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Pebax copolymers produced by Arkema are widely employed for different applications, including active molecular carriers and membranes for gas separation. In the present work, a new modification approach for Pebax®2533 is presented, along with the characterization of the newly obtained materials. Pebax was modified by grafting, through a nucleophilic acyl substitution, a benzoyl group on Polyamide12 block. The yield of the reaction was confirmed by FTIR and NMR analysis, while thermal DSC and TGA characterizations were then carried out on the polymeric products characterized by different degrees of substitution to understand their properties. Finally, self-standing films were obtained by casting and gas permeation tests were conducted at 35 °C using CO2, N2, CH4, O2 and He, in order to understand the potentiality of the new material as membrane for gas separation. DSC showed that in the modified Pebax, named “Benzoyl-P2533” (BP2533), the crystalline phase of the Nylon block was canceled, as expected, but at the same time the degree of crystallinity of the block of Polytetramethyleneoxide increased from 19%, measured for the unmodified Pebax, to a max of 35% for the fully substituted material. For this reason, gas permeability showed small but consistent increment, in the order of 10–11% for most of the gas tested, with the only exception being helium, where the increment resulted to be around 48%. As a consequence, the overall selectivity of CO2 against helium dropped with respect to pristine Pebax. For all the other gases, on the other hand the selectivity with respect to CO2 remained substantially constant, resulting in slight but neat improvement of the ability of the new material to separate this gas.