催化学报 ›› 2015, Vol. 36 ›› Issue (5): 771-777.DOI: 10.1016/S1872-2067(14)60282-5

• 论文 • 上一篇    下一篇

Preparation and characterization of HypoGel-supported Pd nanocatalysts for Suzuki reaction under mild conditions

Kin Hong Liewa, Wan Zurina Samada, Norazzizi Nordina, Poh Lee Loha, Joon Ching Juanb, Mohd Ambar Yarmoa, Badrul Hisham Yahayac, Rahimi M. Yusopa,c   

  1. a School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 UKM, Bangi, Selangor Darul Ehsan, Malaysia;
    b Nanotechnology & Catalysis Research Centre (NANOCAT), University of Malaya, 50603 Kuala Lumpur, Malaysia;
    c Kluster Perubatan Regeneratif, Institut Perubatan dan Pergigian Termaju, Universiti Sains Malaysia, 13200 Bertam Kepala Batas, Pulau Pinang, Malaysia
  • 收稿日期:2014-12-19 修回日期:2015-01-07 出版日期:2015-04-17 发布日期:2015-04-17
  • 通讯作者: Rahimi M. Yusop
  • 基金资助:

    This work was supported by the Ministry of Higher Education Malaysia (FRGS/1/2012/ST01/UKM/02/1) and Research Grant from UKM (IP-2014-070 and LAUREATE-2013-002).

Preparation and characterization of HypoGel-supported Pd nanocatalysts for Suzuki reaction under mild conditions

Kin Hong Liewa, Wan Zurina Samada, Norazzizi Nordina, Poh Lee Loha, Joon Ching Juanb, Mohd Ambar Yarmoa, Badrul Hisham Yahayac, Rahimi M. Yusopa,c   

  1. a School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 UKM, Bangi, Selangor Darul Ehsan, Malaysia;
    b Nanotechnology & Catalysis Research Centre (NANOCAT), University of Malaya, 50603 Kuala Lumpur, Malaysia;
    c Kluster Perubatan Regeneratif, Institut Perubatan dan Pergigian Termaju, Universiti Sains Malaysia, 13200 Bertam Kepala Batas, Pulau Pinang, Malaysia
  • Received:2014-12-19 Revised:2015-01-07 Online:2015-04-17 Published:2015-04-17
  • Contact: Rahimi M. Yusop
  • Supported by:

    This work was supported by the Ministry of Higher Education Malaysia (FRGS/1/2012/ST01/UKM/02/1) and Research Grant from UKM (IP-2014-070 and LAUREATE-2013-002).

摘要:

A new heterogeneous catalyst composed of Pd nanoparticles immobilized within a HypoGel resin has been prepared in the absence of any ligands using an extensive cross-linking method. This newly developed nanocatalyst was characterized by N2 adsorption-desorption, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), Fourier transform infrared spectroscopy and inductively coupled plasma-mass spectrometer (ICP-MS) techniques. TEM and XRD results revealed that the Pd nanoparticles were well dispersed with diameters in the range of 4-12 nm, and an average size of about 8 nm. The cross-linked Pd catalyst demonstrated excellent catalytic activity towards the synthesis of a series of biaryl compounds by the reaction of various aryl halides (e.g., bromides andiodides) with phenylboronic acid in the presence of tetrabutylammonium bromide. ICP-MS analysis indicated that there was only 0.25% weight loss of Pd (0.55 ± 0.02 ppm) from the supported catalyst after the first cycle reaction. Furthermore, the catalyst showed excellent reusability (up to five uses) with consistently high levels of catalytic activity following its recovery by filtration.

关键词: HypoGel, Palladium, Heterogeneous catalyst, Suzuki reaction, Water

Abstract:

A new heterogeneous catalyst composed of Pd nanoparticles immobilized within a HypoGel resin has been prepared in the absence of any ligands using an extensive cross-linking method. This newly developed nanocatalyst was characterized by N2 adsorption-desorption, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), Fourier transform infrared spectroscopy and inductively coupled plasma-mass spectrometer (ICP-MS) techniques. TEM and XRD results revealed that the Pd nanoparticles were well dispersed with diameters in the range of 4-12 nm, and an average size of about 8 nm. The cross-linked Pd catalyst demonstrated excellent catalytic activity towards the synthesis of a series of biaryl compounds by the reaction of various aryl halides (e.g., bromides andiodides) with phenylboronic acid in the presence of tetrabutylammonium bromide. ICP-MS analysis indicated that there was only 0.25% weight loss of Pd (0.55 ± 0.02 ppm) from the supported catalyst after the first cycle reaction. Furthermore, the catalyst showed excellent reusability (up to five uses) with consistently high levels of catalytic activity following its recovery by filtration.

Key words: HypoGel, Palladium, Heterogeneous catalyst, Suzuki reaction, Water