Green one-step synthesis of catalytically active palladium nanoparticles supported on cellulose nanocrystals

Marzieh Rezayat, Rebecca K. Blundell, Jason E. Camp, Darren A. Walsh, Wim Thielemans

Research output: Contribution to journalArticle

68 Citations (Scopus)

Abstract

Palladium nanoparticles (PdNPs) supported on cellulose nanocrystals (CNXL) were synthesized in a single step from Pd(hexafluoroacetylacetonate)2 (Pd(hfac)2) in subcritical and supercritical carbon dioxide. CNXLs acted as both the reducing agent and support material for the obtained nanoparticles. Dry Pd nanoparticles supported on the cellulose nanocrystals (PdNP@CNXL) were obtained by simply venting the CO2 and were characterized by FT-IR, X-ray photoelectron spectroscopy (XPS), powder X-ray diffraction (XRD), thermogravimetric analysis (TGA), and transmission electron microscopy (TEM). The results show that the Pd nanoparticle diameters varied between 6 and 13 nm with varying pressure (240-2200 psi), reaction time (2-17 h), and weight ratio of the precursor Pd(hfac)2 to CNXL (1-4% w/w). Particles with diameters above 13 nm appeared not to remain attached to the CNXL surface. Reaction conditions also affected the Pd loading in the final PdNP@CNXL composite. Finally, the PdNP@CNXL composites were shown to be effective catalysts for carbon-carbon bond formation in the Mizoroki-Heck cross-coupling reaction, in line with other reports.

Original languageEnglish
Pages (from-to)1241-1250
Number of pages10
JournalACS Sustainable Chemistry and Engineering
Volume2
Issue number5
Early online date1 Apr 2014
DOIs
Publication statusPublished - 5 May 2014
Externally publishedYes

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palladium
Palladium
Cellulose
Nanocrystals
cellulose
Nanoparticles
Carbon
venting
Reducing Agents
carbon
Composite materials
Reducing agents
nanoparticle
Carbon Dioxide
X ray powder diffraction
X-ray spectroscopy
Thermogravimetric analysis
transmission electron microscopy
Carbon dioxide
X ray photoelectron spectroscopy

Cite this

Rezayat, Marzieh ; Blundell, Rebecca K. ; Camp, Jason E. ; Walsh, Darren A. ; Thielemans, Wim. / Green one-step synthesis of catalytically active palladium nanoparticles supported on cellulose nanocrystals. In: ACS Sustainable Chemistry and Engineering. 2014 ; Vol. 2, No. 5. pp. 1241-1250.
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abstract = "Palladium nanoparticles (PdNPs) supported on cellulose nanocrystals (CNXL) were synthesized in a single step from Pd(hexafluoroacetylacetonate)2 (Pd(hfac)2) in subcritical and supercritical carbon dioxide. CNXLs acted as both the reducing agent and support material for the obtained nanoparticles. Dry Pd nanoparticles supported on the cellulose nanocrystals (PdNP@CNXL) were obtained by simply venting the CO2 and were characterized by FT-IR, X-ray photoelectron spectroscopy (XPS), powder X-ray diffraction (XRD), thermogravimetric analysis (TGA), and transmission electron microscopy (TEM). The results show that the Pd nanoparticle diameters varied between 6 and 13 nm with varying pressure (240-2200 psi), reaction time (2-17 h), and weight ratio of the precursor Pd(hfac)2 to CNXL (1-4{\%} w/w). Particles with diameters above 13 nm appeared not to remain attached to the CNXL surface. Reaction conditions also affected the Pd loading in the final PdNP@CNXL composite. Finally, the PdNP@CNXL composites were shown to be effective catalysts for carbon-carbon bond formation in the Mizoroki-Heck cross-coupling reaction, in line with other reports.",
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Green one-step synthesis of catalytically active palladium nanoparticles supported on cellulose nanocrystals. / Rezayat, Marzieh; Blundell, Rebecca K.; Camp, Jason E.; Walsh, Darren A.; Thielemans, Wim.

In: ACS Sustainable Chemistry and Engineering, Vol. 2, No. 5, 05.05.2014, p. 1241-1250.

Research output: Contribution to journalArticle

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T1 - Green one-step synthesis of catalytically active palladium nanoparticles supported on cellulose nanocrystals

AU - Rezayat, Marzieh

AU - Blundell, Rebecca K.

AU - Camp, Jason E.

AU - Walsh, Darren A.

AU - Thielemans, Wim

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N2 - Palladium nanoparticles (PdNPs) supported on cellulose nanocrystals (CNXL) were synthesized in a single step from Pd(hexafluoroacetylacetonate)2 (Pd(hfac)2) in subcritical and supercritical carbon dioxide. CNXLs acted as both the reducing agent and support material for the obtained nanoparticles. Dry Pd nanoparticles supported on the cellulose nanocrystals (PdNP@CNXL) were obtained by simply venting the CO2 and were characterized by FT-IR, X-ray photoelectron spectroscopy (XPS), powder X-ray diffraction (XRD), thermogravimetric analysis (TGA), and transmission electron microscopy (TEM). The results show that the Pd nanoparticle diameters varied between 6 and 13 nm with varying pressure (240-2200 psi), reaction time (2-17 h), and weight ratio of the precursor Pd(hfac)2 to CNXL (1-4% w/w). Particles with diameters above 13 nm appeared not to remain attached to the CNXL surface. Reaction conditions also affected the Pd loading in the final PdNP@CNXL composite. Finally, the PdNP@CNXL composites were shown to be effective catalysts for carbon-carbon bond formation in the Mizoroki-Heck cross-coupling reaction, in line with other reports.

AB - Palladium nanoparticles (PdNPs) supported on cellulose nanocrystals (CNXL) were synthesized in a single step from Pd(hexafluoroacetylacetonate)2 (Pd(hfac)2) in subcritical and supercritical carbon dioxide. CNXLs acted as both the reducing agent and support material for the obtained nanoparticles. Dry Pd nanoparticles supported on the cellulose nanocrystals (PdNP@CNXL) were obtained by simply venting the CO2 and were characterized by FT-IR, X-ray photoelectron spectroscopy (XPS), powder X-ray diffraction (XRD), thermogravimetric analysis (TGA), and transmission electron microscopy (TEM). The results show that the Pd nanoparticle diameters varied between 6 and 13 nm with varying pressure (240-2200 psi), reaction time (2-17 h), and weight ratio of the precursor Pd(hfac)2 to CNXL (1-4% w/w). Particles with diameters above 13 nm appeared not to remain attached to the CNXL surface. Reaction conditions also affected the Pd loading in the final PdNP@CNXL composite. Finally, the PdNP@CNXL composites were shown to be effective catalysts for carbon-carbon bond formation in the Mizoroki-Heck cross-coupling reaction, in line with other reports.

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