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首页> 外文期刊>Journal of the Taiwan Institute of Chemical Engineers >Phenyl-amino sulfonic solid acid-MCM-41 complex: A highly active and selective catalyst for the synthesis of mono-alkylated products in the solvent free tert-butylation of phenol
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Phenyl-amino sulfonic solid acid-MCM-41 complex: A highly active and selective catalyst for the synthesis of mono-alkylated products in the solvent free tert-butylation of phenol

机译：苯氨基磺酸固体酸-MCM-41络合物：一种高活性和选择性的催化剂，用于在苯酚的无溶剂叔丁基化中合成单烷基化产物

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摘要

A simple post synthesis route was established for heterogenizing 3-(3-aminophenylamino)propane-1- sulfonic acid onto functionalized mesoporous MCM-41 to give an inorganic–organic hybrid, MCM-3- NHPhSO3H. The XRD analysis of the hybrid material exhibited three well-resolved diffraction peaks for the (1 0 0), (1 1 0) and (2 0 0) planes, which indicates the retention of the mesostructure. The ~(13)C CP-MAS NMR spectroscopy of the hybrid material showed four intense carbon peaks from 107 to 131 ppm, corresponding to the aromatic ring of the grafted ligand. Surface properties of the material revealed a pore size of 1.84 nm and a specific surface area of 572 m~2 g~(-1). The TEM images of the hybrid showed a well-ordered honey-comb structure after the series of modifications. The catalytic performance of MCM- 3-NHPhSO3H resulted in 99% conversion of tert-butylphenol (TBA) with selectivity to only monoalkylated products. The initial selectivity yield of 98% tert-butylphenol ether (TBPE) had decreased until a product distribution of 64% 2-(tert-butyl)phenol (2-TBP), 32% 4-(tert-butyl)phenol (4-TBP), 3% (TBPE) and 1% isobutene (IBE) was obtained. The catalyst could be regenerated without significant loss in reactivity.
机译：建立了一个简单的后合成路线，将3-（3-氨基苯基氨基）丙烷-1-磺酸杂化到功能化的介孔MCM-41上，得到无机-有机杂化物MCM-3-NHPhSO3H。杂化材料的XRD分析显示了（1 0 0），（1 1 0）和（2 0 0）平面的三个分辨良好的衍射峰，这表明介观结构的保留。杂化材料的〜（13）C CP-MAS NMR光谱显示了从107至131 ppm的四个强碳峰，对应于接枝的配体的芳环。该材料的表面性质显示其孔径为1.84 nm，比表面积为572 m〜2 g〜（-1）。经过一系列修改后，杂种的TEM图像显示出井井有条的蜂窝状结构。 MCM-3-NHPhSO3H的催化性能导致99％的叔丁基苯酚（TBA）转化为仅单烷基化产物。直到98％的叔丁基苯酚醚（TBPE）的初始选择性产率下降，直到产物分布为64％的2-（叔丁基）苯酚（2-TBP），32％的4-（叔丁基）苯酚（4- （TBP），3％（TBPE）和1％异丁烯（IBE）。催化剂可以再生而没有明显的反应性损失。

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