In this paper, a new generic synthesis route for the single-step production of adsorbent hollow fibres, based on polymer dry/wet spinning followed by a phase inversion process, is presented. This main advantage of this preparation technique is that it avoids impregnation of precursors or the use of chemicals for zeolite deposition, while dramatically reducing production times and costs. Primary factors (polymer, solvent and temperature) affecting the structure and adsorption performance of adsorbent hollow fibres are studied. The adsorptive properties of HiSiv 3000 hollow fibres and their commercial particulate counterpart have been obtained in a laboratory-scale flow system using n-butane as the adsorbate. The fibres prepared from solvents such as N, N-dimethylformamide, N, N-dimethylacetamide and 1-methyl-2-pyrrolidone (NMP) and from three types of polymers, namely, polysulfone, polyethersulfone (PESF) and polyvinylidenefluoride, are compared. The adsorbent hollow fibre prepared from NMP/PESF gave the s...