The conventional open ponding system employed for palm oil mill agro-effluent (POME) treatment fails to lower the levels of organic pollutants to the mandatory standard discharge limits. In this work, carbon doped black TiO₂ (CB-TiO₂) and carbon-nitrogen co-doped black TiO₂ (CNB-TiO₂) were synthesized via glycerol assisted sol-gel techniques and employed for the remediation of treated palm oil mill effluent (TPOME). Both the samples were anatase phase, with a crystallite size of 11.09–22.18 nm, lower bandgap of 2.06–2.63 eV, superior visible light absorption ability, and a high surface area of 239.99–347.26 m²/g. The performance of CNB-TiO₂ was higher (51.48%) compared to only (45.72%) CB-TiO₂. Thus, the CNB-TiO₂ is employed in sonophotocatalytic reactions. Sonophotocatalytic process based on CNB-TiO₂, assisted by hydrogen peroxide (H₂O₂), and operated at an ultrasonication (US) frequency of 30 kHz and 40 W power under visible light irradiation proved to be the most efficient for chemical oxygen demand (COD) removal. More than 90% of COD was removed within 60 min of sonophotocatalytic reaction, producing the effluent with the COD concentration well below the stipulated permissible limit of 50 mg/L. The electrical energy required per order of magnitude was estimated to be only 177.59 kWh/m³, indicating extreme viability of the proposed process for the remediation of TPOME.

The release of phenolic-contaminated treated palm oil mill effluent (TPOME) poses a severe threat to human and environmental health. In this work, manganese-modified black TiO₂ (Mn-B-TiO₂) was produced for the photodegradation of high concentrations of total phenolic compounds from TPOME. A modified glycerol-assisted technique was used to synthesize visible-light-sensitive black TiO₂ nanoparticles (NPs), which were then calcined at 300 °C for 60 min for conversion to anatase crystalline phase. The black TiO₂ was further modified with manganese by utilizing a wet impregnation technique. Visible light absorption, charge carrier separation, and electron–hole pair recombination suppression were all improved when the band structure of TiO₂ was tuned by producing Ti³⁺ defect states. As a result of the enhanced optical and electrical characteristics of black TiO₂ NPs, phenolic compounds were removed from TPOME at a rate of 48.17%, which is 2.6 times higher than P25 (18%). When Mn was added to black TiO₂ NPs, the Ti ion in the TiO₂ lattice was replaced by Mn, causing a large redshift of the optical absorption edges and enhanced photodegradation of phenolic compounds from TPOME. The photodegradation efficiency of phenolic compounds by Mn-B-TiO₂ improved to 60.12% from 48.17% at 0.3 wt% Mn doping concentration. The removal efficiency of phenolic compounds from TPOME diminished when Mn doping exceeded the optimum threshold (0.3 wt%). According to the findings, Mn-modified black TiO₂ NPs are the most effective, as they combine the advantages of both black TiO₂ and Mn doping.