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...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-phenylphosphine oxide-2,1-ethanediyl)pentacyclo[9.5.1.1^(3,9).l^(5,15).1^(7,13)]octasiloxane(FR-3) were synthesized by a convenient pathway from the reaction of diphenylphosphine oxide(DPPO) and vinyl-terminated siloxanes under the catalysis of triethylborane. The chemical structures of the target compounds were confirmed by nuclear magnetic resonance(^1H 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(FT 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℃ .展开更多
基金the National Natural Science Foundation of China(No.51173188)
文摘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-phenylphosphine oxide-2,1-ethanediyl)pentacyclo[9.5.1.1^(3,9).l^(5,15).1^(7,13)]octasiloxane(FR-3) were synthesized by a convenient pathway from the reaction of diphenylphosphine oxide(DPPO) and vinyl-terminated siloxanes under the catalysis of triethylborane. The chemical structures of the target compounds were confirmed by nuclear magnetic resonance(^1H 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(FT 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℃ .