More Benign Synthesis of Palladium Nanoparticles in Dimethyl Sulfoxide and Their Extraction into an Organic Phase

Abstract

We present the successful synthesis and stabilization of 3.5 nm Pd nanoparticles (standard deviation of 0.49 nm) within dimethyl sulfoxide (DMSO) via fast, homogeneous reduction of a Pd salt using NaBH 4 in the absence of traditional capping ligands. These Pd nanoparticles were found to be extremely stable and did not exhibit precipitation and/or agglomeration within the DMSO solvent even after more than 9 months. Moreover, these Pd nanoparticles were conveniently separated from the DMSO solvent medium via vacuum freeze drying by taking advantage of the high freezing point of DMSO. We have also successfully extracted the Pd nanoparticles from the DMSO phase into an organic phase (i.e., hexane), thereby providing a facile and efficient means for the generation of organic phase dispersible metal nanoparticles with complete recycle of the DMSO solvent.

Capping Agent Effect on Pd-Supported Nanoparticles in the Hydrogenation of Furfural

“…A shift at 286 nm (blue curve, Figure S1c) after adding PDDA to the Pd precursor, suggests a possible ligand-to-metal charge transfer interaction between PDDA and [PdCl 4 ] 2-, as already evidenced in the case of Au [31]. The disappearance of the peaks related to Pd 2+ and the observed scattering suggest the complete reduction to Pd 0 and the formation of metal nanoparticles [32,33].…”

Solid State Morphology and Size Tuning of Nanostructured Platinum Using Macromolecular Complexes

“…the (111) , (200) , (200) and (311) planes [15]. Although several solution preparation of Pt° nanoparticles have been reported [14][15][16][17][18][19][20][21][22][23][24][25][26][27] no solid state methods for to prepare Pt° nanoparticles are available. The first way, solution methods, in spite of that to allow the size and morphology control, their incorporation to a solid state device could be not easy.…”

“…General chemical methods of nanoparticles preparation depart from a Pt precursor, usually a salt of Pt (II) or Pt (IV) (e.g. H 2 PtCl 4 or H 2 PtCl 6 ) in presence of a reducer such as an alcohol, NaBH 4 or H 2 and polymer stabilizers (also CO or other ligand) [16][17][18][19][20]. The use of Pt(acac) 2 or Pt(dba) 2 as a metallic forerunner with various reducers and stabilizers has also been reported [21][22][23][24].…”

Morphological study of microwave-assisted facile synthesis of gold nanoflowers/nanoparticles in aqueous medium and their catalytic application for reduction of p-nitrophenol to p-aminophenol

“…Guin et al 21 carried out synthesis of iron oxide nanoparticles in DMSO by thermal decomposition. Liu et al 22 have prepared Pd nanoparticles using DMSO as solvent via reduction method. Rodriguez-Gattorno et al 23 have demonstrated the synthesis of silver nanoparticles by spontaneous reduction of silver 2-ethylhexanoate in presence of DMSO.…”