Direct Synthesis of 2D-Hexagonal Mesoporous Iron Silicate and its Catalytic Activity for Selective Friedel-Crafts Alkylation

Swapan Das, M. Bhunia, A. Bhaumik
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引用次数: 4

Abstract

D-hexagonal mesoporous iron silicate (HMFeS) has been synthesized hydrothermally in the presence of a mixture of an amphiphilic triblock copolymer, pluronic F127 and 1,2,4-trivinylcyclohexane (TVCH) as swelling agent under acidic aqueous conditions. The direct incorporation of iron(III) into 2D-hexagonal silicate framework can be monitored in a optimized molar ratio of water and hydrochloric acid. The mesophase of the materials was investigated by using small-angle powder X-ray diffractions (PXRD), transmission electron microscopy (TEM) image analysis and nitrogen adsorption/desorption studies. TEM image and PXRD revealed that the material had 2D-hexagonal mesoporous architecture. The morphology of the material was investigated by using scanning electron microscope (SEM) and framework bonding by utilizing FT IR spectroscopy. The atomic absorption spectrophotometer (AAS) was used to estimate the incorporated iron sites within the silicate framework. BET surface area (780 m 2 g -1 ) and peak pore size of HMFeS (10.07 nm) is much higher than the pure silica SBA-15 (611 m 2 g -1 and peak pore size of 9.09 nm). This mesoporous material (HMFeS) acts as a very good catalyst in the Friedel Craft benzylation and benzoylation reactions of arenes under optimized reaction condition using benzyl chloride and benzoyl chloride as the bezylating and benzoylating agents, respectively.
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二维六方介孔硅酸铁的直接合成及其选择性Friedel-Crafts烷基化的催化活性
以两亲性三嵌段共聚物、pluronic F127和1,2,4-三乙烯基环己烷(TVCH)为溶胀剂,在酸性条件下水热合成了d -六方介孔硅酸铁(HMFeS)。在优化的水和盐酸的摩尔比下,可以监测铁(III)直接掺入二维六方硅酸盐框架。采用小角粉末x射线衍射(PXRD)、透射电子显微镜(TEM)图像分析和氮气吸附/解吸研究对材料的中间相进行了研究。TEM和PXRD分析表明,该材料具有二维六方介孔结构。利用扫描电子显微镜(SEM)和红外光谱(FT IR)对材料的形貌进行了研究。采用原子吸收分光光度计(AAS)测定了硅酸盐骨架内的铁结合位点。HMFeS的BET表面积(780 m 2 g -1)和峰值孔径(10.07 nm)远高于纯二氧化硅SBA-15 (611 m 2 g -1)和峰值孔径(9.09 nm)。该介孔材料(HMFeS)在以氯化苄和苯甲酰氯为苯甲酰化剂和苯甲酰化剂的优化反应条件下,对芳烃的Friedel Craft苯甲酰化反应和苯甲酰化反应有很好的催化作用。
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