| Summary: | Poly(2,5-dimercapto-1,3,4-thiadiazole) (PBT) nanosheets were synthesized by chemical oxidative synthesis under mild conditions. The media, oxidant species, monomer concentrations, oxidant/monomer molar ratio, and temperature were optimized to achieve higher yields and better performance. The molecular structure, morphology, and properties of the nanosheets were analyzed by Fourier transform infrared (FT-IR), ultraviolet-visible (UV-Vis), and fluorescence spectroscopies, wide-angle X-ray diffraction (WAXD), matrix-assisted laser desorption/ionization/time-of-flight (MALDI-TOF) mass spectrometry, X-ray photoelectron spectroscopy (XPS), scanning electronic microscopy (SEM), transmission electron microscopy (TEM), and simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC). It was found that the polymerization of 2,5-dimercapto-1,3,4-thiadiazole occurs via dehydrogenation coupling between two mercapto groups to form the –S–S– bond. PBTs show the highest polymerization yield of up to 98.47% and form uniform nanosheets with a thickness of 89~367 nm. poly(2,5-dimercapto-1,3,4-thiadiazole) polymers (PBTs) exhibit good chemical resistance, high thermostability, interesting blue-light emitting fluorescence, and wonderful heavy metal ion adsorption properties. Particularly, the PBT nanosheets having a unique synergic combination of three kinds of active –S–, –SH, and =N– groups with a moderate specific area of 15.85 m2 g−1 exhibit an ultra-rapid initial adsorption rate of 10,653 mg g−1 h−1 and an ultrahigh adsorption capacity of up to 680.01 mg g−1 for mercury ion, becoming ultrafast chelate nanosorbents with a high adsorption capacity. With these impressive properties, PBT nanosheets are very promising materials in the fields of water treatment, sensors, and electrodes.
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