Transitional metal oxides are excellent candidates as heterogeneous catalysts for activating persulfate towards organics degradation. In this study, MnCo2O4 spinel was successfully prepared using a solvent-free molten method. The catalytic performance was systematically investigated and MnCo2O4 powder catalyst was successfully immobilized on polyurethane (PU) membrane through electrospinning to assess its application potential. The results showed that peroxymonosulfate (0.1 g L−1) activated by MnCo2O4 (0.1 g L−1) reached 99.92 % degradation in 10 min when treating 0.04 g L−1 rhodamine B as target pollutant. The abundant oxygen vacancies formation, synergistic effect of Co and Mn ions and high electron transfer mobility are contributing to production of reactive oxygen species. Combining with quenching experiment and time-resolved EPR, the contribution of various active species was proposed, of which 1O2 exhibited the dominant role. The flowing reaction run by the MnCo2O4-PU membrane activating PMS exhibited universal degradation on different target pollutants.