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Microporous materials have a great importance in catalysis, delivery, storage and separation in terms of their performance and efficiency. Most microporous materials are comprised of inorganic frameworks, while thermally rearranged (TR) polymers are a microporous organic polymer which is tuned to optimize the cavity sizes and distribution for difficult separation applications. The sub-nano sized microcavities are controlled by in situ thermal treatment conditions which have been investigated by positron annihilation lifetime spectroscopy (PALS). The size and relative number of cavities increased from room temperature to 230 °C resulting in improvements in both permeabilities and selectivities for H(2)/CO(2) separation due to the significant increase of gas diffusion and decrease of CO(2) solubility. The highest performance of the well-tuned TR-polymer membrane was 206 Barrer for H(2) permeability and 6.2 of H(2)/CO(2) selectivity, exceeding the polymeric upper bound for gas separation membranes.

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New polyamides, containing a benzimidazole side group and ethylene oxide moieties in the structural repeat unit, were synthesized by low‐temperature polycondensation. The aim of this design was to obtain polyamides that were more soluble in common organic solvents and hence had better processability than benzimidazole polyamides while maintaining the water sorption properties characteristic of the latter. The results showed that the number of ether linkages of the repeat unit played an important role in the glass‐transition temperature and in the water sorption properties, the polyamides with one or two ethylene oxide units being more hydrophilic than benzimidazole polyamides. However, the length of the ethylene oxide chain played a minor role in the solubility because the second member of the series, with two ether linkages (i.e., one ethylene oxide unit), reached the same level of solubility as those polyamides with more ethylene oxide moieties. No crystallinity was observed by X‐ray and calorimetric measurements for the new polymers. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 112–121, 2005