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Mechanochemical and wet chemical syntheses of CaIn-layered double hydroxide and its performance in a transesterification reaction compared to those of other Ca2M(III) hydrocalumites (M: Al, Sc, V, Cr, Fe, Ga) and Mg(II)-, Ni(II)-, Co(II)- or Zn(II)-based hydrotalcites
Journal of Catalysis ( IF 7.3 ) Pub Date : 2020-09-02 , DOI: 10.1016/j.jcat.2020.07.038
Márton Szabados , Anna Adél Ádám , Péter Traj , Szabolcs Muráth , Kornélia Baán , Péter Bélteky , Zoltán Kónya , Ákos Kukovecz , Pál Sipos , István Pálinkó

The feasibility of indium introduction into the hydrocalumite group of layered double hydroxides (LDHs) was investigated for the first time. Mechanochemical and co-precipitation techniques were applied in the syntheses. During the development of preparation, a yet unknown CaIn chloride-hydroxide solid side-product was found and synthesized in phase-pure state. The as-prepared materials were characterized by X-ray diffractometry, Fourier-transform infrared, Raman, and UV–Vis diffuse reflectance spectroscopies. Their thermal behavior was mapped up to 900 °C, while the surface and textural attributes were studied by scanning and transmission electron microscopies, specific surface area measurements and pore size analysis. For the LDH, the Ca2.3InCl(OH)6.6·4H2O and for the side-product, the Ca3In4Cl2(OH)16·6H2O stoichiometric formula was calculated. Various further hydrocalumites (M(III): Al3+, Sc3+, V3+, Cr3+, Fe3+, Ga3+) were synthesized, their surface basicity was investigated by CO2 temperature programmed desorption. These materials and the indium-containing phases were tested as catalysts in the transesterification reactions of dimethyl carbonate with glycerol. All solids proved to be active: their glycerol conversion capabilities and recycling abilities were determined and compared to the well-known Mg-, Ni-, Co–, Zn-based hydrotalcites.



中文翻译:

与其他Ca 2 M(III)水钙铝石(M:Al,Sc,V,Cr,Fe,Ga)和Mg(II)相比,CaIn层状双氢氧化物的机械化学和湿化学合成及其在酯交换反应中的性能-,Ni(II)-,Co(II)-或Zn(II)基水滑石

首次研究了将铟引入层状双氢氧化物(LDHs)的水铝钙石组的可行性。在合成过程中采用了机械化学和共沉淀技术。在制备过程中,发现了未知的CaIn氯化物-氢氧化物固体副产物,并以纯相合成。所制备的材料通过X射线衍射,傅立叶变换红外,拉曼和UV-Vis漫反射光谱学进行表征。将它们的热行为映射到最高900°C,同时通过扫描和透射电子显微镜,比表面积测量和孔径分析研究表面和纹理属性。对于LDH,Ca 2.3 InCl(OH)6.6 ·4H 2O和副产物,计算出Ca 3 In 4 Cl 2(OH)16 ·6H 2 O化学计量公式。合成了其他各种水钙铝石(M(III):Al 3+,Sc 3+,V 3+,Cr 3+,Fe 3+,Ga 3+),并通过CO 2研究了它们的表面碱性。程序升温脱附。在碳酸二甲酯与甘油的酯交换反应中,将这些材料和含铟的相作为催化剂进行了测试。事实证明,所有固体均具有活性:确定了它们的甘油转化能力和回收能力,并将其与众所周知的基于Mg,Ni,Co,Zn的水滑石粉进行比较。

更新日期:2020-09-20
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