Metal nanoparticles (M-NPs) of ruthenium, rhodium, iridium and platinum were synthesized and supported on covalent triazine-based framework from 1,4-dicyanobenzene (CTF-1) by rapid microwave induced decomposition of their binary metal(0) carbonyls for Ru, Rh and Ir or Pt(acac)2 in the presence of CTF-1 in the ionic liquid (IL) 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([BMIm][NTf2]) or in propylene carbonate (PC). (High-resolution) transmission electron microscopy, (HR-)TEM showed the formation of M-NPs on CTF-1 with, e.g., size distributions of 3.0 (±0.5) nm for Ru@CTF-1 synthesized in [BMIm][NTf2] and 2 (±1) nm for Rh@CTF-1 synthesized in PC. The crystalline phases of the M-NPs and the absence of significant impurities were verified by powder X-ray diffraction (PXRD) and selected area electron diffraction (SAED). The metal content of the M@CTF-1 composites was determined by flame atomic absorption spectroscopy (AAS) to be between 3 and 12 wt%. The Rh@CTF-1 composite nanomaterial proved to be a highly active (∼31 000 mol cyclohexane per (mol Rh) per h) heterogeneous catalyst for the hydrogenation of benzene to cyclohexane under mild (10 bar H2, 70 °C) and solvent-free conditions with over 99% conversion. The catalyst could be re-used for at least ten consecutive hydrogenation reactions. Additionally, Rh@CTF-1 is an active electrocatalyst for the hydrogen evolution reaction (HER) with an operating potential of −58 mV, while Pt@CTF-1 and commercial Pt/C shows a more negative operating potential of −111 and −77 mV. Also the onset potential of −31 mV for Rh@CTF-1 is much more positive than that of Pt@CTF-1 (−44 mV) and commercial Pt/C (−38 mV).

Rhodium nanoparticles supported on covalent triazine-based frameworks as re-usable catalyst for benzene hydrogenation and hydrogen evolution reaction

Herein we report a very simple ‘mix and heat’ synthesis of a very fine Rh-nanoparticle loaded carbon fullerene-C60 nanocatalyst (Rh(0)NPs/Fullerene-C60) for the very first time. The preparation method used no reducing agent and capping agent to control the morphology of the nanocatalyst. Transmission electron microscopy (TEM) results confirmed the uniform decoration of small Rh-nanoparticles on the surface of fullerene-C60. The Rh-content in Rh(0)NPs/Fullerene-C60 was found to be 2.89 wt%. The crystalline properties of Rh(0)NPs/Fullerene-C60 were studied by X-ray diffraction (XRD). The metallic state of Rh-nanoparticles in Rh(0)NPs/Fullerene-C60 was confirmed by X-ray photoemission spectroscopy (XPS). Raman results depicted good interaction between Rh-nanoparticles and fullerene-C60. To our delight, the present Rh(0)NPs/Fullerene-C60 showed excellent catalytic activity in the reduction of 4-nitrophenol with NaBH4 in water. Very high kapp, k′ and TOF values of 82.14 × 10−3 min−1, 4107 × 10−3 min−1 and 138 min−1, respectively, were calculated for the Rh(0)NPs/Fullerene-C60 catalyzed reduction of 4-nitrophenol. To the best of our knowledge, this is the most efficient fullerene-based nanocatalyst for the rapid reduction of 4-nitrophenol reported to date. Moreover, the catalytic activity of Rh(0)NPs/Fullerene-C60 was also tested towards Suzuki cross-coupling reactions. Reusability of the Rh(0)NPs/Fullerene-C60 was also tested.

/pdf/reducing-agent-free-facile-preparation-of-rh-nanoparticles-46rney1mp2.pdf

Reducing-agent-free facile preparation of Rh-nanoparticles uniformly anchored on onion-like fullerene for catalytic applications

A potential high durable heterogeneous catalyst for the industrial selective hydrogenation of nitrile butadiene rubber (NBR) has been established by immobilizing palladium (Pd) nanoparticles on macroporous hollow silica (MHS) microspheres in the present work Compared with the Pd nanoparticles supported on macroporous hollow silica (Pd/MHS) via conversional incipient wetness impregnation with different free chelating reagents (HCl or EDTA) catalysts, the Pd nanoparticles supported on the modified macroporous hollow silica (Pd/M-MHS) catalyst showed better distribution of Pd nanoparticles and catalytic performance High hydrogenation degree (HD) toward the –CH CH– group of 97% was achieved in acetone solution at 70 °C with H 2 pressure of 45 MPa for 6 h, while the nitrile (–C N) group had not been hydrogenated in the reaction And there was no obvious change in the relative molecular weight and polydispersion index of the product in comparison with the raw NBR The HD for the 5th reuse was 905%, remaining more than 93% of its HD for the original time, demonstrating its high durable activity

Macroporous hollow silica microspheres-supported palladium catalyst for selective hydrogenation of nitrile butadiene rubber

