摘要
由季戊四醇和三氯氧磷出发,经由两步反应合成了三(１氧代－１－磷杂－２,６,７－三氧杂双环[２．２．２]辛烷－４－亚甲基)磷酸酯(Ｔｒｉｍｅｒ),并采用元素分析、ＦＴＩＲ、１Ｈ ＮＭＲ、３１Ｐ ＮＭＲ及Ｘ射线四圆衍射等技术确定了新化合物的分子结构．结构分析表明,Ｔｒｉｍｅｒ分子中含３个结构高度对称的双环笼状磷酸酯单元,属单斜晶系,Ｃｃ空间群,晶胞参数为α＝１．２７５ ４(３)ｎｍ,ｂ＝１．８５８ ２(４)ｎｍ,ｃ＝１．１２６ ９(２)ｎｍ,Ｖ＝２．３２４ ２(８)ｎｍ３,Ｚ＝４．最终偏离因子Ｒ＝０．０３２ ２,Ｒｗ＝０．０９０ ７．ＴＧ－ＤＴＡ与ＤＳＣ结果表明,Ｔｒｉｍｅｒ具有优异的热稳定性与成炭性能,将成为一种高效能的膨胀型阻燃剂．
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 Cc, with unit cell dimensions a= 1. 275 4(3) nm, b=1. 858 2(4) nm, c=1.1269(2)nm, V= 2.324 2(8) nm3, four molecules per unit cell. The final R=0.032 2, Rw=0.090 7 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-DTAand DSC have convincingly demonstrated that Trimer has an excellent thermal stability and char formingcharacteristics, which is expected to be a promising intumescent flame retardant.
出处
《高等学校化学学报》
SCIE
EI
CAS
CSCD
北大核心
2002年第4期695-699,共5页
Chemical Journal of Chinese Universities
基金
高等学校博士点专项科研基金资助.
