To develop highly efficient organic dyes adsorbents are of great importance for environmental issues. In this work, a negatively charged porous organic polymer (POP) is synthesized by simple aromatic nucleophilic substitution (SNAr) and hydrolysis reaction. This polymer POP‐TFP‐COOH structure is confirmed by IR and 13C cross‐polarization/magic‐angle‐spinning nuclear magnetic resonance. Due to the existence of phenyl rings and carboxylic acid groups, POP‐TFP‐COOH displays excellent adsorption ability for the positive dye methylene blue (MB), with a maximum value of 2740 mg g−1. This porous polymer can be reused at least four times without obvious loss of its adsorption capacity.
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