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超声化学法快速合成甲烷和乙烷桥联的周期性介孔有机硅。

Ultrafast sonochemical synthesis of methane and ethane bridged periodic mesoporous organosilicas.

机构信息

Department of Chemistry, Lehigh University, Bethlehem, Pennsylvania 18015, USA.

出版信息

Langmuir. 2010 Jan 19;26(2):1147-51. doi: 10.1021/la902239m.

Abstract

Periodic mesoporous organosilicas (PMOs) with methane and ethane bridging groups were synthesized by the condensation of bis(triethoxysilyl)methane and bis(triethoxysilyl)ethane, respectively, in an ultrafast sonochemical method with a short reaction time of 30 min using a cationic template (1-hexadecyl)trimethylammonium bromide (HTABr). Subsequently, the template HTABr was extracted by another 30 min of sonication in an acetone/HCl mixture. The whole experimental process for the synthesis and extraction of the PMOs took about 1 h, which is much shorter than any other reported methods. Both the PMOs have very high surface areas of 1200-1390 m(2) g(-1) with a narrow pore size distribution of approximately 3 nm. This sonochemical method further extended for the synthesis of large pore (pore size of approximately 5 nm) methane and ethane bridged PMOs using a triblock copolymer Pluronic P123 as template. The methane and ethane bridged PMO materials thus obtained were characterized by small-angle X-ray scattering, transmission electron microscopy, nitrogen sorption, and solid-state NMR techniques.

摘要

周期性介孔有机硅(PMOs)具有甲烷和乙烷桥联基团,分别由双(三乙氧基硅基)甲烷和双(三乙氧基硅基)乙烷在超快速超声化学方法中缩合而成,反应时间短至 30 分钟,使用阳离子模板(1-十六烷基)三甲基溴化铵(HTABr)。然后,通过在丙酮/ HCl 混合物中再进行 30 分钟的超声处理来提取模板 HTABr。PMOs 的合成和提取的整个实验过程耗时约 1 小时,比任何其他报道的方法都要短得多。两种 PMOs 的比表面积均非常高,达到 1200-1390 m(2)g(-1),孔径分布狭窄,约为 3nm。该超声化学方法进一步扩展到使用三嵌段共聚物 Pluronic P123 作为模板合成大孔(孔径约为 5nm)甲烷和乙烷桥联 PMOs。通过小角 X 射线散射、透射电子显微镜、氮气吸附和固态 NMR 技术对得到的甲烷和乙烷桥联 PMO 材料进行了表征。

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