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Sludge residue (SLR), straw residue (STR) and vinegar residue (VR) combined with food waste and cattle manure were used as composting substance, respectively. The dynamics of enzymatic activity during composting, including dehydrogenase, urease, polyphenol oxidase and cellulase activity, and the change of humic acid composition (HA, FA) before and after composting were monitored and analyzed. The results showed that the activities of dehydrogenase and urease in the composting process of STR were increased first and then decreased with composting, and the polyphenol oxidase and cellulase activity were higher, which accelerated the decomposition and humification of organic matter. Compared with STR and VR, the dehydrogenase and urease activities of SLR remained high at the end of composting, which were 19.25μg/(g·h) and 6.22mg/(g·d), respectively, indicating that there was some unstable organic matter. After 30 days of composting, STR presented the highest degree of humification in compost, humification ratio (HR), humification index (HI), degree of polymerization (DP) and percentage of HA (PHA) was 28.89%, 19.24%, 1.99 and 66.60%, respectively. The molecular weights of humic acid were changed from 2.024Da, 3.284Da and 2.090Da before composting to 2.061Da, 3.929Da and 3.990Da after composting. Compost was used for different purposes depending on the molecular weight of humic acid. Therefore, based on multivariate parameter characterization of different residues, it provided a theoretical basis for efficient resource utilization of biogas residue and its product application.