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Electrocatalytic production of glycolic acid via oxalic acid reduction on titania debris supported on a TiO_(2)nanotube array

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Journal of Energy Chemistry 2022年第5期31卷 669-678页

作者： Francesco Pio Abramo Federica De Luca Rosalba Passalacqua Gabriele Centi gianfranco giorgianni Siglinda Perathoner Salvatore Abate Department of ChiBioFarAM(Industrial Chemistry) University of MessinaERIC aisbl and INSTM/CASPEV.le F.Stagno d’Alcontres 31Messina 98166Italy University of Calabria Department of Environmental EngineeringLaboratory of Industrial Chemistry and Catalysis Via P.Bucci87036 RendeCSItaly

Electrodes prepared by anodic oxidation of Ti foils are robust and not toxic materials for the electrocatalytic reduction of oxalic acid to glycolic acid, allowing the development of a renewable energy-driven process for producing an alcoholic compound from an organic acid at low potential and room temperature. Coupled with the electrochemical synthesis of the oxalic acid from CO_(2),this process represents a new green and low-carbon path to produce added value chemicals from CO_(2). Various electrodes prepared by anodic oxidation of Ti foils were investigated. They were characterized by the presence of a TiO_(2) nanotube array together with the presence of small patches, debris, or TiO_(2) nanoparticles. The concentration of oxygen vacancies, the amount of Ti^(3+) measured by X-ray photoelectron spectroscopy(XPS) and the intensity of the anodic peak measured by cyclic voltammetry, were positively correlated with the achieved oxalic acid conversion and glycolic acid yield. The analysis of the results indicates the presence of small amorphous TiO_(2) nanoparticles(or surface patches or debris) interacting with TiO_(2) nanotubes, the sites responsible for the conversion of oxalic acid and glycolic acid yield. By varying this structural characteristic of the electrodes, it is possible to tune the glycolic acid to glyoxylic acid relative ratio. A best cumulative Faradaic efficiency(FE) of about 84% with FE to glycolic acid around 60% and oxalic conversion about 30% was observed.

关键词： Oxalic acid TiO_(2)nanotubes Glyoxylic acid Glycolic acid Electrocatalysis

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Role of size and pretreatment of Pd particles on their behaviour in the direct synthesis of H_2O_2

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Journal of Energy Chemistry 2016年第2期25卷 295-303页

作者： Salvatore Abate Katia Barbera Gabriele Centi gianfranco giorgianni Siglinda Perathoner University of Messina ERIC aisbl and INSTMCASPE Section Industrial Chemistry

Two families of catalysts, based on Pd nanoparticles supported on ceramic asymmetric tubular alumina membranes, are studies in the direct synthesis of H2O2. They are prepared by depositing Pd in two ways：（i） reduction with N2H4 in an ultrasonic bath and（ii） by impregnation-deposition. The first preparation leads to larger particles, with average size of around 11 nm, while the second preparation leads to smaller particles, with average size around 4 nm. The catalytic membranes were tested as prepared, after thermal treatment in air and after further pre-reduction with H2 in mild（100 ℃） conditions. Samples were characterized by TEM, CO-chemisorption monitored by DRIFTS method and TPR, while catalytic tests have been performed in a semi-batch recirculation membrane reactor. Experimental catalytic results were analysed using two kinetics models to derive the reaction constants for the parallel and consecutive reactions of the kinetic network. Smaller particles of Pd show lower selectivity due to the higher rate of parallel combustion, even if the better dispersion of Pd and thus higher metal surface area in the sample lead to a productivity in H2O2 similar or even higher than the sample with the larger Pd particles. Independently on the presence of smaller or larger Pd nanoparticles, an oxidation treatment leads to a significant enhancement in the productivity, although the catalyst progressively reduces during the catalytic process. The inhibition of the parallel combustion reaction（to water） induced from the calcination treatment remains after the in-situ reduction of the oxidized Pd species formed during the *** is likely due to the elimination of defect sites which dissociatively activate oxygen, and tentatively attributed to Pd sites able to give three- and four-fold coordination of CO.

关键词： H2O2 direct synthesis Pd nanoparticles Kinetics of H2O2 synthesis Pd role in H2O2 synthesis

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