Institut für Organische Chemie, Universität Tübingen, Auf der Morgenstelle 18, Germany.
Langmuir. 2009 Dec 1;25(23):13481-7. doi: 10.1021/la901986w.
Silicon hydride terminated silica surfaces were prepared at high temperatures by a chlorination-reduction sequence. SiH groups are desired for further surface modification as an alternative to the native silanol groups which are unfavorable for RPLC applications. Only few silanol groups remain in these materials and mostly SiH moieties with the highest degree of cross-linking are obtained. The retention properties of basic analytes on the SiH terminated material confirm that the surfaces is mostly free of silanols and that therefore the remaining SiOH groups are bulk species. A reagentless, radical initiated hydrosilylation reaction is introduced for the functionalization of the hydride terminated surface with 1-octadecene. (13)C CP/MAS NMR and DRIFT spectroscopy demonstrate the reaction of the carbon-carbon double bond and the SiH group as well as the linkage of C18 groups to the silica surface. These novel C18 materials show promising performance in RPLC separation, especially for the separation of organic bases.
硅氢化物封端的二氧化硅表面通过氯化-还原序列在高温下制备。SiH 基团是进一步表面改性的理想选择，因为其替代了对 RPLC 应用不利的天然硅醇基团。这些材料中只剩下少量的硅醇基团，并且主要得到交联度最高的 SiH 部分。碱性分析物在 SiH 封端材料上的保留性能证实，表面基本上不含硅醇，因此剩余的 SiOH 基团是体相物质。本文引入了一种无试剂、自由基引发的硅氢加成反应，用 1-十八烯对氢化物封端表面进行功能化。(13)C CP/MAS NMR 和 DRIFT 光谱证明了碳-碳双键和 SiH 基团的反应，以及 C18 基团与二氧化硅表面的连接。这些新型 C18 材料在 RPLC 分离中表现出良好的性能，特别是对有机碱的分离。
