催化学报 ›› 2015, Vol. 36 ›› Issue (11): 1852-1860.DOI: 10.1016/S1872-2067(15)60968-8

• 论文 • 上一篇    下一篇

中孔MCM-41锚合Zr(IV)-salen催化剂制备及用于硫化物氧化制亚砜和Knoevenagel缩合反应

Maryam Hajjamia, Farshid Ghorbanib, Sedighe Rahimipanaha, Safoora Roshania   

  1. a 伊拉姆大学理学院化学系, 伊拉姆, 伊朗;
    b 库尔德斯坦大学自然资源学院环境系, 萨南达杰, 伊朗
  • 收稿日期:2015-06-19 修回日期:2015-09-06 出版日期:2015-11-02 发布日期:2015-11-02
  • 通讯作者: Maryam Hajjami. 电话/传真: +98-8412227022; 电子信箱: mhajjami@yahoo.com, m.hajjami@ilam.ac.ir

Efficient preparation of Zr(IV)-salen grafted mesoporous MCM-41 catalyst for chemoselective oxidation of sulfides to sulfoxides and Knoevenagel condensation reactions

Maryam Hajjamia, Farshid Ghorbanib, Sedighe Rahimipanaha, Safoora Roshania   

  1. a Department of Chemistry, Faculty of Science, Ilam University, P.O. Box 69315516, Ilam, Iran;
    b Department of Environment, Faculty of Natural Resource, University of Kurdistan, 66177-15177 Sanandaj, Iran
  • Received:2015-06-19 Revised:2015-09-06 Online:2015-11-02 Published:2015-11-02

摘要:

通过NH2-MCM-41与水杨醛反应得到席夫碱配体, 然后加入八水氧氯化锆形成络合物, 制得Zr(IV)-salen-MCM-41催化剂. 采用X射线衍射、N2吸附-脱附、热重、红外光谱、电感耦合等离子体发射光谱和能量散射谱等分析手段对催化剂结构进行了表征. 在含有该催化剂的体系中进行了硫化物选择氧化为亚砜以及醛与丙二腈和氰乙酸乙酯的Knoveonagel缩合反应, 并考察了催化剂的循环使用性能.

关键词: 锆(IV)-salen-MCM41, 中孔, 亚砜, Knoveonagel缩合, 硫化物

Abstract:

Zr(IV)-salen-MCM-41 was prepared by reaction of NH2-MCM-41 with salicylaldehyde to afford Schiff base ligands. Thereafter, ZrOCl2·8H2O was reacted with the Schiff base ligands for complex formation. The structural properties of the synthesized materials were investigated by a number of analytical techniques including X-ray diffraction, N2 sorption-desorption, thermogravimetric analysis, Fourier transform infrared spectroscopy, inductively coupled plasma atomic emission spectroscpopy, and energy dispersive X-ray spectroscopy. Catalytic studies of the mesoporous materials functionalized with Zr(IV)-Schiff base complexes were investigated and extended to selective oxidation of sulfides to sulfoxides and the Knoevenagel condensation reactions of aldehydes with malononitriles and ethyl cyanoacetate. Additionally, catalyst recycling of the Zr-salen-MCM-41 materials was also studied.

Key words: Zr(IV)-salen-MCM-41, Mesoporous material, Sulfoxide, Knoveonagel condensation, Sulfide