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Two new pyrene‐cored covalent organic polymers (COPs),  CK‐COP‐1  and  CK‐COP‐2 , were synthesized via the one‐step polymerization of two thiophene‐based isomers, 1,3,6,8‐tetra(thiophene‐2‐yl) pyrene ( L 1  ) and 1,3,6,8‐tetra(thiophene‐3‐yl) pyrene ( L 2  ). The resulting pyrene‐cored COPs exhibit rather different surface areas of 54 m 2  g −1  and 615 m 2 g −1  for  CK‐COP‐1  and  CK‐COP‐2 , respectively. The CO 2  uptake capacities of  CK‐COP‐1  and  CK‐COP‐2  also show different values of 2.85 and 9.73 wt % at 273 K, respectively. Furthermore,  CK‐COP‐2  offers not only a larger CO 2  adsorption capacity but also a better CO 2 /CH 4  selectivity at 273 K compared with  CK‐COP‐1 .  CK‐COP‐1  and  CK‐COP‐2  also exhibit considerable differences in their photophysical property. The different structure and properties of  CK‐COPs  could be attributed to the isomer effect of their corresponding thiophene‐based monomers. © 2017 Authors. Journal of Polymer Science Part A: Polymer Chemistry Published by Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem.  2017 ,  55 , 2383–2389

Pyrene‐cored covalent organic polymers by thiophene‐based isomers, their gas adsorption, and photophysical properties