Synthesis of a novel super-microporous layered material and its catalytic application in the vapor-phase Beckmann rearrangement of cyclohexanone oxime |
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Authors: | Xianji Guo Wenhua Hou Weiping Ding Yining Fan Qijie Yan Yi Chen |
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Affiliation: | aKey Laboratory of Mesoscopic Chemistry, Nanjing University, Nanjing 210093, PR China bDepartment of Chemistry, Zhengzhou University, Zhengzhou 450052, PR China |
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Abstract: | A novel well-ordered super-microporous layered material, silica-pillared niobic acid, was synthesized by a guest-exchange route and structurally characterized by powder X-ray diffraction (XRD), infrared absorption spectroscopy (IR), thermogravimetric and differential thermal analysis (TG/DTA), transmission electron micrographs (TEM), nitrogen adsorption method and ammonia-temperature-programmed desorption (NH3-TPD). The obtained silica-pillared layered niobic acid had a supergallery of 1.78 nm, a large BET surface area of 250 m2 g−1, and a high thermal stability exceeding 973 K.The pillared layered material was also found to be an efficient solid acid catalyst for the vapor-phase Beckmann rearrangement of cyclohexanone oxime. When 1-hexanol was fed with cyclohexanone oxime, this solid catalyst exhibited a 100% conversion of the oxime with a selectivity of ε-caprolactam beyond 85% at a reaction temperature of 613 K and a WHSV of 0.17 h−1 in terms of cyclohexanone oxime, and there was no significant change of the conversion and selectivity within 6 h. |
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Keywords: | Super-microporous structure Silica-pillared layered niobic acid Supergallery Catalytic activity Cyclohexanone oxime Vapor-phase Beckmann rearrangement |
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