Cunninghamia lanceolata has been the dominated species of plantation forest in South China. And thermoplasticization can decreases the hydroscopicity to increase the additional value of Cunninghamia lanceolata biomass. However, many heat release volatiles would produce air pollution during thermoplasticization process. Therefore, the heat release behavior of Cunninghamia lanceolata biomass was studied by TD-GC/MS to make full use of and prevent the pollution of the volatile materials. The main constituents were cedrol(34.34%), phenol, 2,4-bis(1,1-dimethylethyl)( 11.49%), acetic acid(6.83%), carbon disulfide(3.1%), etc at 150°С. And the main constituents were acetic acid(20.22%), cedrol(17.20%), 1h-3a,7-methanoazulene, 2,3,4,7,8, 8a-hexahydro-3,6,8,8-tetramethyl-(3.58%), benzofuran, 2,3-dihydro-(3.26%), etc at 180°С. The heat release volatiles of Cunninghamia lanceolata biomass might be used as raw materials of bioenergy, rare biomedicines, and so on. Particularly, the volatiles had good application prospects and popularized value in purification of cedrol and acetic acid.