化学学报 ›› 2005, Vol. 63 ›› Issue (16): 1469-1473.    下一篇

研究论文

胺基化树脂负载Pd(0)对Heck反应催化性能的研究

杨元法*1,曾朝霞1,罗孟飞1,李巧玲2,黄朝表1   

  1. (1浙江师范大学物理化学研究所 浙江省固体表面反应化学重点实验室 金华 321004)
    (2浙江大学分析测试中心 杭州 310028)
  • 投稿日期:2005-03-14 修回日期:2005-07-21 发布日期:2010-12-10
  • 通讯作者: 杨元法

Aminated Functional Resin Supported Pd(0) Catalysts for Heck ReactionAA

YANG Yuan-Fa*1, ZENG Chao-Xia1, LUO Meng-Fei a, LI Qiao-Ling2, HUANG Chao-Biao1   

  1. (1 Institute of Physical Chemistry, Zhejiang Key Laboratory for Reactive Chemistry on Solid Surfaces, Zhejiang Normal University, Jinhua 321004)
    (2 Center of Analysis and Test, Zhejiang University, Hangzhou 310028)
  • Received:2005-03-14 Revised:2005-07-21 Published:2010-12-10
  • Contact: YANG Yuan-Fa

将氯球用胺化剂、乙二胺、胍进行胺化后负载氯化钯, 在乙醇溶液中用硼氢化钾还原, 制备了含胺功能基树脂负载钯(0)的催化剂; 研究了催化剂对含各种取代基碘代苯与丙烯酸的Heck芳基化反应催化性能. 结果表明, 该类催化剂具有良好的催化活性和重复使用性能, 其中用乙二胺功能化树脂负载的Pd(0)催化剂在90 ℃重复使用17次时能保持良好的催化活性. 催化剂反应前后的SEM形貌图和过滤液的活性试验表明催化剂活性组分Pd(0)在反应中有沥取(leaching)现象.

关键词: 胺化树脂, 负载型钯催化剂, Heck反应, 循环使用

Aminated resin supported Pd(0) catalysts were prepared by the process: reaction of chloromethyl polystyrene resins with aminating agent or ethylenediamine or guanidine and reduction of palladium chloride immobilized on functional resins by KBH4 in anhydrous alcohol. These catalysts were found to have good activity and reusability in the Heck vinylation of aryl iodides and acrylate, among which the ethylenediamine modified resin supported Pd(0) catalyst kept a high activity at the 17th run at 90 ℃. The SEM image of the catalysts before and after Heck reaction and the filtration/leaching test indicated that the active species Pd(0) underwent leaching in Heck reaction.

Key words: aminated resin, supported Pd(0) catalyst, Heck reaction, recycling