Facile synthesis of MIL-100(Fe) under HF-free conditions and its application in the acetalization of aldehydes with diols

Facile synthesis of MIL-100(Fe) under HF-free conditions and its application in the acetalization of aldehydes with diols
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无HF条件下简易合成MIL-100(Fe)及其在醛与二醇缩醛化反应中的应用

DOI:
10.1016/j.cej.2014.07.119
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发表时间:
2015
影响因子:
15.1
通讯作者:
Weidong Zhu
Weidong Zhu
中科院分区:
工程技术1区
文献类型:
--
作者:
Fumin Zhang;Jing Shi;Yan Jin;Yanghe Fu;Yijun Zhong;Weidong Zhu

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以硝酸铁和偏三甲酸(H3BTC)为原料,在无HF条件下,通过简单的低温(<100℃)反应合成了介孔羧酸铁[MIL-100(Fe)]。用X射线衍射仪、氮气吸附、XPS、热重分析、红外光谱和扫描电子显微镜对合成的MIL-100(Fe)进行了系统的表征,并将其用于催化多种醛与二醇的液相缩合反应。与其他常用的制备MIL-100(Fe)的方法相比,目前的合成策略具有合成条件温和、环境友好等优点。此外,合成的MIL-100(Fe)催化剂在醛和二元醇的缩醛反应中表现出优异的催化性能,这是由于可用的不饱和金属中心的Lewis酸性,并伴随着MIL-100(Fe)骨架中丰富的介孔笼,优于商业树脂和沸石催化剂。
Mesoporous iron(III) carboxylate [MIL-100(Fe)] has been successfully synthesized by a simple unappreciated low-temperature (<100 °C) route via the reaction of ferric nitrate and trimesic acid (H3BTC) under HF-free conditions. The synthesized MIL-100(Fe) was systematically characterized by XRD, N2adsorption, XPS, TGA, FT-IR, and SEM and used as a catalyst in the liquid-phase acetalization of various aldehydes with diols. In comparison with other methods commonly used for the preparation of MIL-100(Fe), the current synthesis strategy has merits such as mild and environmentally benign synthesis conditions. Additionally, the synthesized MIL-100(Fe) shows some excellent catalytic properties in the acetalization of aldehydes with diols, due to the Lewis acidity of the available unsaturated metal sites, accompanied with abundant mesoporous cages in the framework of MIL-100(Fe), superior to commercial resin and zeolite catalysts.
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