scholarly journals Nucleophilic reactivity and electrocatalytic reduction of halogenated organic compounds by nickel o-phenylenedioxamidate complexes

2016 ◽  
Vol 45 (34) ◽  
pp. 13556-13564 ◽  
Author(s):  
Siva Prasad Das ◽  
Rakesh Ganguly ◽  
Yongxin Li ◽  
Han Sen Soo

Nickel(ii)-ate complexes supported by o-phenylenebis(N-methyloxamide) reacted with alkyl halides to form new imidate tautomers which were characterized by X-ray crystallography and FT-IR spectroscopy, and used for electroreduction of chloroform.

2010 ◽  
Vol 63 (2) ◽  
pp. 252 ◽  
Author(s):  
Jingli Xie ◽  
Ryan Gilbert-Wilson ◽  
Boujemaa Moubaraki ◽  
Keith S. Murray ◽  
Anthony G. Wedd

Two new hybrid materials [Fe(bipy)3]3[ZnW12O39(OH)Fe(bipy)2(H2O)]2 and [Fe(bipy)3]2[CoW12O40] were obtained by hydrothermal synthesis. They contain [Fe(bipy)3] n+ (bipy = 2,2′-bipyridyl; n = 2 or 3) cations and Keggin-type polyoxotungstate anions. Both have been characterized by elemental analysis, FT-IR spectroscopy, 1H-NMR spectrometry, and single crystal X-ray crystallography. The anion in the former salt features [FeII(bipy)2(OH2)]2+ units covalently bound via a W=O-Fe bridge to the protonated anion [ZnW12O39(OH)]5–. The latter salt contains discrete [CoW12O40]6– anions.


2017 ◽  
Author(s):  
◽  
Sharista Raghunath

The presence of dyes in effluent poses various environmental as well as health hazards for many organisms. Although various remediation strategies have been implemented to reduce their effect, dyes still manage to infiltrate into the environment and hence new strategies are required to address some of the problems. This study investigated the innovation of two cationic water-soluble polymers viz., Proline-Epichlorohydrin-Ethylenediamine Polymer (PEP) and Thiazolidine-Epichlorohydrin-Ethylenediamine Polymer (TEP) that were used to remediate selected synthetic dyes from synthetic effluent by adsorption and dye reduction. Both polymers were synthesized using monomers of a secondary amine, epichlorohydrin and ethylenediamine and were subsequently characterized and modified and their remediation potential studied. In the first study, PEP was synthesized and characterized by 1H-NMR Spectroscopy, FT-IR Spectroscopy, dynamic light scattering, and thermogravimetric analysis (TGA). Thereafter PEP was modified with bentonite clay, by simple mixing of the reactants, to form a Proline-Epichlorohydrin-Ethylenediamine Polymer-bentonite composite (PRO-BEN); it was characterized by FT-IR Spectroscopy, scanning electron microscopy (SEM)/ energy dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Adsorption studies were then undertaken with a synthetic effluent containing three textile dyes, viz., Reactive Blue 222 (RB 222), Reactive Red 195 (RR 195) and Reactive Yellow (RY 145). Various conditions were investigated including pH of the solution, temperature, sodium chloride concentration, initial dye concentration and the dosage of adsorbent used. The experimental data for all dyes followed a Langmuir isotherm. The adsorption process was found to be pseudo-second order. According to the thermodynamic parameters, the adsorption of the dyes was classified as physisorption and the reaction was spontaneous and exothermic. The data were also compared using studies with alumina as an adsorbent. Results showed that PRO-BEN exhibited better absorptivity and desorption than alumina making its use a better recyclable remediation strategy for the removal of organic dyes in wastewater treatment plants. In the second study, TEP was synthesized and then characterized by FT-IR Spectroscopy, 1H-NMR Spectroscopy, TGA and DLS. Thereafter, TEP was used to prepare TEP capped gold nanoparticles (TEP-AuNPs). Herein, two methods were investigated: the Turkevich method and an adaptation of the Turkevich method using bagasse extract. The TEP-AuNPs was characterized by FT-IR Spectroscopy, SEM, EDX, DLS and TEM. Thereafter the reduction of each of Allura Red, Congo Red and Methylene Blue was investigated with the TEP-AuNPs for its catalytic activity toward dye reduction. This study showed that the batch of AuNPs prepared by the Turkevich method had higher rates of dye reduction compared with AuNPs prepared using bagasse extract. Also the quantity of TEP used as capping agent greatly influenced the size, shape and surface charge of the nanoparticles as well as their catalytic performance: the Vroman effect explained this behavior of the TEP-AuNPs. It was finally concluded that whilst PRO-BEN, in the first study, showed excellent dye remediation properties, the second study on TEP-AuNPs showed good catalytic activity for the reduction of selected dyes, however, it was more effective at lower polymer concentration. Finally, both materials displayed good potential for the clean-up of selected synthetic dyes from synthetic effluents.


