Abstract: To provide resource utilization approaches for polluted substrates such as excess sludge, lake bottom silt and black and odorous river sediment, this study takes excess sludge as an example and explores the effect of combined pretreatment of the two on promoting acid production from excess sludge through experiments with different dosages of sodium percarbonate (SPC) and ammonium persulfate (APS). The results showed that production of short-chain fatty acids (SCFAs) was the highest in the SPC₁-APS₃ group (2027.86 mg COD/L), while it was only 157.18 mg COD/L in the control group. Three-dimensional fluorescence spectroscopy results showed that the SPC₁-APS₃ group demonstrated superior extracellular polymer stripping and sludge lysis efficiency. Meanwhile, this experimental group achieved enrichment of acid-producing functional bacterial communities during anaerobic fermentation, with Firmicutes accounting for 22.09%, among which the main acid-producing bacterial genus Clostridium accounted for 15.94%. This study provides a universal strategy for the efficient resource utilization of polluted substrates such as lake bottom silt and black-odorous river sediment with similar high organic matter content and refractory characteristics.