Synthesis, Structure and Thermal Property of Tri(1-oxo-2, 6, 7-trioxa-1-phosphabicyclo[2.2.2]octane-methyl)phosphate

Abstract

Abstract: A novel caged bicyclic phosphate flame retardant tri(1-oxo-2, 6, 7-trioxa-1-phosphabicyclo[2.2.2]octane-methyl) phosphate (Trimer) was synthesized from 1-oxo-4-hydroxymethyl-2, 6, 7-trioxal-phos-phabicyclo[2.2.2]octane(PEPA) and phosphorus oxychloride in this paper.Its structure was character-ized by elemental analysis, FTIR, ¹H NMR, ³¹P NMR and X-ray diffraction analysis.The crystals aremonoclinic, space group C_c, with unit cell dimensions a= 1.2754(3) nm, b=1.8582(4) nm, c=1.1269(2)nm, V= 2.3242(8) nm³, four molecules per unit cell.The final R=0.0322, R_w=0.0907 for 2177 unique reflections.The crystal data reveal that the three cages in Trimer are structurally equivalent,and that the corresponding average bond lengths and bond angles are appropriate.The results of TG-DTA and DSC have convincingly demonstrated that Trimer has an excellent thermal stability and char formingcharacteristics, which is expected to be a promising intumescent flame retardant.

Key words: Caged bicyclic phosphate, Intumescent flame retardant, Crystal structure, Thermal stability, Char forming characteristics

CLC Number:

O627.51

TrendMD:

LI Xin, OU Yu-Xiang, ZHANG Yun-Hong. Synthesis, Structure and Thermal Property of Tri(1-oxo-2, 6, 7-trioxa-1-phosphabicyclo[2.2.2]octane-methyl)phosphate[J]. Chem. J. Chinese Universities, 2002, 23(4): 695.

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Synthesis, Structure and Thermal Property of Tri(1-oxo-2, 6, 7-trioxa-1-phosphabicyclo[2.2.2]octane-methyl)phosphate

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