Synthesis and Surface Chemistry of Spherical Mesoporous Organic−Inorganic Hybrid Particles with an Integrated Alcohol Functionality on the Pore Surface

Synthesis and Surface Chemistry of Spherical Mesoporous Organic−Inorganic Hybrid Particles with an Integrated Alcohol Functionality on the Pore Surface
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孔表面具有集成醇官能团的球形介孔有机-无机杂化颗粒的合成和表面化学

DOI:
10.1021/cm035014t
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发表时间:
2004
影响因子:
8.6
通讯作者:
J. E. O'gara
J. E. O'gara
中科院分区:
材料科学2区
文献类型:
--
作者:
Julia Ding;C. Hudalla;James T. Cook;D. Walsh;Cheryl E. Boissel;P. Iraneta;J. E. O'gara

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描述了新型介孔有机-无机球形杂化颗粒,其含有孔表面不可或缺的 3-羟丙基有机官能团。 3-羟丙基杂化颗粒的合成分三个步骤,从四乙氧基硅烷和[3-(甲基丙烯酰氧基)丙基]三甲氧基硅烷的4:1(mol/mol)混合物开始,其中单体聚合成聚(有机烷氧基硅烷)油,然后通过溶胶-凝胶反应形成杂化硅酸盐珠,最后进行碱性水热处理以从酯保护基中释放醇。通过核磁共振波谱和氮吸附分析对硅酸盐前体和最终产物进行了表征。通过运行一系列经典醇反应,包括溴化、酯化(氨基甲酸和碳酸)和醚化(威廉姆森,环氧化物开环),探索了杂化醇官能团的异质表面化学。溴化类似物通过氰化作用进一步转化……
Novel mesoporous organic−inorganic spherical hybrid particles are described that contain a 3-hydroxypropyl organic functionality which is integral to the pore surface. The 3-hydroxypropyl hybrid particle is synthesized in three steps starting from a 4:1 (mol/mol) mixture of tetraethoxysilane and [3-(methacryloxy)propyl]trimethoxysilane, where the monomers are polymerized to a poly(organoalkoxysilane) oil, followed by sol−gel reaction to the hybrid silicate bead, which is finally subjected to an alkaline hydrothermal treatment to liberate the alcohol from the ester protecting group. The silicate precursor and final product were characterized by NMR spectroscopy and nitrogen sorption analysis. The heterogeneous surface chemistry of the hybrid's alcohol functionality was explored by running a series of classical alcohol reactions including bromination, esterification (carbamic and carbonic), and etherification (Williamson, epoxide ring opening). The brominated analogue was further converted via cyanation and...