Polythioureas are emerging materials with fascinating properties, such as self-healing and adhesion, high refractive indices, high dielectric constants, and heavy metal ion adsorption.With the increasing requirement for polymer structures and properties suiting a wide range of potential applications, versatile synthetic approaches are demanded to access a great diversity of polythiourea structures efficiently and economically. In this work, a commercially available difluorocarbene precursor, difluoromethylene phosphobetaine (PDFA), was selected to react with sulfur and electron-deficient aromatic amines to enable the efficient syntheses of electron-deficient polythioureas from amine monomers with low reactivity based on the high reactivity of a difluorothiocarbonyl intermediate. A one-pot catalyst-free multicomponent reaction of sulfur, PDFA and an amine was designed, which could take place efficiently in DMAc at 60 °C under nitrogen and was applicable for aromatic amines with both electron-donating and electron-withdrawing groups, producing thioureas in high yields (up to 93%). Most importantly, catalyst-free multicomponent polymerizations of sulfur, PDFA, and diamines were also developed in DMAc at 60 °C with commercially available monomers, showing high efficiency (Mws up to 65 900 g mol−1 and yields up to 99%) and wide monomer applicability, providing an efficient synthetic approach for syntheses of polythioureas. Moreover, these polythiourea thin films showed high refractive indices (n633 nm up to 1.8133), suggesting their potential application in optical devices.
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