A temperature pressure swing adsorption (TPSA) system was developed to purify and recover the unreacted vinyl chloride (VCM) in a polyvinyl chloride (PVC) plant. A literature review on adsorbent materials was performed for the adsorption equilibrium separation of VCM and nitrogen (N-2). Using a one-dimensional (1D) mathematical model, a 7-step, 2-column TPSA system was designed to treat an industrial scale 40/60% (v/v) VCM/N-2 mixture. This system was designed to produce a 95% (v/v) VCM rich stream and a N-2 stream with a VCM content not higher than 8 ppm (w/w). This process showed a VCM productivity of 0.46 mol/kg(ads).h and an energy consumption of 3.62 MJ/kg(VCM). The obtained VCM stream can be directly recycled to the polymerization reactor, while the inert stream can be safely released to the atmosphere. A process comparison and optimization was performed to study the effects of the steps configuration and duration on the system performance.