A series of silica supported Pd (Pd/SiO2) catalysts were prepared in various HCl concentrations (CHCl) of the impregnation solution with different electrostatic interactions between Pd precursor and support, and their catalytic properties were evaluated by the selective hydrogenation of nitrile butadiene rubber (NBR). The results show that with the CHCl increasing from 0.1 to 5 M, the particle size of Pd nanoparticles dramatically decreases from 24.2 to 5.1 nm and stabilizes at ∼5 nm when CHCl is higher than 2 M. Using the catalysts prepared with a high CHCl (>2 M), an excellent hydrogenation degree (HD) of ∼94% with 100% selectivity to C═C can be acquired under mild conditions. Interestingly, the HD could be remarkably increased from 65 to 92% by increasing only CCl– from 0.1 to 2 M with the addition of NaCl while keeping CH+ at 0.1 M. This is because PdCl42– is the predominant existing form of precursor at high CCl–, which has a strong electrostatic attraction with the positively charged support favorab...

Synthesis of Pd/SiO2 Catalysts in Various HCl Concentrations for Selective NBR Hydrogenation: Effects of H+ and Cl– Concentrations and Electrostatic Interactions

The mesopore-elimination treatment and silanol-groups recovery for macroporous silica microspheres and its application as an efficient support for polystyrene hydrogenation

Selective hydrogenation of nitrile butadiene rubber (NBR) with rhodium nanoparticles supported on carbon nanotubes at room temperature

The invention relates to a preparation method of a carbon nano tube supported nanometer particle catalyst. The method comprises the steps of: adding a metal precursor, a reducing agent and a carbon nanotube to the water solution, fully mixing, and conducting microwave heating under the high pressure condition. The preparation process of the catalyst provided by the invention is simple, and has mild preparation conditions; the green raw materials are subjected to microwave heating reduction; the whole process has the characteristics of green, environment-friendliness, energy saving, high efficiency, good stability of catalyst, and no oxygen isolation operation; and the prepared catalyst for the first time realizes catalytic hydrogenation reaction at room temperature, and is high in catalytic activity, easy for separation and beneficial for industrial application.

Preparation method of carbon nano tube supported nanometer particle catalyst

The invention provides a preparation method for hydrophilic aminated hydrogenated butadiene-acrylonitrile rubber. The method comprises the steps that 1, a nanometer Rh metal catalyst and butadiene-acrylonitrile rubber are mixed and dispersed evenly; 2, mixed liquid obtained in the step 1 is added in a reaction kettle, and first-step catalytic hydrogenation is performed under the hydrogen pressure of 1-5 MPa; 3, a RhCl(PPh3)3 catalyst with the mass fraction of 0.5-2.0% is added in a catalytic hydrogenation reaction product, and reacting is performed for 1-3 h under the hydrogen pressure of 1-5 MPa. The invention further provides the hydrophilic aminated hydrogenated butadiene-acrylonitrile rubber prepared through the preparation method. The prepared aminated hydrogenated butadiene-acrylonitrile rubber has the good hydrophilicity, and the hydrophilicity of the aminated hydrogenated butadiene-acrylonitrile rubber is improved along with increasing of the amino group content; existence of amino groups in the aminated hydrogenated butadiene-acrylonitrile rubber supplies active sites to introduction of organic matter containing carboxyl groups and epoxy groups.

Preparation method for hydrophilic aminated hydrogenated butadiene-acrylonitrile rubber and prepared product

A recyclable heterogeneous rhodium catalyst (MTS-T-Rh) was prepared by loading Rh species onto an amino-silica support grafted by tannin, an intermediate linker and stabilizer, and fully c...

Highly active and reusable rhodium catalyst for selective hydrogenation of nitrile–butadiene rubber

The invention provides a preparation method of a non-loaded nano-metal catalyst. The method comprises the steps that 1, a metal precursor and deionized water are mixed and evenly stirred at room temperature to obtain a metal precursor water solution, namely the solution A; 2, sodium hydroxide is dissolved in a hydrazine hydrate to obtain a hydrazine hydrate solution of the sodium hydroxide; 3, the solution A is dropped into a solution B, and a reaction is carried out for 1-5 h on the conditions of stirring and backflow. The invention further provides application of the non-loaded nano-metal catalyst. The method is used for preparing the non-loaded nano-metal Rh catalyst, the prepared catalyst is free of load, the reducing agent hydrazine hydrate and nano Rh are subjected to complexation in the preparation process, so that the nano Rh has monodispersity, and the average grain diameter is 1.84 nm. The nano-metal Rh catalyst cost is greatly reduced, and the catalyst technological process is simplified. The catalyst is used for carrying out a catalytic hydrogenation reaction, the catalytic activity of the catalyst is high, and the catalyst is easy to separate in a reaction system and is stable in air.

Preparation and application of non-loaded nano-metal catalyst

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