Abstract Mechanochemical treatment causes the formation of mineral Cl compounds during the degradation of polychlorinated compounds by planetary ball mill. In the present study, the three types of industrial waste comprising of sludge from petrochemical wastewater treatment plants as source of pollutants, scrap iron and petrochemical water treatment plant sludge as co‐milling reagents were used. The raw samples and the milled products were analyzed by gas chromatography–mass spectrometry, Fourier transform infrared spectroscopy, Raman Spectroscopy, and X‐ray diffraction. Further analyses such as ion chromatography and X‐ray fluorescence were performed. The analysis results confirmed that the milling process degraded persistent organic pollutants and showed that major changes occurred in the organic phases, carbon and chlorine bonds. The yield of chloride ions was investigated using Ion Chromatography. The highest percentage of de‐Cl products (95.6%) was achieved after 6?h in equal proportions of reagents. Furthermore, CaCl2 and FeCl2 were present in the final milling product.
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