Abstract: A sixstep combined vacuum and temperature swing adsorption process（VTSA）was studied for CO2 capture from flue gas. Experiments under different regeneration conditions were investigated and the VTSA performance for CO2 separation was evaluated. Purity of CO2 from flue gas can be concentrated from 15.0% to 93.4% with a recovery of 95.4% under desorption at 10 kPa and 423 K. Simulations were also performed and the model was verified by the experimental results. Finally, a modified fivestep VTSA cycle without cooling step was also proposed to enhance the unit productivity.