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Preparation of Palladium Nanoparticles/polymer Microspheres and Their Catalytic Property

Author: RenShen
Tutor: XieYi；ChenMingQing
School: Jiangnan University
Course: Materials Science
Keywords: The polymer microspheres Situ reduction Pd nanoparticles Pt @ Pd nanoparticles Catalytic activity
CLC: O631.3
Type: Master's thesis
Year: 2011
Downloads: 54
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Abstract


Degradation chain transfer radical polymerization and end-group substitution was prepared by the reaction of poly-N-vinyl acetamide (PNVA) macromonomer by Fourier transform infrared (FT-IR) spectroscopy, UV - visible spectrophotometer (UV-vis ), proton nuclear magnetic resonance (1H-NMR) to characterize its molecular structure, the terminal double bond of the macromonomer prepared PNVA import was 70%. In a mixed medium of the ethanol / water, obtained by synthesis PNVA macromer reactive dispersion stabilizer, with acrylonitrile (AN) and styrene (St) three yuan dispersion copolymerization, prepared PNVA-g-PAN / PSt polymer microspheres. FT-IR and ~ 1H-NMR measurement results show that, the polymer microspheres structure of the PNVA-g-PAN/PSt meet the expected design. Its shape and size was measured by a scanning electron microscope (SEM), the results show: structured polymer microsphere morphology, particle size is more homogeneous, has a convex surface morphology; change the reaction system PNVA amount of polymeric microspheres can be controlled tablets diameter, as PNVA the dosage increased, its particle size becomes small, the particle diameter in the range between 500-1000 nm; change the volume ratio of ethanol / water can influence the stability of the polymer microspheres, when ethanol / water volume ratio ≤ 7/3, polymeric microspheres dispersion stability, good shape; to change the ratio of St and AN, may change the surface morphology of the polymer microspheres, when the decrease in the amount of AN in the convex surface morphology of the polymer microspheres become less obvious. Further to PNVA-g-PAN/PSt polymeric microspheres as a carrier, PdCl2 as a metal source, in a mixed medium of the ethanol / water and ethanol as the reducing agent at 90 ℃ will fully amide group PNVA on ligand the Pd2 situ reduction of Pd nanoparticles, prepared nano Pd / PNVA-g-PAN / PST composite microspheres, and to the same method to obtain Pt @ Pd / PNVA-g-PAN / PSt composite microspheres. Using a transmission electron microscope (TEM), respectively, to characterize the size of the resultant supported Pd and Pt PD nanoparticles, and found that Pd and Pt _AT_ Pd nanoparticles evenly distributed on the surface of the polymer microspheres, the former particle size of about 9 nm, the latter particle size of between 9-22 nm, and X-ray diffraction (XRD) characterization results match. By thermal gravimetric analysis (TG) to characterize the description of the composite microspheres the Pd nanoparticles content can be controlled between 15% -30%. Preliminary studies indicate that the catalytic activity of supported Pd nanoparticles obtained on oxidation of glucose; good catalytic activity of supported Pd and Pt @ Pd nanoparticles cross-coupling reaction of iodobenzene with acrylic acid, the product of the closing The rate can reach 90% or more. And supported Pd nanoparticles able to be recycled, reused five times remain higher catalytic activity for Heck reaction catalyzed by the yield could meet the 88%.

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CLC: > Mathematical sciences and chemical > Chemistry > Polymer chemistry ( polymer ) > Polymer physics and physical chemistry of polymers > The chemical nature of polymers
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