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Study on the Synthesis of Solvent-Stabilized Palladium Nanoparticles and Their Catalytic Activity

Author: TongXia
Tutor: HuangTao；LiuHanFan
School: Central South University for Nationalities
Course: Organic Chemistry
Keywords: Palladium Palladium acetate Nanoparticles Methyl isobutyl ketone Glycol N-butanol Microwave Self-assembly gamma - Al2O3 Catalytic hydrogenation
CLC: TB383.1
Type: Master's thesis
Year: 2009
Downloads: 63
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Abstract


Metal nanoparticles attracted much attention because of its widely used in the field of catalysis, optics, microelectronics, magnetic, optical sensing, information storage, biological markers. Metal nano-materials is closely related to its particle size, morphology, composition and structure. Pd as an important platinum group elements has been attracting widespread interest. Pd is widely used as a catalyst, is closely related to its applications in catalysis, and its significant hydrogen-absorbing capacity. In the last decade, people preparing various surfactant or polymer compound stable morphology of Pd nanoparticles. Such a protecting agent parcel catalytic metal nanoparticles relatively poor performance. Therefore, this article explore Controlled Synthesis of Pd nanoparticles protected by surfactant or a polymer stabilizer. Microwave thermal decomposition method, Pd (OAc) 2 as the precursor, methyl isobutyl ketone (MIBK) as the solvent, in the presence of a small amount of butanol, KOH and water was prepared by the average particle Take approximately 4.48 ± 1.18 nm, palladium nanoparticles, and the UV - visible spectroscopy (UV-vis), transmission electron microscopy (TEM), a powder X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) The products were characterized. By changing the concentration of the precursor in the reaction system of Pd (OAc) 2, Pd (OAc) 2 / KOH molar ratio of n-butanol and can effectively control the amount of water, the particles have an average particle size and dispersion degrees. MIBK as the solvent, in the presence of a small amount of ethylene glycol (EG) (or butanol) and the amount of KOH, Pd (OAc) 2 the microwave irradiation 60sec thermal decomposition uniform particle size, degree of dispersion the solvent stability of the urchin-like palladium nanoparticles. XRD analysis showed that the urchin-like palladium nanoparticles are prepared for the fcc structure is smaller by many average particle diameter of approximately 2.4 nm Pd nanoparticles self-assembled secondary structure, consistent with the results of TEM observation. The sea urchin-like self-assembly of palladium nanoparticles can be stably stored at low temperatures, placed a few months does not change. Self-assembled palladium nano-particles have an average particle diameter of the obtained EG was added a smaller, more uniform size dispersity better, and more protrusions from the surface of the particles is greater than the surface area compared with the Add-butanol system. Each of cyclohexene and styrene as a substrate to explore the gamma-Al the 2 O 3 load in the different structure of Pd nanoparticles hydrogenation activity. The results showed that the solvent stability of the small particle size PD (n-butanol) / gamma-Al the best 2 the O 3 of catalytic hydrogenation performance, which is, because of its particle size more small, large surface area, the the no protective agent package can take advantage of the active center; followed by gamma-Al 2 O 3 load sea urchin-like palladium nanoparticles (Pd (EG) / γ-Al 2 O 3 ); the no load sea urchin-like palladium nanoparticles Pd (EG) and PVP protection agent palladium nanoparticles (Pd ( EG) / PVP / gamma-the Al 2 O 3 ) poor catalytic performance.

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