Abstract: Driven by the goals of carbon peaking and neutrality, and the EU's ESG regulations, the activated carbon adsorption-recovery process has demonstrated increasing competitiveness due to its advantages in treating volatile organic compounds (VOCs) and recovering solvents, effectively reducing product carbon tariffs. This study utilized phenolic resin, hexamethylenetetramine, and ethanol to prepare phenolic resin-based spherical activated carbon (PSAC). It investigated the effect of temperature on the adsorption performance of PSAC using toluene and ethyl acetate as target VOCs. Additionally, a comparison was conducted with high-performance asphalt-based spherical activated carbon (BAC). The results indicated that the adsorption capacity of ethyl acetate reached its peak at 40 ℃, measuring 695.0 mg/g, while the optimal toluene adsorption capacity was achieved at 50 ℃, recorded at 450.3 mg/g. Yoon-Nelson, Thomas, and Adams-Bohart models all fit the adsorption penetration curve well. The pseudo-second-order kinetic model was found to be more suitable for simulating VOC adsorption than the pseudo-first-order model. PSAC exhibited a multi-level porous structure comprising macropores, mesopores, and micropores, with a concentrated micropore distribution. The adsorption capacity of PSAC was 101.4% of that of BAC. Meanwhile, PSAC had a higher VOCs adsorption rate (0.096 /min), lower diffusion resistance, and lower preparation cost (46 000 yuan/t). After 12 cycles, the adsorption performance of VOCs exceeded 80%. PSAC possessed significant commercial value and market competitiveness, which could support future reactor design and process applications, and provide a clear advantage in the face of carbon tariff challenges.