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3. Facile new approach to high sulfur-content materials and preparation of sulfur–lignin copolymers

   https://doi.org/10.1039/c9ta10742h  

   Karunarathna, Menisha S. ; Tennyson, Andrew G. ; Smith, Rhett C. ( January 2020 , Journal of Materials Chemistry A)

   This report introduces a new approach to high sulfur-content materials. This route, RASP (radical-induced aryl halide/sulfur polymerization), expands the substrate scope beyond olefins required for the traditional inverse vulcanization route to such materials. RASP allows direct reaction of two unmodified industrial waste products to give lignin–sulfur composites.
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5. Copolymerization of an aryl halide and elemental sulfur as a route to high sulfur content materials

   https://doi.org/10.1039/c9py01706b  

   Karunarathna, Menisha S. ; Lauer, Moira K. ; Tennyson, Andrew G. ; Smith, Rhett C. ( March 2020 , Polymer Chemistry)

   High sulfur-content materials (HSMs) have been investigated for a plethora of applications owing to a combination of desirable properties and the low cost of waste sulfur as a starting monomer. Whereas extended sulfur catenates are unstable with respect to orthorhombic sulfur (S 8 rings) at STP, oligomeric/polymeric sulfur chains can be stabilized when they are confined in a supporting matrix. The vast majority of reported HSMs have been made by inverse vulcanization of sulfur and olefins. In the current case, a radical aryl halide–sulfur polymerization (RASP) route was employed to form an HSM ( XS81 ) by copolymerizing elemental sulfur with the xylenol derivative 2,4-dimethyl-3,5-dichlorophenol (DDP). XS81 is a composite of which 81 wt% is sulfur, wherein the sulfur is distributed between cross-linking chains averaging four sulfur atoms in length and trapped sulfur that is not covalently attached to the network. XS81 (flexural strength = 2.0 MPa) exhibits mechanical properties on par with other HSMs prepared by inverse vulcanization. Notably, XS81 retains mechanical integrity over many heat-recast cycles, making it a candidate for facile recyclability. This is the first report of an HSM comprising stabilized polymeric sulfur that has been successfully prepared from a small molecular comonomer by RASP. Preparationmore »of XS81 thus demonstrates a new route to access HSMs using small molecular aryl halides, a notable expansion beyond the olefins required for the well-studied inverse vulcanization route to HSMs from small molecular comonomers.« less