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Issue 3, 2011
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Synthesis of Pd nanocrystals in phosphonium ionic liquids without any external reducing agents

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Abstract

Trihexyl(tetradecyl)phosphonium ionic liquids (ILs) are found to support the formation of Pd(0) nanoparticles without the addition of reducing agents such as NaBH4. The resulting particles are highly crystalline and have been characterized by a range of techniques including TEM and XRD. Their sizes are in the range 7 ± 2 nm. The particle formation process is highly dependent on the anion of the IL with no nanoparticles observed when the chloride derivative was used. Particle shape could be controlled through varying the anion of the IL and the Pd(II) precursor used. Palladium chloride reagents gave truncated octahedron shaped particles in trihexyl(tetradecyl)phosphonium dodecylbenzenesulfonate, whereas palladium acetate under the same conditions afforded a mixture of shapes including triangular plates. We propose that the presence of chloride anions in the reaction mixtures led to oxidative etching of the particles and that this process can be reduced in the presence of certain anion partners in the IL including bis(2,4,4-trimethylpentyl)phosphinate. Two possible reduction mechanisms based on reactions of the phosphonium cation are suggested for the formation of the Pd(0) species. The resulting nanoparticles are effective in catalyzing the Suzuki reaction of 4-bromotoluene and benzene boronic acid.

Graphical abstract: Synthesis of Pd nanocrystals in phosphonium ionic liquids without any external reducing agents

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Publication details

The article was received on 25 Nov 2010, accepted on 25 Jan 2011 and first published on 15 Feb 2011


Article type: Paper
DOI: 10.1039/C0GC00851F
Green Chem., 2011,13, 681-686

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    Synthesis of Pd nanocrystals in phosphonium ionic liquids without any external reducing agents

    H. A. Kalviri and F. M. Kerton, Green Chem., 2011, 13, 681
    DOI: 10.1039/C0GC00851F

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