Novel phosphorus-silicon synergistic flame retardants:Synthesis and characterization

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Three novel flame retardants containing both phosphorus and silicon elements in their structures,including [(1,1,3,3-tetramethyl-1,3-disiloxanediyl)di-2,1-ethanediyl]bis(diphenylphosphine oxide) (FR-1),[(2,4,6,8-tetramethylcyclotetra-siloxane-2,4,6,8-tetrayl)tetra-2,1-ethanediyl]tetrakis[diphenylphosphine oxide] (FR-2) and 1,3,5,7,9,11,13,15-octakis(di-phenylpho-sphine oxide-2,1-ethanediyl)pentacyclo[9.5.1.13,9.15,15.17,13]octasiloxane (FR-3) were synthesized by a convenient pathway from the reaction of diphenylphosphine oxide (DPPO) and vinyl-terminated siloxanes under the catalysis of tfiethylborane.The chemical structures of the target compounds were confirmed by nuclear magnetic resonance (1a NMR,13C NMR,29Si NMR and 31p NMR),matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) and Fourier transform infrared (Fr IR) measurements.Thermogravimetric analysis (TGA) results indicated that the new flame retardants possessed good thermal stability both in nitrogen and in air.FR-3 containing polyhedral oligosilsesquioxanes (POSS) moiety exhibited the best thermal properties with a 10% weight loss temperature >400 ℃ and a residual weight ratio >39% at 700 ℃.
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