The electrochemical behaviour of Cu(II)/Cu(I) redox couple in 1-hexyl-3-methylimidazolium chloride (C 6 mimCl) ionic liquid was studied using glassy carbon electrode at 375 K by cyclic voltammetry, chronopotentiometry and electrochemical impedance spectroscopy. In this electrochemical study, we have made an attempt to avoid the problem of water contamination in hygroscopic C 6 mimCl ionic liquid by setting the temperature at 375 K without glove box. This high temperature cyclic voltammetric study revealed two-step one electron reductions of Cu(II) to Cu(I) followed by Cu(I) to Cu metal. The reduction of Cu(II) to Cu(I) was found to be quasi-reversible at 375 K. The diffusion coefficients of Cu(II) and Cu(I), and the charge transfer rate constant of Cu(II) in C 6 mimCl were estimated by Randles-Ševčik equation and Nicholson's method, respectively, and found to be consistent with the quasi-reversible process. Further, constant potential electrodeposition of metallic copper was carried out on a stainless steel electrode at 375 K and the deposit was characterised by X-ray diffraction and electron microscopy.
A series of Keggin-based ionic liquids are synthesized by reacting in situ generated first-row transition-metal ion (Mn 2+ , Fe 3+ , Co 2+ , Ni 2+ , Cu 2+ , and Zn 2+ ) substituted monolacunary Keggin with tetraoctylammonium (TOA) cations. These ionic liquids contain highly charged bulky anions and are found to be hydrophobic, thermoreversible, and self-healing with melting temperatures less than 100 °C. The ionic liquids are characterized by Fourier transform infrared, Raman, X-ray diffraction, scanning electron microscopy, thermogravimetric analysis, differential scanning calorimetry, NMR, electron paramagnetic resonance, X-ray photoelectron spectroscopy, and UV−vis spectroscopic techniques. These ionic liquids show flakelike microscopic morphology and possess lamellar structure packed with Keggin and TOA cation layers alternately at room temperature. They contain highly charged anionic oxide clusters of size ∼1 nm and are excellent hydrophobic solvents for the removal of Cd 2+ and Pb 2+ metal ions.
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