In this study, the combined process of phenolic condensation-persulfate(PS) advanced oxidation was adopted to treat semi-coking wastewater. Using the phenolic condensation method as a pretreatment unit to remove phenolic substances for the preparation of phenol-formaldehyde resins, and using an aerated/PS/pyrite oxidation system as a deep treatment unit to remove chemical oxygen demand (COD) and ammonia nitrogen (NH3-N) from the wastewater. Analysis and characterization of phenol-formaldehyde resin, organic compounds in wastewater, and pyrite using FT-IR, TG-DTG, GC-MS, and XPS techniques. The results showed that under the conditions of adding 1.8vt % formaldehyde, pH 10.5, reaction temperature 95 ℃ and reaction time 3 h, the removal rates of volatile phenol, COD and NH3-N in semi-coke wastewater were 97.54 %, 41.14 % and 56.50 %, and the yield of phenolic resin was 6.62 g/L. Subsequently, treated with an aerated/PS/pyrite system, the PS concentration 0.4 mol/L, the pyrite dosage 15 g/L, the pH 3, the temperature 65 ℃, and the aeration 3 h, the removal rates of COD and NH3-N are 99.20 % and 86.80 %. In the phenolic condensation process, phenolic substances in semi-coke wastewater generate phenoxy anions under the influence of OH-, which undergo addition reactions with formaldehyde to produce hydroxymethyl phenol. Hydroxymethyl phenol further undergoes condensation reactions with other phenolic substances and itself to form phenolic resin, while amide compounds are generated through reactions between ammonia nitrogen and carboxylic acid substances. In the aeration/PS/pyrite system, Fe2+ released from pyrite oxidation activates PS to produce SO4•− and O2•−. The contribution of free radical oxidation and decomposition of pollutants such as phenols, amides, and NH3-N in wastewater is 84.60 %. Specifically, SO4•− oxidation contributes 61.54 %, while O2•− accounts for 22.21 %. Amide compounds and phenolic substances in the wastewater are oxidized, leading to ring opening and chain scission, resulting in the formation of alkane compounds.
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