催化学报

催化学报 ›› 2014, Vol. 35 ›› Issue (6): 929-936.DOI: 10.1016/S1872-2067(14)60125-X

• 研究论文 • 上一篇    下一篇

Esterification of levulinic acid into ethyl levulinate catalysed by sulfonated hydrothermal carbons

Filoklis D. Pileidis, Maham Tabassum, Sam Coutts, Maria-Magdalena Titirici   

  1. Queen Mary University of London, School of Engineering and Materials Science, Mile End Road, E1 4NS, London, United Kingdom
  • 收稿日期:2014-04-11 修回日期:2014-04-30 出版日期:2014-05-30 发布日期:2014-06-03
  • 通讯作者: Maria-Magdalena Titirici

Esterification of levulinic acid into ethyl levulinate catalysed by sulfonated hydrothermal carbons

Filoklis D. Pileidis, Maham Tabassum, Sam Coutts, Maria-Magdalena Titirici   

  1. Queen Mary University of London, School of Engineering and Materials Science, Mile End Road, E1 4NS, London, United Kingdom
  • Received:2014-04-11 Revised:2014-04-30 Online:2014-05-30 Published:2014-06-03

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摘要：

The synthesis of carbon-based, heterogeneous sulphonic catalysts for the production of levulinate esters. Hydrothermal treatment at moderated temperatures was employed to generate highly functional carbonaceous materials, referred to as hydrothermal carbons (HTCs), from both glucose, cellulose and rye straw. The products were sulfonated to generate solid acid-catalysts. Characterisation of the as-synthesised materials as well as catalyst activity tests were performed. SEM images indicate the micrometre-sized particles present in both HTCs were largely unaffected by sulfonation, although cellulose-derived HTC displayed signs of inadequate hydrolysis. FT-IR spectroscopy and elemental analysis confirmed successful incorporation of sulphonic groups. 13C solid state NMR, in addition to TGA, elucidated the carbons' structural composition and supported the commonly-proposed hydrothermal carbonisation mechanism. Finally, the catalysts were tested via levulinic acid-ethanol esterification and gave high conversion and ester-selectivities (> 90%).

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关键词: Sulfonated hydrothermal carbons, Glucose, Cellulose, Rye straw, Esterification, Levulinic acid, Ethyl levulinate

Abstract:

The synthesis of carbon-based, heterogeneous sulphonic catalysts for the production of levulinate esters. Hydrothermal treatment at moderated temperatures was employed to generate highly functional carbonaceous materials, referred to as hydrothermal carbons (HTCs), from both glucose, cellulose and rye straw. The products were sulfonated to generate solid acid-catalysts. Characterisation of the as-synthesised materials as well as catalyst activity tests were performed. SEM images indicate the micrometre-sized particles present in both HTCs were largely unaffected by sulfonation, although cellulose-derived HTC displayed signs of inadequate hydrolysis. FT-IR spectroscopy and elemental analysis confirmed successful incorporation of sulphonic groups. 13C solid state NMR, in addition to TGA, elucidated the carbons' structural composition and supported the commonly-proposed hydrothermal carbonisation mechanism. Finally, the catalysts were tested via levulinic acid-ethanol esterification and gave high conversion and ester-selectivities (> 90%).

Key words: Sulfonated hydrothermal carbons, Glucose, Cellulose, Rye straw, Esterification, Levulinic acid, Ethyl levulinate