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Sustainable Catalysis: Rational Pd Loading on MIL‐101Cr‐NH 2 for More Efficient and Recyclable Suzuki–Miyaura Reactions
Author(s) -
Pascanu Vlad,
Yao Qingxia,
Bermejo Gómez Antonio,
Gustafsson Mikaela,
Yun Yifeng,
Wan Wei,
Samain Louise,
Zou Xiaodong,
MartínMatute Belén
Publication year - 2013
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.201302621
Subject(s) - palladium , catalysis , thermogravimetric analysis , fourier transform infrared spectroscopy , materials science , nanoparticle , scanning electron microscope , nuclear chemistry , sorption , transmission electron microscopy , chemical engineering , inorganic chemistry , chemistry , nanotechnology , organic chemistry , composite material , adsorption , engineering
Palladium nanoparticles have been immobilized into an amino‐functionalized metal–organic framework (MOF), MIL‐101Cr‐NH 2 , to form Pd@MIL‐101Cr‐NH 2 . Four materials with different loadings of palladium have been prepared (denoted as 4‐, 8‐, 12‐, and 16 wt %Pd@MIL‐101Cr‐NH 2 ). The effects of catalyst loading and the size and distribution of the Pd nanoparticles on the catalytic performance have been studied. The catalysts were characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier‐transform infrared (FTIR) spectroscopy, powder X‐ray diffraction (PXRD), N 2 ‐sorption isotherms, elemental analysis, and thermogravimetric analysis (TGA). To better characterize the palladium nanoparticles and their distribution in MIL‐101Cr‐NH 2 , electron tomography was employed to reconstruct the 3D volume of 8 wt %Pd@MIL‐101Cr‐NH 2 particles. The pair distribution functions (PDFs) of the samples were extracted from total scattering experiments using high‐energy X‐rays (60 keV). The catalytic activity of the four MOF materials with different loadings of palladium nanoparticles was studied in the Suzuki–Miyaura cross‐coupling reaction. The best catalytic performance was obtained with the MOF that contained 8 wt % palladium nanoparticles. The metallic palladium nanoparticles were homogeneously distributed, with an average size of 2.6 nm. Excellent yields were obtained for a wide scope of substrates under remarkably mild conditions (water, aerobic conditions, room temperature, catalyst loading as low as 0.15 mol %). The material can be recycled at least 10 times without alteration of its catalytic properties.