Abstract: Driven by the goals of carbon peaking, carbon 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. The phenolic resin, hexamethylenetetramine, and ethanol are utilized to prepare phenolic resin-based activated carbon (PSAC). This study investigates 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 indicate that the adsorption capacity of ethyl acetate reaches its peak at 40 °C, measuring 695.0 mg/g, while the optimal toluene adsorption capacity is achieved at 50 °C, recorded at 450.3 mg/g. The Yoon-Nelson, Thomas, and Adams-Bohart models all fit the adsorption penetration curve well. The pseudo-second-order kinetic model is found to be more suitable for simulating VOC adsorption than the pseudo-first-order model. PSAC exhibits a multi-level porous structure comprising macropores, mesopores, and micropores, with a concentrated micropore distribution. The adsorption capacity of PSAC is 101.4% of that of BAC. Meanwhile, PSAC has a higher VOCs adsorption rate (0.096 min^-1), lower diffusion resistance, and lower preparation cost (46,000 yuan/ton). After 12 cycles, the adsorption performance of VOCs exceeds 80%. PSAC possesses significant commercial value and market competitiveness, supporting future reactor design and process applications, and providing a clear advantage in the face of carbon tariff challenges.