Dry sedimentation sludge (DS) from the treatment of wastewater in the textile industry was utilized to obtain a carbocatalyst via a simple drying step. The DS was evaluated for its ability to activate peroxymonosulfate (PMS) to deal with pharmaceuticals in aqueous solutions. Also, a comprehensive characterization of the DS was performed using techniques including X-ray diffraction (XRD), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), elemental microanalysis (CHNS), X-ray fluorescence (XRF), and Fourier-transform infrared spectroscopy (FTIR). Initially, the ability of the DS + PMS system to degrade three pharmaceuticals (two antibiotics and one analgesic) in water was assessed. Ciprofloxacin (CIP), sulfamethoxazole (SMX), and diclofenac (DFC) were considered. Based on the first results, the antibiotic CIP was selected as a model pollutant. Thus, experiments investigated the effects of CIP concentration, DS dosage, PMS concentration, and pH. Under optimal conditions (1.0 g L−1 DS, 1.5 mM PMS, and neutral pH), the DS + PMS catalytic system demonstrated high antibiotic degradation, achieving a 71 % reduction in CIP concentration within 10 min. Mechanistic studies indicated that the degradation pathway followed a non-radical mechanism, primarily involving singlet oxygen (1O2). This was supported by scavenger tests and confirmed via electron paramagnetic resonance (EPR) spectroscopy, which detected the formation of the TEMP-1O2 adduct, providing direct evidence of 1O2 generation and its persistence over time. The system maintained its efficiency in complex matrices such as wastewater and urine, achieving high CIP removal (around 72 % in 10 min, for both matrices). Even after five reuse cycles, the DS retained over 45 % of CIP degradation capacity. Additionally, the DS + PMS system effectively eliminated antimicrobial activity against S. aureus and E. coli by transforming CIP into biologically inactive substances. Aligned with circular economy principles, this work offers a sustainable approach to valorizing industrial waste and repurposing it as a catalyst for the efficient removal of water pollutants. © 2025 Elsevier B.V.