Abstract: The thermogravimetric, pyrolysis behavior and pyrolytic products of coconut shells meal were analyzed by thermogravimetry-Fourier transform infrared spectroscopy(TG-FTIR) and pyrolysis-gas chromatography and mass spectrometry(Py-GC-MS). Three-dimensional infrared spectroscopy was used to detect the gas products in the pyrolysis process, based on the analysis of TG and DTG curves under N₂/air atmosphere. The results showed that the maximum weight loss peak temperature(T_m) was 347.8℃, and the residual was 32.0%, CO₂ was the main gas product under the N₂ atmosphere. The solid residual was only 6.5%, and T_m was 282.1℃, and the released gas were CO₂, CO, H₂O and CH₄, under the air atmosphere.Py-GC-MS results showed that phenolic compounds were the main products. There were 39 pyrolysis products, among which 12 kinds of products were phenolic compounds (GC content 40.0%) at the temperature 400℃. There were 56 pyrolysis products, among which 18 kinds of products were phenolic compounds (GC content 45.8%) at the temperature 700℃.