4.5 Article

Alkylation of Toluene to Mono-benzylated Toluene over Micro-mesoporous Zeolite: Effect of Post-synthetic Treatment and Catalytic Application

Journal

Publisher

WILEY-V C H VERLAG GMBH
DOI: 10.1002/ejic.202300674

Keywords

alkylation; zeolites; hierarchical zeolite; mono-benzylated toluene; post-synthetic modification.

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Hierarchical micro-mesoporous zeolites with different pore structure were synthesized using post-synthetic modification with acid and base. The structural changes were investigated through various characterization techniques, and the acidic characteristics of the materials were evaluated. In the toluene alkylation reaction, the base-treated samples showed higher mesoporous pore volume and better catalytic performance.
Post-synthetic modification using acid (HNO3) and base (NaOH) are utilised to synthesize hierarchical micro-mesoporous zeolites with different pore structure. To investigate structural change in materials, X-ray diffraction (XRD), Scanning electron microscope (SEM), Inductive coupled plasma-optical emission spectrometry (ICP-OES), 29Si and 27Al MAS NMR, and N2 adsorption-desorption isotherms techniques were employed. Acid base titration, and ammonia-temperature programmed desorption (NH3-TPD) was performed to evaluate acidic characteristics of materials. As revealed by characterisation, the structure was well preserved after the modification. Hierarchical materials along with parent materials have been evaluated in the toluene alkylation with benzyl alcohol producing mono-benzylated toluene. All zeolite samples were proved to be catalytically active by their result in the alkylation reaction. Acid treated samples were compared with base treated and parent samples. The results indicate that, base modification significantly increases the mesoporous pore volume in all zeolite as compared to acid modification. Moreover, the highest benzyl alcohol conversion was found to be 98 % in the base modified Beta, with the highest mono-benzylated toluene selectivity (69 %). Reaction optimization was also studied by altering reaction duration, temperature, and catalyst amount. The reaction products were analysed using Gas Chromatography (GC) and confirmed using Gas chromatography mass spectrometry (GC-MS). This research study showcases the post-synthetic modification of Beta, ZSM-5, and Y-zeolite using acid and alkali treatment. The resulting catalysts were characterized, and their suitability for the synthesis of benzyl toluene via acid-catalyzed alkylation reaction was investigated. The enhanced catalytic properties observed in the alkali-treated Beta (Beta-BT) catalyst can be attributed to the generation of mesopores within the original microporous zeolite structure and the subsequent increase in the acidity of the catalyst.image

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