2020 ◽  
Vol 1 (4) ◽  
pp. 22-25
Author(s):  
Azwan Morni

This study reports a green method for the synthesis of gold nanoparticles (AuNPs) using the aqueous extract of Salix aegyptiaca extract. The effects of gold salt concentration, extract concentration and extract quantity were investigated on nanoparticles synthesis. Novel methods of ideally synthesizing AuNPs are thus thought that are formed at ambient temperatures, neutral pH, low costs and environmentally friendly fashion. AuNPs were characterized with different techniques such as UV–vis spectroscopy, FT-IR spectroscopy, X-ray diffraction, and TEM. FT-IR spectroscopy revealed that gold nanoparticles were functionalized with biomolecules that have primary carbonyl group, -OH groups and other stabilizing functional groups. TEM experiments showed that these nanoparticles are formed with various shapes and X-ray diffraction pattern showed high purity and face centered cubic structure of AuNPs. For electrochemical properties of AuNPs, a modified glassy carbon electrode using AuNPs (AuNPs/GCE) was investigated. The results show that electronic transmission rate between the modified electrode and [Fe (CN)6]3-/4- increased.


2011 ◽  
Vol 239-242 ◽  
pp. 2839-2842
Author(s):  
Hong Mei Mu ◽  
Peng Fei ◽  
Bi Tao Su ◽  
Zi Qiang Lei

A series of Fe3+-dopped polyaniline (Fe3+/PANI) nanomaterials with different morphologies and a higher conductivity were successfully synthesized using a simple and static interfacial polymerization by using FeCl3 as both oxidant catalyst and dopant. The effect of surfactants CTAB and SDS and the concentration of FeCl3 on the morphology and conductivity of Fe3+/PANI nanomaterial were investigated. The samples were characterized by Transmission Electron Microscopy (TEM), SDY-4 probes conductivity meter, X-ray Diffractometry (XRD), Energy dispersive spectroscopy (EDS) and Fourier transform infrared (FT-IR) spectroscopy techniques. TEM’s results showed that their morphologies changed with the type of the surfactant and the concentration of FeCl3. Introducing surfactants CTAB and SDS into Fe3+/PANI remarkably improved the conductivity of the material. The conductivities of CTAB/Fe3+/PANI and SDS /Fe3+/PANI nanomaterials were respectively about 4.8×10-2 and 1.3×10-2 S/cm while the conductivity of Fe3+/PANI was found to be 1.5×10-4 S/cm. The different morphology and high conductivity may be ascribed to the mutual effects of the surfactant and oxidant.


2016 ◽  
Vol 71 (1) ◽  
pp. 81-84 ◽  
Author(s):  
Eugen Weisheim ◽  
Hans-Georg Stammler ◽  
Norbert W. Mitzel

AbstractThe reaction of 1,3,5-triethynyl-1,3,5-trimethyl- 1,3,5-trisilacyclohexane with (dimethylamino)trimethylstannane afforded 1,3,5-tris[(trimethylstannyl)ethynyl]- 1,3,5-trimethyl-1,3,5-trisilacyclohexane with tin-functionalised ethynyl groups. The compound was characterized by single-crystal X-ray diffraction, elemental analysis, mass spectrometry, NMR and FT-IR spectroscopy.


