Immobilized copper(II) on nitrogen‐rich polymer‐entrapped Fe3O4 nanoparticles: a highly loaded and magnetically recoverable catalyst for aqueous click chemistry

A heterogeneous magnetic copper catalyst was prepared via anchoring of copper sulfate onto multi‐layered poly(2‐dimethylaminoethyl acrylamide)‐coated magnetic nanoparticles and was characterized using various techniques. The catalyst was found to be active, effective and selective for one‐pot three‐component reaction of alkyl halide, sodium azide and alkyne, known as copper‐catalyzed click synthesis of 1,2,3‐triazoles. As little as 0.3 mol% of catalyst was found to be effective under the optimum conditions. The catalyst could also be recycled and reused up to seven times without significant loss of activity. Thermal stability, high loading level of copper on catalyst, broad diversity of alkyl/benzyl/allyl bromide/chloride and alkyl/aryl terminal alkynes without isolation of azide intermediate, and good to excellent yields of products make this procedure highly economical. Copyright © 2015 John Wiley & Sons, Ltd.     

An aptasensor for tetracycline using a glassy carbon modified with nanosheets of graphene oxide

Microchimica Acta - The authors describe an aptasensor for tetracycline (TET) based on the use of a glassy carbon electrode (GCE) modified with graphene oxide nanosheets. The latter were placed on...     

Suzuki–Miyaura coupling reaction in water in the presence of robust palladium immobilized on modified magnetic Fe3O4 nanoparticles as a recoverable catalyst

Aryl halides and especially inactive aryl chlorides were coupled to benzenoid aromatic rings in a Suzuki–Miyaura coupling reaction in the absence of organic solvents and toxic phosphine ligands. The reaction was catalysed by a recoverable magnetic nanocatalyst, Pd@Fe₃O₄, in aqueous media. This method is green, and the catalyst is easily removed from the reaction media using an external magnetic field and can be re‐used at least 10 times without any considerable loss in its activity. The catalyst was characterized using scanning and transmission electron microscopies, thermogravimetric analysis, inductively coupled plasma spectroscopy, Fourier transform infrared spectroscopy, CHN analysis, X‐ray diffraction and vibrating sample magnetometry.     

Synthesis of <Emphasis Type="Italic">N</Emphasis>-hydroxy-imidamide-functionalized graphene: an efficient metal-free electrocatalyst for oxygen reduction

Metal-free electrocatalysts for oxygen reduction reaction (ORR) are key to the development of efficient, durable, and low-cost alternatives to noble-metal-based electrocatalysts in fuel cell cathodes. In recent years, many efforts are directed to the metal-free catalyst based on heteroatom-doped graphene. In this work, we demonstrate that the graphene surface can be converted into the catalyst for the oxygen reduction by chemical functionalization. In this context, we first synthesized malononitrile-functionalized graphene oxide. Amidoximation of nitrile group and reduction in graphene oxide were then carried out by hydroxylamine in one step. The electrochemical behavior of functionalized graphene-modified electrode for the reduction in oxygen was studied. The results showed that the electrocatalyst fabricated by this method exhibited striking catalytic activities in alkaline solution. In alkaline solution, this catalyst showed a competitive activity to the commercial Pt catalyst via four-electron transfer pathway with better ORR selectivity and stability. In addition, this metal-free electrocatalyst exhibited tolerance to methanol crossover effect. Based on its outstanding performance, this functionalized graphene electrocatalyst showed the promising prospect of a metal-free catalyst for fuel cell with much lower cost than currently used Pt/C catalyst.     

The Oxidation of Thiocyanate to Polythiocyanic Acid Using Peroxydisulfate in Aqueous Solution

Abstract

The oxidation of thiocyanate to polythiocyanic acid by peroxydisulfate was carried out in an aqueous solution at room temperature. The primary step is the decomposition of peroxydisulfate into sulfate-free radicals. At room temperature in the presence of peroxydisulfate as a oxidizing agent, HSCN polymerizes to (HSCN)_n. The oxidation of thiocyanate in an aqueous solution is often complicated, but here we obtained the polythiocyanic acid as a major product. The products were characterized by elemental analysis, IR, UV- visible, H-NMR spectroscopy, and X-ray powder diffraction.     

Synthesis and Characterization of Organosoluble Poly(imide-ether)s with Bulky 2,3-Diaryl Imidazole Moiety: Study Physical,Thermal and Optical Properties

Two new symmetrical diamines were designed and synthesized having different functional groups such as a pair of phenyl ether linkages, 2,3-diaryl substituted imidazole rings and CF₃ groups as pendant, and characterized by FT-IR, ¹H and ¹³C-NMR spectroscopy and elemental analysis. A series of new fluorescent poly(imide-ether)s (PIEs) was prepared by polymerization of the diamines with commercial tetracarboxylic dianhydrides such as pyromellitic dianhydride and 3,3′,4,4′-benzophenone tetracarboxylic dianhydride. The resulting PIEs were amorphous and had intrinsic viscosity [η] in the range of 0.42–0.51 dL/g. The weight average molecular weights (Mw) of these polymers were measured by GPC and were in the range of 28658–35595 g/mol with molecular weight distribution (MWD) of 2.12–2.27. These polymers were readily soluble in a variety of organic solvents and formed low-colored and flexible thin films with cut-off wavelength (λ₀) in the range of 385–420 nm, and all PIEs films exhibited high optical transparency. They also possessed good thermal stability with 10% weight loss temperatures (T_10%) in the range 486–537°C in N₂. The glass transition temperatures (T_g) of PIEs are in the range 251–324°C. These polymers showed fluorescence emission in film and in solution at 459–476 nm with the quantum yields in the range 4–12%.