Water-assisted electrochemical fabrication of Cu/Cu 2 O nanoparticles in protic ionic liquid and their catalytic activit

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Water‑assisted electrochemical fabrication of Cu/Cu2O nanoparticles in protic ionic liquid and their catalytic activity in the synthesis of quinazolinones Akshay V. Bhujbal1 · Amol B. Raut1 · Bhalchandra M. Bhanage1 Received: 2 June 2020 / Accepted: 8 October 2020 © Akadémiai Kiadó, Budapest, Hungary 2020

Abstract The present study reports a simple protocol involving Cu/Cu2O nanoparticles synthesis via electrochemical deposition process in 1-methylpiperidinium trifluoromethane sulphonate [HmPip][OTf] protic ionic liquid. The phase and morphology of the prepared nanoparticles were examined using different characterization techniques such as XRD, XPS, FEG-SEM, TEM, EDX, and FT-IR. A highly efficient, ligand-free method was developed to synthesize quinazolinones from substituted 2-halobenzoic acids with amidines via microwave-assisted Cu/Cu2O nano-catalyst in ethylene glycol as a green solvent. Up to five cycles Cu/Cu2O nanoparticles show good recyclability without loss in its activity. Graphic abstract

Electronic supplementary material  The online version of this article (https​://doi.org/10.1007/s1114​ 4-020-01882​-w) contains supplementary material, which is available to authorized users. Extended author information available on the last page of the article

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Reaction Kinetics, Mechanisms and Catalysis

Keywords Cu/Cu2O nanoparticles · Electrodeposition · Ionic liquid · Quinazolinone synthesis

Introduction Operationally simple bottom-up approaches such as chemical vapor deposition, hydrothermal, solution synthesis method, surfactant-assisted route have been successfully employed for the synthesis of nanomaterials [1–7]. The shape and size of the nanomaterial are known to have substantial effects on their physical, chemical, and optical properties [8–11]. Therefore, it becomes crucial to discover and to supervise the growth mechanism that leads to a specific morphology and structure of nanomaterials. It has been well known that the size and shape of nanoparticles are the factors that can be governed by changing the temperature, reaction condition, capping agents, starting materials such as solvent, reducing agents, pH value, precursors [12–19]. Cuprous oxide (­Cu2O) is a p-type semiconductor with a direct bandgap value of 2.2 eV [20, 21]. ­Cu2O having potential applications in gas sensing, catalysis, dye degradation, solar energy conversion, CO oxidation, lithium-ion batteries, micro/ nanoelectronics, photoactivated water splitting, and antibacterial activity [22–29]. In the past decade, C ­ u2O nanomaterial with various morphologies has been successfully synthesized such as octahedral, pyramids, nanowires, nanospheres, nanocages, multi pods, hollow structures [30–38]. Zhou et al. demonstrated the multi-step synthesis of Cu/Cu2O nanoparticles through a solvent-thermal route in a stainless steel autoclave using N,N-dimethylformamide (DMF) as solvent [39]. However, as long reaction time (26 h), high temperature (180 °C), and two-step synthesis routes are the voids of this study. Salavati-Ni