Conventional circulating activated sludge techniques (CASS) are time consuming (72 h) and energy intensive, all of which greatly limits their use. Although advanced oxidation techniques (e.g., photocatalysis, photoelectrocatalysis UV/•OH, and Electro-Fenton) can reduce the treatment time by several hours, the slow generation and fast coupling of electron and hole make the low degradation efficiency. In this work, an intact route using a two-step strategy is developed to eliminate organic dyes from wastewater in only a few minutes. The electron and hole exhibit “fast generation and slow coupling” by using the new technique via electrolytic discharge plasma (EDP) combined with a core-shell structure Au@SiO2 nanocatalyst for [Rhodamine (RhB)/Eosin yellowish (EY)] dyes degradation in wastewater. Results demonstrate that the synergy of EDP and Au@SiO2 nanocatalyst enhances degradation kinetics, and it is effective in degrading different concentrations of RhB and EY dyes in the range of 50–1.5 mg/L. Then, the Au@SiO2 nanocatalyst (over 99%) and carbon impurities are filtered by a porous nanocomposite ultrafiltration membrane. Favorable contributions of the two-step strategy are further ascertained based on chemical oxygen demand (COD) and relative removal efficiency. This two-step strategy provides an unprecedented rapid approach for industrial wastewater treatment.
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