The advanced oxidation processes (AOPs) play an important role in the degradation of hardly decomposable organic pollutants. AOPs methods rely on the production of highly reactive hydroxyl OH• radicals. The aim of the conducted research was to intensify biogas production in the methane fermentation process of excess sludge subjected to the process of deep oxidation with Fenton's reagent. In the process of oxidation of sewage sludge with the Fenton reagent, doses of iron ions in the range 0.02–0.14 g Fe2+/g TS (total solids) were used Hydrogen peroxide was measured in the proportions 1: 1–1:10 in relation to the mass of iron ions. The basic substrate of the study was excess sludge. In the case of excess sludge oxidation with the use of Fenton's reagent, the most favorable process conditions were considered to be the dose of iron ions 0.08 g Fe2+/g d.m. and a Fe2+: H2O2 ratio of 1:5. As a result of subjecting the excess sludge to disintegration with the Fenton reagent in the above-mentioned dose, with respect to the fermentation process of unprocessed sludge, about two-fold increase in the digestion degree of excess sludge and about 35% increase of the biogas yield was obtained.