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aonxoidiacticoonunotferthsecaonx,aalatneewanoioxnidgateinoenrapteadkinwatsheobCsOer2veredduatct0io.4n5 pVr,ocwehssichuncdoerreaspsoantdueradtetdo tChOe2 oaxtimdaotsiopnheoref [t4h3e] (oSxcahlaemteea3n)i.oNnogtentheraatttehde ipneatkhseaCt Ohi2ghredruocxtiidoantiopnropcoestesnutinadl evralauesactuorraetsepdonCdOe2d atomtohsephoexrieda[4ti3o]n(Socfhieomdied3e).aNndotteritihoadtidthee, rpeesapkesctaivt ehliyg.hDeruoextiodathtieonlopwotoenxitdialtivoanlupeostceonrtriaelspvoanludedof tosiltvher,oixtiwdatsionotopf oiosdsiibdle taondrectroirioddaindye,arneosdpeictciovuelnyt.erDsuceantosothaes ltowdeotxeicdt athtieonaptoutrenotifatlhveaaluneioonfic siplvroedr,uicttws faosrnmoetdp.ossible to record any anodic counter scan so as to detect the nature of the anionic Catalysts 2019, 9, 413 6 of 12 products formed. Figure 4. Cyclic voltammograms of 5 mL solution in DMF/0.10 M TBABF4 containing 10.2 mM 4- Figure 4. Cyclic voltammograms of 5 mL solution in DMF/0.10 M TBABF4 containing 10.2 mM Fiogduorebe4n.zCoyncitlricilevoulntadmermaongirtarmogsenofa5tmmoLspshoelruetiaondinCOD2MaFtm/0o.1s0phMereTBuAsiBnFg4 (cao)nGtaCinaingd 1(b0.)2AmgM. Sc4a-n 4-iodobenzonitrile under a nitrogen atmosphere and CO2 atmosphere using (a) GC and (b) Ag. −1. iordatoeb0e.n5zVonsitrile−u1n.deranitrogenatmosphereandCO2 atmosphereusing(a)GCand(b)Ag.Scan Scan rate 0.5 V s rate 0.5 V s−1. Scheme 3. Mechanism proposal for the electrochemical reduction of 1 using a GC electrode under a Scheme 3. Mechanism proposal for the electrochemical reduction of 1 using a GC electrode under a CO2 atmosphere. SCchOe2maetm3o. sMpehcehrea.nism proposal for the electrochemical reduction of 1 using a GC electrode under a CO2 atmosphere. The CV of 1 at the silver cathode under a CO2 atmosphere in DMF showed three reduction peaks at −2.23 V, −2.09, and −2.40 V vs. SCE. The first and third peaks corresponded to the electrochemical reduction of 1 and benzonitrile, respectively. The second peak corresponded to the electrochemical reduction of CO2. This assignment of the second reduction peak to the electrochemical reduction of CO2 can be confirmed since the peak current value was directly linked to the CO2 concentration, as it can be seen in Figure 4b. In the case of using silver as a working electrode, the electrochemical processes and their associated reactivity were easily controlled by the applied potential. Note that in this case, since the electrochemical reduction of CO2 occurred prior to the benzonitrile reduction, no electrocatalytic processes were observed related to the role of benzonitrile as a redox mediator (Scheme 4). The same general electrochemical trend was observed when DMF was replaced by [PP13]TFSI under a N2 and a CO2 atmosphere at the GC and silver electrodes. However, when using [EMIM]TFSI, the electrochemical reduction of benzonitrile was not detected in any of the cases due to the fact that the reduction of the imidazolium cation appeared at less negative potentials either in inert or CO2 atmospheres [44].PDF Image | Electrocatalytic Processes for the Valorization of CO2
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