催化学报

催化学报 ›› 2011, Vol. 32 ›› Issue (1): 144-148.DOI: 10.3724/SP.J.1088.2010.00744

• 研究论文 • 上一篇    下一篇

CoO/SiO2-Al2O3 催化剂上苯胺和 1,6-己二醇气相高效合成 1-苯基氮杂环庚烷

刘兴海, 朱海艳, 石雷, 孙琪   

  1. 辽宁师范大学化学化工学院功能材料化学研究所, 辽宁大连 116029
  • 收稿日期:2010-07-30 修回日期:2010-10-04 出版日期:2011-01-13 发布日期:2014-05-22

Efficient Vapor-Phase Synthesis of 1-Phenylazepane from Aniline and 1,6-Hexanediol over CoO/SiO2-Al2O3 Catalyst

LIU Xinghai, ZHU Haiyan, SHI Lei*, SUN Qi   

  1. Institute of Chemistry for Functionalized Materials, Faculty of Chemistry and Chemical Engineering, Liaoning Normal University, Dalian 116029, Liaoning, China
  • Received:2010-07-30 Revised:2010-10-04 Online:2011-01-13 Published:2014-05-22

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摘要： 研究了 CoO/SiO2-Al2O3 催化剂上苯胺和 1,6-己二醇气相催化合成 1-苯基氮杂环庚烷的反应, 并采用 N2 吸附-脱附、X 射线衍射、H2 程序升温还原和 NH3 程序升温脱附技术对催化剂进行表征. 结果表明, CoO/SiO2-Al2O3 催化剂表现出较高的活性和选择性. 当 CoO 担载量为 0.3 mmol/g 时, 催化剂前体在 700 °C (2.8 °C/min) 下焙烧 4 h 以及在 325 °C 下 50% H2-50% N2 (60 ml/min) 混合气中原位还原 2 h, 产物收率达到 80%. 催化剂的比表面积大、活性组分分散度高以及酸性较弱时有利于目标产物的生成.

关键词: 氧化钴, 二氧化硅, 氧化铝, 负载型催化剂, 1-苯基氮杂环庚烷, 苯胺, 1,6-己二醇

Abstract: Vapor-phase catalytic synthesis of 1-phenylazepane from aniline and 1,6-hexanediol over CoO/SiO2-Al2O3 catalyst was investigated and the catalyst samples were characterized by N2 adsorption-desorption, X-ray diffraction, H2 temperature-programmed reduction, and NH3 temperature-programmed desorption. The results indicated that the CoO/SiO2-Al2O3 catalyst showed higher activity and selectivity. When CoO loading was 0.3 mmol/g and the catalyst precursor was calcined at 700 °C (2.8 °C/min) for 4 h followed by reduction in situ at 325 °C for 2 h in the mixture gas of 50% H2-50% N2 (60 ml/min) before reaction, the yield of 1-phenylazepane could be up to 80%. The catalyst with larger specific surface area, higher dispersion of the active component, and weaker acidity favored the synthesis of the target product.

Key words: cobaltous oxide, silica, alumina, supported catalyst, 1-phenylazepane, aniline, 1,6-hexanediol