催化学报 ›› 2010, Vol. 31 ›› Issue (7): 827-832.

• 研究论文 • 上一篇    下一篇

SBA-15 固载离子液体功能化脯氨酸的制备及其催化 Knoevenagel 缩合反应

沈加春, 郭建平, 孙艳美, 唐斌艳, 陈小花, 尹笃林   

  1. 湖南师范大学化学化工学院, 资源精细化与先进材料湖南省高校重点实验室, 湖南长沙 410081
  • 收稿日期:2010-07-25 出版日期:2010-07-25 发布日期:2010-07-25

Knoevenagel Condensation Catalyzed by Immobilized Ionic Liquids-Proline on SBA-15

SHEN Jiachun, GUO Jianping*, SUN Yanmei, TANG Binyan, CHEN Xiaohua, YIN Dulin*   

  1. College of Chemistry and Chemical Engineering, Key Laboratory of Resources Fine-Processing and Advanced Materials of Universities of Hunan Province, Hunan Normal University, Changsha 410081, Hunan, China
  • Received:2010-07-25 Online:2010-07-25 Published:2010-07-25

摘要: 以 L-脯氨酸为原料合成了离子液体功能化脯氨酸前驱体 (IL-Pro), 并将其固载到 SBA-15 介孔分子筛上, 制得 IL-Pro/SBA-15 催化剂. 用红外光谱、热重、N2 吸附-脱附、X 射线衍射和透射电镜等手段表征了 IL-Pro/SBA-15 催化剂, 并考察了该催化剂在 Knoevenagel 缩合反应中的催化性能. 结果表明, 固载离子液体功能化脯氨酸没有破坏 SBA-15 的有序介孔结构, 但孔体积、孔径和比面表积有所下降; IL-Pro/SBA-15 的失重峰在 250~360 oC (峰值为 310 oC). 在以苯甲醛和丙二腈为底物的 Knoevenagel 反应中, IL-Pro/SBA-15 催化剂表现出较高的活性, 缩合产物收率高达 94%; 经简单分离后催化剂可重复使用 7 次以上而活性基本保持不变.

关键词: L-脯氨酸, 功能化离子液体, SBA-15 分子筛, 负载型催化剂, Knoevenagel 反应, 苯甲醛, 丙二腈

Abstract: The IL-Pro/SBA-15 catalyst was prepared using SBA-15 as the support to immobilize ionic liquid proline, which was synthesized from L-proline. The IL-Pro/SBA-15 catalyst was characterized by FT-IR spectroscopy, thermal gravity analysis-derivative thermogravimetry, N2 adsorption-desorption, X-ray diffraction, and transmission electron microscopy, and the catalytic performance of the catalyst was measured for Knoevenagel reaction. The results showed that the mesoporous structure of SBA-15 was not affected by immobilization; however, the pore diameter, pore volume, and surface area were decreased. Mass loss of the supported ionic liquid occurred at 250–360 oC, and reached the maximum at 310 oC. The Pro-IL/SBA-15 catalyst had higher activity in Knoevenagel reaction of benzaldehyde with malononitrile and gave the corresponding product yield of 94%. The supported catalyst could be easily separated from the reaction system and reused at least seven times without loss of catalytic activity.

Key words: L-proline, functionalized ionic liquid, SBA-15 zeolite, supported catalyst, Knoevenagel reaction, benzaldehyde, malononitrile