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以新戊二醇、三氯氧磷以及1,2,3-三羟基苯等为原料,经过两步反应合成新型阻燃剂1,2,3-三(5,5-二甲基-1,3-二氧杂己内磷酰氧基)苯,采用元素分析、FTIR、MS、1H NMR及X射线四圆衍射等技术确定了标题化合物的分子结构.结构分析表明,该标题化合物属于三斜晶系,P-1空间群,每个结构单元含有2个分子,晶胞参数为a=0.70450(14)nm,b=1.2850(3)nm,c=1.5609(3)nm,α=69.19(3)°,β=86.29(3)°,γ=86.60(3)°,V=1.3171(5)nm3,Dc=1.438g/cm3,μ=0.286mm-1,F(000)=600,Z=2,由4635个独立衍射点得到最终偏离因子[I>2σ(I)]R=0.0574,Rw=0.1061.实验分析表明,该标题化合物具有良好的热稳定性和成炭性,对环氧树脂具有较好的阻燃效果,最佳添加量为20%.
Using neopentyl glycol, phosphorus oxychloride and 1,2,3-trihydroxybenzene as raw materials, a novel flame retardant, 1,2,3-tris (5,5-dimethyl-1 , 3-dioxanaporphosphoryloxy) benzene, the molecular structure of the title compound was confirmed by elemental analysis, FTIR, MS, 1H NMR and X-ray diffraction. The structural analysis showed that the title compound belongs to tris (3) nm, c = 1.5609 (3) nm, α = 69.19, respectively. The crystal structure of the P-1 space group is composed of two groups of elements, (3) ° β = 86.29 (3) ° γ = 86.60 (3) ° V = 1.3171 (5) nm3 Dc = 1.438 g / cm3 μ = 0.286 mm-1 F The final deviation factor [I> 2σ (I)] was obtained from 4635 independent diffraction points with R = 0.0574 and Rw = 0.1061. The experimental results show that the title compound has good thermal stability and carbon formation. Oxygen resin has better flame retardant effect, the best dosage is 20%.