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One of the most widely used approaches for valorizing CO2, is to use organic halides with electrochemical techniques, which makes it possible to activate the CO2 (Scheme 1, Equations (1)–(4)); In a first step, a one electron transfer process generates the organic radical anion, which later converts to an anion though a second reduction electron transfer and a halide anion. The key to this approach relies on the reduction potential value of the organic halides and the stability of the organic anion C 2020, 6, 34 3 of 21 formed after the reduction process [51−65]. Scheme 1. Electrochemical strategies to valorize CO Scheme1.ElectrochemicalstrategiestovalorizeCO2.. One of the most common techniques to analyze electrocatalysis is cyclic voltammetry, which provides direct and rapid information regarding the relationship between driving force (i.e., overpotential) and catalytic turnover (i.e., current) compared to rather complicated alternative methods monitored by spectroscopy or other means. However, understanding detailed mechanistic schemes behind voltammograms is quite challenging due to complicated and intertwining processes, such as mass transport, electron transfer, chemical reaction and interfacial chemistry between electrode and reactants. In this sense, developing the foot of the wave analysis (FOWA) of cyclic voltammetry by Savéant and Costentin has provided a feasible method to benchmark molecular electrocatalysts by turnover frequency (TOF) and turnover number (TON) [92–96]. Molecular catalysts are an attractive option owing to the high degree of tunability of electronic and geometric parameters, which allows for systematic reactivity studies that can lead to new catalyst design guidelines. The well-defined structure of the catalytic sites also allows the establishment of a precise structural model for better analysis of the multiple proton-coupled electron transfer processes involved in CO2 reduction and better understanding of the CO2 reduction mechanism. For example, Leung et al. proposed a mechanism for CO production using Co-based porphyrins [97,98], where the [Co(P)–(CO2)]2− intermediate will be protonated to form [Co(P)–(COOH)]−. Later, it will decompose to provide CO. Koper and co-workers proposed a different mechanism [99], where the formation of the CO −, anion intermediate, will be protonated yielding to [Co(P)–(COOH)]0 intermediate. 2 Then, [Co(P)–(COOH)]0 will decompose to CO. Finally, Yao et al. proposed a pre-activation process to form a local proton source could facilitate CO2 reduction [100]. The electrocatalysts participates in an electron transfer reaction (on the electrode surface) and facilitates acceleration of a chemical reaction. Both electron transfer and chemical kinetics must be fast for an efficient electrocatalyst. In addition, an optimal electrocatalyst must display a good thermodynamic match between the redox potential (E0) for the electron transfer reaction and the chemical reaction that is being catalyzed (in this work; CO2 reduction). Chemical tuning of the electrocatalyst can optimize these factors. A general approach for an electrocatalytic system is given in Scheme 2. The electrocatalytic activity can be analyzed in terms of in cyclic voltammetry (CV). In a CV under a dry inert atmosphere, an electrocatalyst should show a reversible redox couple. Upon addition of the reagent which is catalyzed (i.e., CO2), the diffusion limited current should increase significantly, while the potential shifts anodically, and the reversibility in the return oxidation wave is lost due to the chemical reaction between reagent and electrocatalyst. Electrocatalyst offer critical solutions to lowering the overpotentials, improving selectivity, and increasing the reaction kinetics of carbon dioxide conversion [101]. There are a lot of different catalysts reported in literature, although most ofPDF Image | Electrochemical Tuning of CO2 Reactivity in Ionic Liquids
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