Citation: Hao Yang, Da Shi, Sheng-Fu Ji, Dan-Ni Zhang, Xue-Fei Liu. Nanosized Pd assembled on superparamagnetic core-shell microspheres：Synthesis, characterization and recyclable catalytic properties for the Heck reaction[J]. Chinese Chemical Letters, ;2014, 25(9): 1265-1270. doi: 10.1016/j.cclet.2014.05.003 shu

Nanosized Pd assembled on superparamagnetic core-shell microspheres：Synthesis, characterization and recyclable catalytic properties for the Heck reaction

1.
State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China

Corresponding author: Sheng-Fu Ji,
Received Date: 31 January 2014
Available Online: 29 April 2014
Fund Project: Financial support from the National Natural Science Foundation of China (No. 21173018) is gratefully acknowledged. (No. 21173018)

A series of magnetically recyclable Pd/Fe₃O₄@γ-Al₂O₃ catalysts were synthesized using the superparamagnetic Fe₃O₄@γ-Al₂O₃ core-shell microspheres as the supporter and nano-Pd particles assembled on γ-Al₂O₃ shell as the active catalytic component. The structure of the catalysts was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), N2 adsorption-desorption and vibrating sample magnetometer (VSM). The catalytic activity and the recyclability properties of the catalysts for the Heck coupling reaction with aryl bromides and the olefins were investigated. The results show that the microspheres of the magnetic Pd/Fe₃O₄@γ-Al₂O₃ catalysts were about 400 nm and the nano-Pd particles assembled on γ-Al₂O₃ shell were about 3-4 nm in size. The saturation magnetization (MS) of the magnetic catalysts was sufficiently high to allow magnetic separations. In the Heck coupling reactions, the magnetic Pd/Fe₃O₄@γ-Al₂O₃ catalysts exhibited good catalytic activity and recyclability. With Pd/Fe₃O₄@γ-Al₂O₃ (0.021 mol%) catalyst, the bromobenzene conversion and product yield reached about 96.8% and 91.2%, respectively, at 120℃ and in 14 h. After being recycled for six times, the conversion of bromobenzene and the recovery of the catalyst were about 80% and 90%, respectively. The nano-Pd particles were kept well dispersed in the used Pd/Fe₃O₄@γ-Al₂O₃ catalysts.
- Nano-Pd,
- Superparamagnetic,
- Core-shell,
- Catalyst,
- Heck reaction
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