Chitosan-lead (CS-Pb) carbon aerogels were prepared by ionic cross-linking and high-temperature carbonization using chitosan (CS) as the carbon precursor. The obtained carbon aerogels were characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD), and X-ray photoelectron spectroscopy (XPS). The obtained aerogels have a 3D structure and a large surface area, which can effectively prevent the agglomeration phenomenon of metals. Differential thermal analysis (DTA) was used to analyze the catalytic performance of a carbon aerogel for ammonium perchlorate (AP). The results showed that the CS-Pb carbon aerogel reduced the peak temperature of AP pyrolysis from 703.9 to 627.7 K. According to the Kissinger method calculations, the Ea of AP decomposition decreased about 27.2 kJ/mol. The TG data at different warming rates were analyzed by the Flynne-Walle-Ozawa (FWO) and Kissinger-Akahira-Sunose (KAS) methods, which are two of the isoconversion methods, and the activation energies of AP and AP+CS-Pb-3.5 were calculated. Between the conversion degrees (α) of 0.1 and 0.9, the Ea values obtained by the two isoconversion methods are similar and have a certain match. Also, the two isoconversion methods confirm Kissinger's calculation. Finally, thermogravimetry-mass spectrometry (TG-MS) was used to monitor the gases generated during the thermal decomposition of the AP+CS-Pb-3.5 system in real time.