This paper examines a novel method of regenerating saturated activated carbon after adsorption of complex phenolic, polycyclic aromatic hydrocarbons with low energy consumption by using superheated water pretreatment combined with CO2 activation. The effects of the temperature of the superheated water, liquid–solid ratio, soaking time, activation temperature, activation time, and CO2 flow rate of regeneration and adsorption of coal-powdered activated carbon (CPAC) were studied. The results show that the adsorption capacity of iodine values on CPAC recovers to 102.25% of the fresh activated carbon, and the recovery rate is 79.8% under optimal experimental conditions. The adsorption model and adsorption kinetics of methylene blue on regenerated activated carbon (RAC) showed that the adsorption process was in accordance with the Langmuir model and the pseudo-second-order kinetics model. Furthermore, the internal diffusion process was the main controlling step. The surface properties, Brunauer-Emmett-Teller (BET) surface area, and pore size distribution were characterized by Fourier transform infrared spectroscopy (FT-IR) and BET, which show that the RAC possesses more oxygen-containing functional groups with a specific surface area of 763.39 m2 g−1 and a total pore volume of 0.3039 cm3 g−1. Micropores account for 79.8% and mesopores account for 20.2%.