The electrochemical degradation of 4-chlorophenol and its main by-products was investigated in acid medium using binary oxides electrodes of nominal composition Ti/Ru 0.3 Ti 0.7 O 2 and Ti/Ru 0.3 Sn 0.7 O 2 prepared by thermal decomposition through two different routes: inorganic precursors dissolved in isopropanol and polymeric precursors (PPM). The aim of this study was to investigate the influence of both the composition and preparation methodology of these electrodes in the electrooxidation of the organic pollutants 4-chlorophenol and its by-products. Electrolyses were carried out using a filter press-type flow cell and monitored by high performance liquid chromatography (HPLC), total organic carbon (TOC), and chloride analyses. Besides CO 2 , the by-products formed in the reactions were 1,4-benzoquinone, 4-chlorocatechol, and hydroquinone, as well as oxalic, maleic, malic, malonic, and succinic acids. The electrocatalytic efficiency with respect to the degradation of by-products was evaluated through the electrooxidation of 1,4-benzoquinone and oxalic acid (OA).The anodes investigated in this work are very promising for the degradation of pollutants because of their excellent efficiency concerning the consumption of 4-chlorophenol and its by-products, although the mineralization of the starting material is not complete. The cleavage of the aromatic ring occurs preferentially in the case of electrodes prepared by decomposition of inorganic precursors due to their larger electrochemically active area and electrocatalytic activity for oxygen evolution reaction (OER). However, OA oxidation is favored on Ti/Ru 0.3 Sn 0.7 O 2 prepared through decomposition of PPM.
Ânodos contendo óxidos de rutênio, titânio e estanho suportados em Ti metálico foram preparados por decomposição térmica para investigar o efeito do solvente (HCl/H 2 O e isopropanol) na composição real de eletrodos de óxidos. As soluções precursoras e suas misturas foram analisadas por Espectrofotometria UV-Vis. A morfologia e a composição dos recobrimentos foram analisadas por Microscopia Eletrônica de Varredura (MEV) e Energia Dispersiva de raios X (EDX). A área eletroquimicamente ativa e a estabilidade dos eletrodos foram estabelecidas por meio da caracterização voltamétrica (HClO 4 1,0 mol L -1 ) e testes de vida útil, respectivamente. Os resultados mostram que a composição e a morfologia dos recobrimentos variam drasticamente em função do solvente. Eletrodos preparados a partir de isopropanol apresentam excelente concordância entre as composições nominais e as experimentais, maior área eletroquimicamente ativa e excelente estabilidade quando comparados àqueles que utilizaram HCl. A preparação das misturas precursoras em isopropanol aumenta o tempo de vida dos eletrodos RuO 2 -TiO 2 -SnO 2 .Anodes containing ruthenium, titanium, and tin oxides supported on metallic Ti were prepared by thermal decomposition of precursor salts in order to investigate the effect that changing the solvent (from HCl/H 2 O to isopropanol) would have on the real composition of the mixed oxide electrodes. The precursor solutions and their mixtures were analyzed by UVVis Spectrophotometry. Coatings morphology and composition were analyzed by Scanning Electronic Microscopy (SEM) and Energy Dispersive X-ray (EDX). Determination of the electrochemically active area and electrode stability was performed by voltammetric characterization (1.0 mol L -1 HClO 4 ) and service life (SL) tests, respectively. Electrodes prepared from isopropanol showed excellent agreement between the nominal and experimental composition and they presented higher electrochemically active area and better stability when compared to those prepared in the presence of HCl. Preparation of the precursor mixture in isopropanol increases RuO 2 -TiO 2 -SnO 2 electrodes service life.
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