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Abstract We report here a high temperature directed, self-assembly to the synthesis of ordered mesoporous organic polymers (OMPs) with different nanopore sizes and BET surface areas. The synthesized OMPs have large BET surface areas (219–512 m2/g), ordered mesopores, and adjustable pore volumes (0.20–0.48 cm3/g). Their rules of sub-nano level structures such as free volumes, unopened nanopores and electronic environment in the synthesized OMP materials were systematically investigated by using positron annihilation lifetime spectroscopy, which acts as an important technique for investigating microstructures of ordered mesoporous organic polymers and optimization of synthetic conditions of porous organic polymers. Highlights • Ordered mesoporous polymers (OMPs) were hydrothermally synthesized at high temperatures. • Ordered mesopores was constructed from self assembly of copolymer template with resol. • OMPs contain abundant sub-nano level structures such as free volumes, unopened nanopores. • Sub-nano level structures of OMPs were investigated by positron annihilation technique. • Positron annihilation act as useful technique for optimization of synthetic conditions of OMPs. [ABSTRACT FROM AUTHOR]