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—We fabricate and study experimentally a promising nanostructured composite adsorbent based on crystalline zeolite NaX. The adsorbent exhibits improved physical mechanical and adsorption properties and is intended for use in pressure swing adsorption systems. Fluoro derivatives of ethylene are found to be the most promising for creating the matrix of block-shaped composite adsorbent materials, since these ensure a mechanical strength and good adhesion between the matrix and incorporated adsorbent. We investigate the effects that the type, ratio of starting materials, and conditions of forming have on the adsorption and mechanical parameters of prepared composite adsorbents. The choice of materials for the adsorbent filler and polymer matrix used in synthesis of block-shaped sorption-active composite materials is substantiated. Studies of the adsorption parameters of prepared materials suggest that the film constituting the polymer (fluoroplastic) matrix, a base of our block-shaped adsorbents, is not continuous, which allows adsorbate molecules to penetrate the bulk of adsorbent. A comparative analysis establishes that the dynamic activity, as measured using water vapor, was 20 to 40% higher in our samples than in conventional commercial adsorbents of the NaX-V-1G type.