Advanced Surface Functionalization of Periodic Mesoporous Silica: Kinetic Control by Trisilazane Reagents
作者:Clemens Zapilko、Markus Widenmeyer、Iris Nagl、Frank Estler、Reiner Anwander、Gabriele Raudaschl-Sieber、Olaf Groeger、Günter Engelhardt
DOI:10.1021/ja065444v
日期:2006.12.1
spectroscopy, and model reactions with calix[4]arene as a mimic for an oxo surface were used to clarify the chemical nature of surface-bonded silyl groups. The trisilylamines exhibited a comparatively slow surface reaction, which allowed for the adjustment of the amount of silylated and nonreacted SiOH groups and led to a stoichiometric distribution of surface functionalities. The 2:1 integral ratio of
介孔二氧化硅MCM-41与一系列新型三甲硅烷基胺(三硅氮烷)(SiHMe2)2NSiMe2R和(SiMe2Vin)2NSiMe2R(R=茚基,去甲茚基,氯丙基,3-(N-吗啉)丙基;Vin=乙烯基)的表面反应,研究了二甲硅烷基烷基胺 (SiHMe2)iPrNSiMe2(CH2)3Cl 和单甲硅烷基二烷基胺 Me2NSiMe2R(R = 茚基、氯丙基、3-(N-吗啉)丙基)。1H、13C 和 29Si MAS NMR 光谱、氮吸附/解吸、红外光谱以及以杯[4]芳烃作为羰基合成表面模拟物的模型反应被用来阐明表面键合的甲硅烷基的化学性质。三甲硅烷胺表现出相对缓慢的表面反应,这允许调整甲硅烷基化和未反应的SiOH基团的量,并导致表面官能团的化学计量分布。2:发现这种三硅氮烷的 SiHMe2 和 SiMe2R 部分的 1 积分比保留在二氧化硅表面上,如混合材料的微量分析以及 13C 和 29Si MAS