scholarly journals Synthesis, Structures, Electrochemistry, and Catalytic Activity towards Cyclohexanol Oxidation of Mono-, Di-, and Polynuclear Iron(III) Complexes with 3-Amino-2-Pyrazinecarboxylate

2020 ◽  
Vol 10 (8) ◽  
pp. 2692
Author(s):  
Anirban Karmakar ◽  
Luísa M.D.R.S. Martins ◽  
Yuliya Yahorava ◽  
M. Fátima C. Guedes da Silva ◽  
Armando J. L. Pombeiro
Keyword(s):  
Coordination Polymer ◽  
Heterogeneous Catalysts ◽  
Saturated Calomel Electrode ◽  
Two Dimensional ◽  
Reaction Conditions ◽  
Ability To Act ◽  
Tert Butyl Hydroperoxide ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

The synthesis and characterization of a set of iron(III) complexes, viz. the mononuclear [Fe(L)3] (1) and [NHEt3][Fe(L)2(Cl)2] (2), the dinuclear methoxido-bridged [Fe(L)2(μ-OMe)]2.DMF.1.5MeOH (3), and the heteronuclear Fe(III)/Na(I) two-dimensional coordination polymer [Fe(N3)(μ-L)2(μ-O)1/2(Na)(μ-H2O)1/2]n (4), are reported. Reactions of 3-amino-2-pyrazinecarboxylic acid (HL) with iron(III) chloride under different reaction conditions were studied, and the obtained compounds were characterized by elemental analysis, Fourier Transform Infrared (FT-IR) spectroscopy, and X-ray single-crystal diffraction. Compound 1 is a neutral mononuclear complex, whereas 2 is mono-anionic with its charge being neutralized by triethylammonium cation. Compounds 3 and 4 display a di-methoxido-bridged dinuclear complex and a two-dimensional heterometallic Fe(III)/Na(I) polynuclear coordination polymer, respectively. Compounds 3 and 4 are the first examples of methoxido- and oxido-bridged iron(III) complexes, respectively, with 3-amino-2-pyrazinecarboxylate ligands. The electrochemical study of these compounds reveals a facile single-electron reversible Fe(III)-to-Fe(II) reduction at a positive potential of 0.08V vs. saturated calomel electrode (SCE), which is in line with their ability to act as efficient oxidants and heterogeneous catalysts for the solvent-free microwave-assisted peroxidative oxidation (with tert-butyl hydroperoxide) of cyclohexanol to cyclohexanone (almost quantitative yields after 1 h). Moreover, the catalysts are easily recovered and reused for five consecutive cycles, maintaining a high activity and selectivity.

Hydrothermal synthesis, crystal structure and properties of a two-dimensional uranyl coordination polymer based on a flexible zwitterionic ligand

2018 ◽  
Vol 74 (3) ◽  
pp. 366-371 ◽  
Author(s):  
Wen Cui ◽  
Ruyu Wang ◽  
Xi Shu ◽  
Yu Fan ◽  
Yang Liu ◽  
...  
Keyword(s):  
Coordination Polymer ◽  
Hydrothermal Reaction ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Uranyl Compounds ◽  
X Ray ◽  
Potential Applications ◽  
Ft Ir ◽  
Fuel Reprocessing ◽  
Ft Ir Spectroscopy

The interaction between the uranyl cation, (UO2)2+, and organic species is of interest due to the potential applications of the resulting compounds with regard to nuclear waste disposal and nuclear fuel reprocessing. The hydrothermal reaction of various uranyl compounds with flexible zwitterionic 1,1′-[1,4-phenylenebis(methylene)]bis(pyridin-1-ium-4-carboxylate) dihydrochloride (Bpmb·2HCl) in deionized water containing drops of H2SO4resulted in the formation of a novel two-dimensional uranyl coordination polymer, namely poly[tetraoxido{μ2-1,1′-[1,4-phenylenebis(methylene)]bis(pyridin-1-ium-4-carboxylate)}di-μ3-sulfato-diuranium(VI)], [(UO2)2(SO4)2(C20H16N2O4)]n, (1). Single-crystal X-ray diffraction reveals that this coordination polymer exhibits a layered arrangement and the (UO2)2+centre is coordinated by five equatorial O atoms. The structure was further characterized by FT–IR spectroscopy, powder X-ray diffraction (PXRD) and thermogravimetric analysis (TGA). The polymer shows high thermal stability up to 696 K. Furthermore, the photoluminescence properties of (1) has also been studied, showing it to exhibit a typical uranyl fluorescence.

scholarly journals Synthesis and Characterization of Graphene Oxide Derivatives via Functionalization Reaction with Hexamethylene Diisocyanate

Proceedings ◽  
2018 ◽  
Vol 3 (1) ◽  
pp. 8 ◽  
Author(s):  
José A. Luceño-Sánchez ◽  
Georgiana Maties ◽  
Camino Gonzalez-Arellano ◽  
Ana M. Díez-Pascual
Keyword(s):  
Graphene Oxide ◽  
High Performance ◽  
Organic Molecules ◽  
Hexamethylene Diisocyanate ◽  
Reaction Conditions ◽  
Ft Ir ◽  
Oxygen Groups ◽  
Functionalization Reaction ◽  
Ft Ir Spectroscopy

