Characterization of electrode fouling during electrochemical oxidation of phenolic pollutant

doi:10.1007/s11783-020-1345-7

Front. Environ. Sci. Eng.

2021, Vol. 15

Issue (4) : 53 https://doi.org/10.1007/s11783-020-1345-7

RESEARCH ARTICLE

Characterization of electrode fouling during electrochemical oxidation of phenolic pollutant

Xuefeng Liu¹, Shijie You¹(

), Fang Ma¹, Hao Zhou²

¹. State Key Laboratory of Urban Water Resource and Environment, Harbin Institute of Technology, Harbin 150090, China
². Conservation Center, Shanghai Museum, Shanghai 200231, China

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Abstract

• Electrode fouling is characterized by non-destructive characterization.

• Electrode fouling is highly dependent on electrochemical process.

• Active chlorine can prevent the formation of polymeric fouling film.

Electrode fouling is a problem that commonly occurs during electro-oxidation water purification. This study focused on identifying the fouling behavior of Pt electrode associated with the formation of polymeric layer during electro-oxidation of phenol. The in situ electrochemical measurements and non-destructive observation of the electrode morphology were reported. The results demonstrated that the electrode fouling was highly dependent on thermodynamic process of electrode that was controlled by anode potential. At anode potential lower than 1.0 V vs SHE, the direct electro-oxidation caused the electrode fouling by the formation of polymeric film. The fouling layer decreased the electrochemically active surface area from 8.38 cm² to 1.57 cm², indicated by the formation of polymeric film with thickness of 2.3 mm, increase in mass growing at a rate of 3.26 μg/cm²/min. The degree to which the anode was fouled was independent of anion in the electrolyte. In comparison, at anode potential higher than 2.7 V vs SHE, the anions (e.g., chloride) could exert a major influence to the behavior of electrode fouling. The presence of chloride was shown to mitigate the fouling of electrode significantly through preventing the formation of polymeric film by active chlorine (e.g., Cl• and Cl₂) produced from anodic oxidation of chloride. Since chloride is the most abundant anionic species existing in both natural and engineered water system, this study not only offers a deep insight into the mechanism of electrode fouling, but also suggests strategies for anti-fouling in the presence of chloride in electro-oxidation process.

Keywords Electro-oxidation Electrode fouling Polymeric film Chloride ions

Corresponding Author(s): Shijie You

Issue Date: 15 October 2020

Cite this article:

Xuefeng Liu,Shijie You,Fang Ma, et al. Characterization of electrode fouling during electrochemical oxidation of phenolic pollutant[J]. Front. Environ. Sci. Eng., 2021, 15(4): 53.

URL:

https://academic.hep.com.cn/fese/EN/10.1007/s11783-020-1345-7
https://academic.hep.com.cn/fese/EN/Y2021/V15/I4/53

Fig.1 (a) Square wave voltammetry (SWV) measurements in the presence and absence of 2.0 mmol/L phenol in 0.1 mol/L NaCl supporting electrolyte at pH 6.8±0.5. (b) Cyclic voltammograms (CV) curves of pristine (red line) and fouled (blue line, inset) flat Pt electrode for ECSA measurement in 0.5 mol/L H₂SO₄ supporting electrolyte. (c) Typical chronoamperometric response of Pt electrode to step-by-step injection of phenol containing with 0.1 mol/L NaCl (pH 6.8±0.5) at 1.0 V vs SHE. (d) Nyquist plots of Pt electrode after electrolysis with 2.0 mmol/L phenol in 0.1 mol/L NaCl (pH 6.8±0.5) at 1.0 V vs SHE.

Tab.1 Parameters used for fitting the impedance results for the Pt electrodes

Fig.2 (a) CV curves and (b) mass change during CV test for 2.0 mmol/L phenol in 0.1 mol/L NaCl supporting electrolyte. (c) Mass change of Pt electrode during electrolysis of 2.0 mmol/L phenol in 0.1 mol/L NaCl at 1.0 V vs SHE. (d) Schematic illustration of concentration profile of phenol close to the electrode surface.

Fig.3 Time course of 3D topographies of Pt electrode surface and surface height curves during electrolysis of 2.0 mmol/L phenol in 0.1 mol/L NaCl electrolyte at 1.0 V vs SHE within 100 min.

Fig.4 FTIR spectra during electrolysis of 2.0 mmol/L phenol in 0.1 mol/L NaCl electrolyte at 1.0 V vs SHE within 100 min.

Fig.5 Chronoamperometric response of Pt electrode to step-by-step injection of phenol at 2.7 V vs SHE in (a) 0.1 mol/L NaCl and (b) 0.1 mol/L Na₂SO₄. Nyquist plots of Pt electrode after electrolysis of 2.0 mmol/L phenol in (c) 0.1 mol/L NaCl and (d) 0.1 mol/L Na₂SO₄ at 2.7 V vs SHE.

Fig.6 High-resolution XPS spectra of (a) pristine and (b) fouled Pt electrode, and (c) Cl 2p after electrolysis of 2.0 mmol/L phenol in 0.1 mol/L NaCl electrolyte at 2.7 V vs SHE. (d) ESR spectra with DMPO serving as trapping agent after 10 min electrolysis.

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