表面硅醇含量。后者通过与简单硅烷的受控反应来确定。所有介孔有序硅石,尤其是厚壁 SBA 型材料和 PMO,都含有数量惊人的总硅醇位,尽管其中多达 90%的硅醇埋藏在壁内,无法与小硅烷接触。

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