Effect of microwave heating on the synthesis of rhodium nanoparticles in ionic liquids

García, Stephany; Buckley, Jannise J.; Brutchey, Richard L.; Humphrey, Simon M.

doi:10.1016/j.ica.2014.07.035

Cited by 7 publications

(4 citation statements)

References 36 publications

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“…TEM analysis of the Pt nanoparticles synthesized in ODE returns an average particle size of 1.7 ± 0.3 nm ( N = 300), and the nanoparticles were more agglomerated than what was observed for IL-synthesized particles (Figure S2). This can be attributed to the fact that ILs can stabilize colloidal nanoparticles (vide supra), , reducing agglomeration. Indeed, while the FT-IR spectra of Pt nanoparticles synthesized in ODE and IL both exhibit characteristic bands from PVP, the spectrum of the IL-synthesized particles also exhibits diagnostic bands for both the BMIM cation and the NTf 2 anion (Figure S4).…”

Section: Resultsmentioning

confidence: 99%

“…Ionic liquids are molten salts, usually comprised of an organic cation and an inorganic or organic anion, that melt below 100 °C . There has been interest in utilizing ILs as alternatives to VOC solvents because of their many advantages over traditional organic solvents, namely, being non-flammable, having negligible vapor pressures (∼10 –10 Pa at 25 °C), possessing high thermal stability, and having the potential to be more easily recovered and recycled. , The vast number of combinations of anions and cations that can be generated allows tailoring of IL properties, such as solubility, density, hydrophobicity, and viscosity. , Finally, ILs are known to be rather chemically inert and display unique liquid–liquid phase separation behaviors, which allow for both facile solvent recycling and simple extractive purification …”

Section: Introductionmentioning

confidence: 99%

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Techno-Economic Analysis of Recycled Ionic Liquid Solvent Used in a Model Colloidal Platinum Nanoparticle Synthesis

Karadaghi

Malmstadt

Allsburg

et al. 2020

ACS Sustainable Chem. Eng.

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Ionic liquids have garnered significant attention over the past 20 years as alternatives to conventional volatile organic solvents because they are non-flammable, have negligible vapor pressures, possess high thermal and chemical stabilities, and can potentially be recycled. A more recent use of ionic liquids is their application as a solvent in the synthesis of colloidal inorganic nanoparticles; however, a major challenge in the adoption of ionic liquids is that they are generally more expensive than their traditional organic solvent counterparts. Herein, we provide insight into how recycling an ionic liquid solvent affects the product characteristics in a model colloidal platinum nanoparticle synthesis, the structure of the ionic liquid through each recycle, and the overall cost of nanoparticle fabrication using a techno-economic analysis. Using a standard ionic liquid, 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide (BMIM-NTf2), as the solvent for a Pt nanoparticle synthesis, we demonstrate that the ionic liquid can be recovered and reused through multiple successive reactions following the initial reaction with virgin, or as-purchased, ionic liquid. The use of recycled ionic liquid does not cause any degradation in the product quality or change in nanoparticle morphology. Techno-economic analysis of this synthesis method revealed that, through ionic liquid recycling, nanoparticle preparation using BMIM-NTf2 can achieve a cost that is not only competitive but also potentially lower than that of the conventional organic solvent, 1-octadecene.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Techno-Economic Analysis of Recycled Ionic Liquid Solvent Used in a Model Colloidal Platinum Nanoparticle Synthesis

Karadaghi

Malmstadt

Allsburg

et al. 2020

ACS Sustainable Chem. Eng.

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“…The presence of water during the synthesis was essential for both metal reduction ands tabilizingp olymer dissolution. [18] Rh NPs have also been prepared using ethylene glycol [25] andv anadocene( Cp 2 V) as reducing agents. [26,27] All these NPs have been stabilized by extensively used organic polymers, PVP or PVA.…”

Section: Introductionmentioning

confidence: 99%

Green Synthesis of Rhodium Nanoparticles that are Catalytically Active in Benzene Hydrogenation and 1‐Hexene Hydroformylation

2018

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Rhodium nanoparticles (Rh NPs) were prepared according to a green method based on the reduction of (acetylacetonato)dicarbonylrhodium(I), Rh(acac)(CO)2, in water at 80 °C. The nanoparticles, which were obtained without the addition of a reducing agent, were stabilized by polyvinylpyrrolidone (PVP) or polyvinyl alcohol (PVA) polymers and characterized by TEM (transmission electron microscopy), XPS (X‐ray photoelectron spectroscopy), and XRD (X‐ray powder diffraction) methods. The excellent catalytic activity of these Rh NPs was evidenced in the hydrogenation of benzene to cyclohexane. In the presence of PPh3, Rh NPs formed a highly active system in the hydroformylation of 1‐hexene. In this system, they acted as a source of soluble rhodium species. Rh NPs were also synthesized in water using rhodium(II) acetate, Rh2(OAc)4, and rhodium(III) chloride, RhCl3, as rhodium sources, and their catalytic activity was compared with that of the rhodium precursors.

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“…We have previously used microwave irradiation (μwI) to synthesize monometallic and bimetallic noble metal NPs and demonstrated some important synthetic benefits of μwI over conventional heating (CvH). − For example, it was shown that the synthesis of Pd, Pt, or RhNPs prepared under μwI enabled improved monodispersity and morphological control. These desirable effects were ascribed to faster and more reproducible MNP nucleation events, facilitated at short-lived, nanosized “hot-spots” that are generated by strong rotational coupling of μw’s with polar solvents and ionic precursors, followed by fast localized energy dissipation.…”

Section: Introductionmentioning

confidence: 99%

Continuous Flow Synthesis of Rh and RhAg Alloy Nanoparticle Catalysts Enables Scalable Production and Improved Morphological Control

et al. 2017

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The pursuit of scalable methods for the preparation of well-defined metallic nanoparticles (MNPs) is addressed in this work via a novel microwave-assisted continuous flow synthesis technique. It is shown that single- and two-phase flow synthesis methods provide access to morphologically well-defined and near-monodisperse RhNPs. The RhNPs can be prepared in shorter reaction times and at lower temperatures than are commonly required in conventional batch reactions. Under single-phase flow conditions, in which Rh(III) is reduced in ethylene glycol, near-monodisperse cuboctahedral RhNPs are obtained; the average NP size can be controlled as a function of the residence time of the reactant stream within the microwave cavity. In contrast, a two-phase microfluidic droplet flow method leads to the highly selective formation of Rh multipods. When compared to cuboctahedral RhNPs of comparable size, the Rh multipods are found to exhibit significantly higher catalytic activity in the vapor-phase hydrogenation of cyclohexene. The potential versatility of this new two-phase flow method coupled with microwave-assisted heating is further demonstrated in the synthesis of well-defined isotropic NPs comprised of classically immiscible RhAg random alloys.

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Effect of microwave heating on the synthesis of rhodium nanoparticles in ionic liquids

Cited by 7 publications

References 36 publications

Techno-Economic Analysis of Recycled Ionic Liquid Solvent Used in a Model Colloidal Platinum Nanoparticle Synthesis

Techno-Economic Analysis of Recycled Ionic Liquid Solvent Used in a Model Colloidal Platinum Nanoparticle Synthesis

Green Synthesis of Rhodium Nanoparticles that are Catalytically Active in Benzene Hydrogenation and 1‐Hexene Hydroformylation

Continuous Flow Synthesis of Rh and RhAg Alloy Nanoparticle Catalysts Enables Scalable Production and Improved Morphological Control

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