Self-prepared beaded activated carbons (SBAC) were derived from carbonized phenolic formaldehyde (PF) resins through an optimal activation procedure (900 o C for 4 h) using CO 2 . A commercial BAC (termed KBAC) was adopted to compare with SBAC over physicochemical properties, adsorption performance against methyl ethyl ketone (MEK) and toluene (TOL), and the regenerability using microwave irradiation. Langmuir, Freundlich, and Dubinin-Radushkevich (D-R) isotherm models showed good fitting results to explain the adsorption equilibrium. The isosteric heat of adsorption was calculated using the Clausius-Clapeyron equation; the parameters obtained from the D-R isotherm indicate that the interactions between adsorbate and adsorbent were mainly due to physisorption. Microwave heating was applied to the regeneration of saturated adsorbents to examine the effect of irradiation power and heating time on the desorption behavior of adsorbate. Within 12 min of microwave irradiation, excellent desorption efficiencies based on gravimetric method were shown, reaching 110.7 ± 14.4, 104.4 ± 2.6, 90.2 ± 2.3, and 85.5 ± 5.7% for MEK-SBAC, MEK-KBAC, TOL-SBAC, and TOL-KBAC, respectively. After an 8-cycle of adsorption/regeneration, the adsorption capacity for SBAC was significantly decreased when loaded with TOL, whereas it was more significant than the virgin sample as loaded with MEK. In contrast, KBAC was able to sustain the adsorption capacity after an 8-cycle of regeneration, proving its stability throughout the microwave heating. Kinetic models were further employed to illustrate the desorption of the adsorbates from BAC samples, showing that intraparticle diffusion in SBAC and KBAC was the rate-limiting step during microwave heating. The core kinetic parameters obtained could provide insights for lab-scale adsorbent beds or practical engineering scale design. In conclusion, this study demonstrates the excellent adsorption performance of SBAC and the feasibility of microwave regeneration of BACs.