2020 ◽  
Vol 76 (7) ◽  
pp. 690-694
Author(s):  
Qianjun Deng ◽  
Jiming Wang ◽  
Guangzhao Li ◽  
Shuhua Zhang

A new ionic pentanuclear FeIII cluster, namely, triethylazanium tetrakis(μ2-5-amino-1,2,3,4-tetrazolido)tetrakis(μ3-4-chloro-2-{[(1H-tetrazol-1-id-5-yl)imino]methyl}phenolato)di-μ3-oxido-pentairon(III) acetonitrile monosolvate monohydrate, (C6H16N)[Fe5(C8H4ClN5O)4(CH2N5)4O2]·CH3CN·H2O, was synthesized using microvial synthesis methods and characterized by elemental analysis, FT–IR spectroscopy, single-crystal X-ray diffraction and thermogravimetric analysis. Magnetic studies reveal that the complex displays dominant antiferromagnetic intracluster interactions between the FeIII ions through the μ3-oxide bridges.


2018 ◽  
Vol 81 (1) ◽  
Author(s):  
Umi Athiyah ◽  
Putu Andika Kusuma ◽  
Tutik Tutik ◽  
Maria L. A. D. Lestari ◽  
Dewi Isadiartuti ◽  
...  

Quercetin has been proposed to exhibit numerous pharmacological benefits yet suffer low bioavailability due to the extremely low solubility. A research to study the impact of cocrystallization of quercetin with succinic acid on the solubility and dissolution profile has been performed. Cocrystallization in molar stoichiometry of 1:1 was carried out via liquid assisted grinding with methanol in ball milling apparatus. Cocrystal formation was identified by hot stage microscopy (HSM) at first, then cocrystal phase was characterized using differential thermal analysis (DTA), powder X-ray diffractometry (PXRD), scanning electron microscopy (SEM), and fourier-transform infrared (FT-IR) spectroscopy. Solubility and dissolution test were conducted as well. DSC thermogram exhibits new endothermic peak at 280.32°C representing the melting point of cocrystal phase alongside with endothermic point of pure compounds. Powder X-ray diffractograms show new diffraction peaks on behalf of cocrystal formation at 2θ=8.92, 9.88, 13.04, 29.78, 35.35°. FT-IR spectroscopy reveals band shifting in –OH group region. On SEM photographs, one can observe crystal habit of succinic acid being covered by crystal with different habit. This indicates that quercetin interacts with succinic acid only on the surfaces and causes imperfect formation of cocrystal phase. Cocrystallization quercetin improves solubility by 1.62 times higher and dissolution rate by 1.25 higher than pure quercetin (one-way ANOVA, p < 0.05).


2018 ◽  
Vol 74 (11) ◽  
pp. 1390-1394 ◽  
Author(s):  
Rami Al-Oweini ◽  
Bassem S. Bassil ◽  
Marwa Itani ◽  
Dilara Börte Emiroğlu ◽  
Ulrich Kortz

Interaction of the mixed-valent 12-manganese coordination complex [MnIII 8MnIV 4O12(CH3COO)16(H2O)4] with the lacunary 9-tungstoarsenate(V) [A-α-AsW9O34]9− resulted in the 10-manganese(III/IV)-containing 36-tungsto-4-arsenate(V), [MnIII 6MnIV 4O4(OH)12(H2O)12(A-β-AsW9O34)4]22− (1). Polyanion 1 was isolated as a hydrated mixed potassium–sodium salt, K14Na8[MnIII 6MnIV 4O4(OH)12(H2O)12(A-β-AsW9O34)4]·104H2O, which crystallizes in the orthorhombic space group Pbcn and was characterized by FT–IR spectroscopy and single-crystal X-ray diffraction, as well as elemental and thermogravimetric analyses. The title polyanion contains a unique [MnIII 6MnIV 4O4(OH)12(H2O)12]14+ core stabilized within the 36-tungsto-4-arsenate(V) framework.


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