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Preparation of magnetically recyclable MIL-53(Al)@SiO2@Fe3O4 catalysts and their catalytic performance for Friedel-Crafts acylation reaction

机译:磁性可循环利用的MIL-53(Al)@ SiO2 @ Fe3O4催化剂的制备及其对Friedel-Crafts酰化反应的催化性能

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摘要

Novel magnetically recyclable MIL-53(Ap@SiO2@Fe3O4 catalysts with different MIL-53(Al) contents were prepared by encapsulating magnetic SiO2@Fe3O4 nanoparticles into MIL-53(Al) through an in situ method. The structure of the catalysts was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy, vibration sample magnetometer (VSM), and N-2 adsorption/desorption techniques. Catalytic activity and recovery properties of the catalysts for Friedel-Crafts acylation reaction of 2-methylindole with benzoyl chloride were evaluated. The results showed that the magnetic MIL-53(Ap@SiO2@Fe3O4 catalysts have the larger surface areas, suitable superparamagnetism, and good catalytic activity for Friedel-Crafts acylation reaction. Over 38.8% MIL-53(Ap@SiO2@Fe3O4 catalyst under the reaction conditions of 25 degrees C for 8 h the conversion of 2-methylindole can reach 98%, and the selectivity of 3-acetylindole and that of N-acetylindole can reach similar to 81% and similar to 18%, respectively. After the reaction, the catalyst can be easily separated from the reactant mixture by an external magnet. The recovered catalyst can be reused for five times, and the conversion of 2-methylindole can be kept over 90% and the selectivity of 3-acetylindole can be maintained at 80%. (C) 2015 Elsevier B.V. All rights reserved.
机译:通过将磁性SiO2 @ Fe3O4纳米粒子通过原位包裹在MIL-53(Al)中,制备了具有不同MIL-53(Al)含量的新型可磁循环使用的MIL-53(Ap @ SiO2 @ Fe3O4)催化剂。通过X射线衍射(XRD),透射电子显微镜(TEM),扫描电子显微镜(SEM),傅立叶变换红外(FT-IR)光谱,振动样品磁力计(VSM)和N-2吸附/解吸技术进行表征。对2-甲基吲哚与苯甲酰氯的Friedel-Crafts酰化反应催化剂的催化活性和回收性能进行了评价,结果表明,MIL-53(Ap @ SiO2 @ Fe3O4)磁性催化剂具有较大的比表面积,合适的超顺磁性和在Friedel-Crafts酰化反应中具有良好的催化活性,在25°C下反应8 h时,超过38.8%的MIL-53(Ap @ SiO2 @ Fe3O4催化剂)2-甲基吲哚的转化率可达到98%, 3-乙酰基吲哚和N-乙酰基吲哚可以分别达到约81%和约18%。反应后,催化剂可以容易地通过外部磁体与反应混合物分离。回收的催化剂可以重复使用五次,并且2-甲基吲哚的转化率可以保持在90%以上,而3-乙酰基吲哚的选择性可以保持在80%。 (C)2015 Elsevier B.V.保留所有权利。

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