Graphene oxide (GO), the oxidized form of graphene, shows unique properties, such as strong mechanical strength, high thermal conductivity, amphiphilicity, and surface functionalization capability that make it very attractive in various fields, ranging from medicine to optoelectronic devices and solar cells. However, its insolubility in non-polar and polar aprotic solvents hinders some applications. To solve this issue, novel functionalization strategies are pursued. In this regard, the current study deals with the preparation and characterization of hexamethylene diisocyanate (HDI)-functionalized GO. Different reaction conditions were tested to optimize the functionalization degree (FD), and detailed characterization was conducted via Fourier-transformed infrared (FT-IR) spectroscopy to confirm the success of the functionalization reaction. The HDI-GO could further react with other organic molecules or polymers via the remaining oxygen groups, which makes them ideal candidates as nanofillers for high-performance GO-based polymer nanocomposites.

Synthesis and Characterization of Triethanolamine Borate

2013 ◽  
Vol 709 ◽  
pp. 28-31
Author(s):  
Cheng Xue Wang ◽  
Tian Tian Liang ◽  
Chun Qiao Wei
Keyword(s):  
Mass Spectrometry ◽  
Differential Scanning Calorimetry ◽  
Synthesis And Characterization ◽  
Spectroscopy Analysis ◽  
Scanning Calorimetry ◽  
Reaction Conditions ◽  
Different Types ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

Starting with boric acid and triethanolamine , the effect of the different types of the water-carrying agent on the yield was invested, and influences of dosage of water-carrying agent ,the mole ratio of reactants, reaction time on yield were discussed, the optimized reaction conditions were confirmed. The structure of the product was described by Fourier transform-infrared (FT-IR) spectroscopy, NMR Spectroscopy analysis, mass spectrometry (MS) and thermodynamic properties was analyzed by differential scanning calorimetry (DSC) and thermogravimetry (TG).

scholarly journals SYNTHESIS OF GRAFT COPOLYMER FROM ETHYL METHACRYLATE ONTO DELIGNIFIED GREWIA OPTIVA FIBER

2021 ◽  
pp. 350-365
Author(s):  
Vivek Nandani ◽  
Kinnari Trived
Keyword(s):  
Ascorbic Acid ◽  
Graft Copolymer ◽  
Gravimetric Analysis ◽  
Electron Microscopic ◽  
Reaction Conditions ◽  
Ethyl Methacrylate ◽  
Grewia Optiva ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

Ethyl methacrylate was grafted onto delignified Grewia optiva fiber using ascorbic acid/H2O2 as redox initiators in an aqueous medium. The reaction variables including concentration of ascorbic acid, H2O2, monomer and amount of backbone as well as time and temperature have been varied for establishing grafting. The influence of these reaction conditions on the grafting yield has been discussed. The overall activation energy of grafting has been calculated. The FT-IR spectroscopy, Thermal Gravimetric Analysis (TGA) and Scanning Electron Microscopic (SEM) techniques have been used for the characterization of graft copolymer.

scholarly journals Copper(II) complex of (±)trans-1,2-cyclohexanediamine azo-linked Schiff base ligand encapsulated in nanocavity of zeolite-Y for the catalytic oxidation of olefins

2016 ◽  
Vol 81 (2) ◽  
pp. 153-162 ◽  
Author(s):  
Maryam Lashanizadegan ◽  
Sahar Shayegan ◽  
Marzieh Sarkheil
Keyword(s):  
Schiff Base ◽  
Schiff Base Ligand ◽  
Heterogeneous Catalysts ◽  
Zeolite Y ◽  
Schiff Base Complex ◽  
Reaction Conditions ◽  
Catalytic Behavior ◽  
Tert Butyl Hydroperoxide ◽  
Oxidation Of Olefins ◽  
Ft Ir

A Schiff base ligand derived from 4-(benzeneazo) salicylaldehyde and (?)trans-1,2-cyclohexanediamine (H2L) and its corresponding Cu(II) complex (CuL) has been synthesized and characterized by FT-IR, UV-VIS and 1H NMR. The copper Schiff base complex encapsulated in the nanopores of zeolite-Y (CuL-Y) by flexible ligand method and its encapsulation have been ensured by different studies. The homogeneous and its corresponding heterogeneous catalysts have been used for oxidation of different alkenes with tert-butyl hydroperoxide. Under the optimized reaction conditions, the oxidation of cyclooctene, cyclohexene, styrene and norbornene catalyzed by CuL gave 89, 63, 46 and 13% conversion, respectively. These olefins were oxidized efficiently with 50, 96, 96 and 92% conversion in the presence of CuL-Y, respectively. Comparison of the catalytic behavior of CuL and CuL-Y showed the higher catalytic activity and selectivity of the heterogeneous catalyst with respect to the homogenous one.

