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Developing low-cost, high-efficiency catalysts for advanced oxidation processes remain a key issue for the degradation of organic pollutants. In this study, a novel FeCo 2 O 4 /rectorite composite was synthesized via a facile combustion process and employed to activate peroxymonosulfate (PMS) for dealing with atrazine (ATZ). The addition of rectorite could result in higher specific surface area, smaller pore size and more hydroxyl groups, which were beneficial to enrich pollutants to the adsorption sites and provide sufficient reactive sites. After meticulous evaluation, the degradation efficiency of FeCo 2 O 4 /rectorite composite towards ATZ exhibited improved PMS activation efficiency which was about 2.6 times than that of pure FeCo 2 O 4. Based on the characterization results, the sulfate radicals and hydroxyl radicals were considered to be the main free radicals which were involved into the circulation of Co(II)–Co(III)–Co(II) as well as the oxidation of ≡Fe(II), which was responsible for the remarkable catalytic efficiency. In addition, the chemical stability and superior catalytic performance of FeCo 2 O 4 /rectorite should also be attributed to the chemical combination between metal ions and the surface hydroxyl groups of rectorite. Overall, these findings are beneficial for understanding the mechanism of PMS activation by natural mineral-based catalysts and contributing to the practical application of sulfate-based technology for organic wastewater treatment. Image 1 • In situ growth of FeCo 2 O 4 on natural rectorite for PMS activation was achieved. • FeCo 2 O 4 /rectorite composite exhibited higher PMS activation efficiency than pure FeCo 2 O 4. • Hydroxyl groups of rectorite accelerated PMS activation significantly via combining with metal oxide. • Both OH• and SO 4 •− were identified as main reactive species. [ABSTRACT FROM AUTHOR]