| Summary: | Organic fluorescent materials are widely applied in different important fields, such as light-emitting display, explosive detection, molecular imprinting, and so on, because of their low cost, easy functionalization, and large-scale fabrication. In this work, we designed and synthesized a new kind of organic fluorescent polysulfate composite material through post-sulfonation sulfur-fluorine exchange polymerization (a new kind of click chemistry) by symmetric molecular. Sulfur-fluorine exchange polymerization: symmetrical structure SO2F−R1−SO2F molecular reacted with symmetrical OH−R2−OH molecular through nucleophilic reaction in the presence of inorganic base. The polysulfate material was further modified by ClSO<sub>3</sub>H to get PSE−SO<sub>3</sub>H materials. Tb<sup>3+</sup> was highly dispersed on PSE−SO<sub>3</sub>H to afford organic-inorganic hybrid fluorescent materials through the conventional coordination chemistry method. The emission wavelength of the organic-inorganic hybrid fluorescent polymer PSE−SO<sub>3</sub>H−Tb<sup>3+</sup> was between 475 and 685 nm, the quantum yield reached 1.18%, and fluorescence lifetime lasted for 730.168 us, with the pure green light emission and long light-emitting lifetime. The fluorescence film was prepared through phase transformation method by the fluorescent polymer material PSE−SO<sub>3</sub>H−Tb<sup>3+</sup>. The film has the strong stability property in different pH conditions (pH 1~13). Thus, this kind of organic fluorescent polysulfate composite material may have certain prospects application in terms of detection and luminescence in extreme chemical environments in the future.
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