scholarly journals Selective Styrene Oxidation to Benzaldehyde over Recently Developed Heterogeneous Catalysts

Molecules ◽  
2021 ◽  
Vol 26 (6) ◽  
pp. 1680
Author(s):  
Marta A. Andrade ◽  
Luísa M. D. R. S. Martins
Keyword(s):  
Heterogeneous Catalysts ◽  
Carbon Materials ◽  
Oxygen Species ◽  
Styrene Oxidation ◽  
Reaction Conditions ◽  
Reactive Metal ◽  
Catalytic Systems ◽  
Tert Butyl Hydroperoxide ◽  
Metal Organic ◽  
Important Intermediate

The selective oxidation of styrene under heterogeneous catalyzed conditions delivers environmentally friendly paths for the production of benzaldehyde, an important intermediate for the synthesis of several products. The present review explores heterogeneous catalysts for styrene oxidation using a variety of metal catalysts over the last decade. The use of several classes of supports is discussed, including metal–organic frameworks, zeolites, carbon materials and silicas, among others. The studied catalytic systems propose as most used oxidants tert-butyl hydroperoxide, and hydrogen peroxide and mild reaction conditions. The reaction mechanism proceeds through the generation of an intermediate reactive metal–oxygen species by catalyst-oxidant interactions. Overall, most of the studies highlight the synergetic effects among the metal and support for the activity and selectivity enhancement.

scholarly journals Synthesis and Structural Characterization of (E)-4-[(2-Hydroxy-3-methoxybenzylidene)amino]butanoic Acid and Its Novel Cu(II) Complex

Molbank ◽  
10.3390/m1179 ◽  
2021 ◽  
Vol 2021 (1) ◽  
pp. M1179
Author(s):  
Eleftherios Halevas ◽  
Antonios Hatzidimitriou ◽  
Barbara Mavroidi ◽  
Marina Sagnou ◽  
Maria Pelecanou ◽  
...  
Keyword(s):  
Schiff Base ◽  
Gamma Aminobutyric Acid ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
Polymeric Compound ◽  
Bridging Ligands ◽  
1H And 13C Nmr ◽  
One Dimensional ◽  
Ft Ir

A novel Cu(II) complex based on the Schiff base obtained by the condensation of ortho-vanillin with gamma-aminobutyric acid was synthesized. The compounds are physico-chemically characterized by elemental analysis, HR-ESI-MS, FT-IR, and UV-Vis. The complex and the Schiff base ligand are further structurally identified by single crystal X-ray diffraction and 1H and 13C-NMR, respectively. The results suggest that the Schiff base are synthesized in excellent yield under mild reaction conditions in the presence of glacial acetic acid and the crystal structure of its Cu(II) complex reflects an one-dimensional polymeric compound. The molecular structure of the complex consists of a Cu(II) ion bound to two singly deprotonated Schiff base bridging ligands that form a CuN2O4 chelation environment, and a coordination sphere with a disordered octahedral geometry.

Diffuse Reflectance FT-IR Characterization of Active Sites under Reaction Conditions: The Production of Oxygenates in the CO/H2 Reaction

1994 ◽  
Vol 48 (10) ◽  
pp. 1208-1212 ◽  
Author(s):  
J. J. Benítez ◽  
I. Carrizosa ◽  
J. A. Odriozola
Keyword(s):  
Infrared Spectra ◽  
Active Sites ◽  
Diffuse Reflectance ◽  
Reaction Conditions ◽  
In Situ Drifts ◽  
Ft Ir

The reactivity of a Lu2O3-promoted Rh/Al2O3 catalyst in the CO/H2 reaction is reported. Methane, heavier hydrocarbons, methanol, and ethanol are obtained. In situ DRIFTS has been employed to record the infrared spectra under the actual reaction conditions. The structure of the observed COads DRIFTS bands has been resolved into its components. The production of oxygenates (methanol and ethanol) has been correlated with the results of the deconvolution calculation. Specific sites for the production of methanol and ethanol in the CO/H2 reaction over a Rh,Lu2O3/Al2O3 catalyst are proposed.

One Step Synthesis and Characterization of Zirconia-Graphene Composites

2012 ◽  
Vol 600 ◽  
pp. 174-177 ◽  
Author(s):  
Jian Fei Xia ◽  
Zong Hua Wang ◽  
Yan Zhi Xia ◽  
Fei Fei Zhang ◽  
Fu Qiang Zhu ◽  
...  
Keyword(s):  
Synthesis And Characterization ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Graphene Composite ◽  
Transmission Electron ◽  
One Step ◽  
Ft Ir ◽  
Xrd Techniques

Zirconia-graphene composite (ZrO2-G) has been successfully synthesized via decomposition of ZrOCl2•6H2O in a water-isopropanol system with dispersed graphene oxide (GO) utilizing Na2S as a precursor could enable the occurrence of the deposition of Zr4+ and the deoxygenation of GO at the same time. Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) techniques were used to characterize the samples. It was found that graphene were fully coated with ZrO2, and the ZrO2 existing in tetragonal phase, which resulted in the formation of two-dimensional composite.

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