The thermogravimetric data of the furfural and vanillin were measured from 30 ℃ to 350 ℃ at different heating rates of 10, 20, 40 ℃/min. Three non-isothermal thermal analysis methods of CR, KAS, and FWO were used to fit the heat release process of the furfural and vanillin. The heat release products of the furfural and vanillin were determined by tube furnace and GC. The results showed that the furfural had 2 weight loss stages and the vanillin had 1 weight loss stage. As the heating temperature increased from 30 ℃ to 350 ℃, the heat release characteristic index of the furfural increased from 2.54×10–3 to 3.19×10–2, and that of the vanillin increased from 3.21×10–4 to 5.63×10–3. The kinetic analysis based on multi-heating rate KAS and FWO showed that the activation energy of furfural was the highest at the conversion rate of 0.7, and that of the vanillin was the highest at the conversion rate of 0.8. The average activation energy of furfural and the vanillin obtained by KAS method was 86.26 kJ/mol and 84.89 kJ/mol, respectively. The average activation energies of furfural and vanillin obtained by FWO method were 88.72 kJ/mol and 89.09 kJ/mol, respectively. The kinetic analysis based on CR method shows that the thermogravimetric processes of furfural and vanillin can be well described by three-dimensional diffusion model of D3.