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Continuous Flow Friedel–Crafts Alkylation Catalyzed by Silica Supported Phosphotungstic Acid: An Environmentally Benign Process
Topics in Catalysis ( IF 2.8 ) Pub Date : 2021-08-27 , DOI: 10.1007/s11244-021-01497-y
Zsófia Császár 1 , József Bakos 1 , Gergely Farkas 1 , Tatjána Juzsakova 2 , Miklós Jakab 3 , Szabolcs Balogh 4 , Ágnes Szegedi 5 , Hanna Solt 5 , Jenő Hancsók 6
Affiliation  

Six silica-supported phosphotungstic acid catalysts (PTA/SiO2) of different composition (20–70 wt% PTA content) have been synthesized and characterized by elemental analysis, BET, BJH, NH3-TPD methods, FT-IR spectroscopy of adsorbed pyridine and 1H MAS NMR techniques. The new composite catalysts were first applied in the Friedel–Crafts alkylation of toluene with 1-octene as a benchmark process under batch conditions in order to screen their activity and recyclability. The combined analytical techniques together with the catalytic studies enabled the identification of the main factors affecting the activity of the catalysts. Based on these preliminary experiments, the best performing catalyst system (50 wt% PTA/SiO2) was investigated in continuous flow mode using an in-house-made flow reactor. The thorough screening of the reaction conditions (temperature, toluene/1-octene molar ratio and flow rate) provided firm evidence that the 50 wt% PTA/SiO2 composite is highly active, selective and stable catalyst under mild reaction conditions even at elevated flow rate. Additionally, the catalyst used in the flow mode could successfully be regenerated and reused in the alkylation process.



中文翻译:

由二氧化硅负载的磷钨酸催化的连续流动 Friedel-Crafts 烷基化:一种环境友好的过程

合成了六种不同组成(PTA 含量为 20–70 wt%)的二氧化硅负载磷钨酸催化剂(PTA/SiO 2),并通过元素分析、BET、BJH、NH 3 -TPD 方法、吸附的 FT-IR 光谱表征。吡啶和1 H MAS NMR 技术。新的复合催化剂首先应用于甲苯与 1-辛烯的 Friedel-Crafts 烷基化反应,作为基准工艺在间歇条件下筛选其活性和可回收性。将分析技术与催化研究相结合,可以确定影响催化剂活性的主要因素。基于这些初步实验,性能最好的催化剂体系(50 wt% PTA/SiO 2) 使用内部制造的流动反应器在连续流动模式下进行研究。对反应条件(温度、甲苯/1-辛烯摩尔比和流速)的彻底筛选提供了确凿的证据,表明 50 wt% PTA/SiO 2复合材料在温和的反应条件下是高活性、选择性和稳定的催化剂,即使在高流速下速度。此外,流动模式中使用的催化剂可以成功地再生并在烷基化过程中重复使用。

更新日期:2021-08-29
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