Based on the global goals for cleaner production and sustainable development, the pyrolysis behavior of cephalosporin residues was studied by TG-MS method. The influence of full temperature window on the safe disposal of residues was analyzed based on the “3-2-2” and “1+1” of thermal analysis kinetics, and the gas by-products of thermal degradation were monitored. Results showed that the pyrolysis of distillation residues were divided into low and high-temperature zones, including six stages. Maximum error rate (8.55%) by multiple scan rate was presented based on “3-2-2” pattern and maximum total fluctuation (33.7) by single scan rate was presented based on “1+1” pattern, which implied that the comprehensive multi-level comparison method was very reliable. The