The current study presents synthesis and characterization of high impact polystyrene - TiO2 nanoparticles mixed matrix membranes for separation of carbon dioxide from nitrogen. The solution-casting method was used for preparation of membranes. The nano mixed matrix membranes were characterized using scanning electron microscopy to ensure the suitable dispersion of nano particles in high impact polystyrene matrix. The effect of TiO2 nanoparticles loading on membrane performance was investigated. The separation performance of synthesized membranes was investigated in separation of CO2 from CO2/N2 mixture. Effect of feed pressure and TiO2 content on separation of CO2 was studied. The results revealed that increase of feed pressure decreases flux of gases through the mixed matrix membrane. The results also confirmed that the best separation performance can be obtained at TiO2 nanoparticles loading of 7 wt.%.