作者:Liyong Zou、Jiyan Liu、Xueqing Liu、Xiaomeng Wang、Jia Chen
DOI:10.1007/s10973-015-5222-8
日期:2016.6
A star-shaped aluminum dimethyl(2,2-dimethyl-1,3-propylene)bis(oxy)bicarbonylethyldiphos phinate (AlCP) was synthesized by esterifying reaction between 2-methy-2,5-dioxo-1,2-oxaphospholane (OP) and neopentyl glycol following by neutralizing with aluminum hydroxide. The structure and composition were confirmed with FTIR, 1H NMR, 31P NMR and X-ray fluorescent spectroscopy. AlCP begins to decompose at 370 °C, matching the initial decomposition temperature of PBT. It endows PBT with desired flame retardancy and anti-dripping property and shows good compatibility with PBT. When the total filler loading is kept at 17, 15–13 mass% AlCP combining with 2–4 mass% MC can make the PBT passing the UL 94 V0 rating and eliminating dripping. In addition, the AlCP has a little influence on the mechanical properties of PBT. The tensile strength and notched impact strength of PBT containing 17 mass% AlCP only reduce by 5.6 and 4 %, respectively, comparing to the pure PBT. The SEM photographs show that AlCP has a good compatibility with PBT. Microcombustion calorimeter, TG-FTIR and SEM results show that AlCP can depress the heating release and promote char forming during combustion and acts mainly in the condensed phase.
通过 2-甲基-2,5-二氧代-1,2-氧代磷杂环戊烷(OP)与新戊二醇的酯化反应,并用氢氧化铝中和,合成了星形二甲基(2,2-二甲基-1,3-丙烯)双羰基乙基二磷酸铝(AlCP)。傅立叶变换红外光谱、1H NMR、31P NMR 和 X 射线荧光光谱证实了其结构和成分。AlCP 在 370 ℃ 开始分解,与 PBT 的初始分解温度一致。它赋予 PBT 理想的阻燃性和防滴落性,并与 PBT 具有良好的相容性。当填料总含量保持在 17%时,15-13 质量%的 AlCP 与 2-4 质量%的 MC 相结合,可使 PBT 通过 UL 94 V0 评级并消除滴落。此外,AlCP 对 PBT 的机械性能影响较小。与纯 PBT 相比,含 17% AlCP 的 PBT 的拉伸强度和缺口冲击强度仅分别降低了 5.6% 和 4%。扫描电镜照片显示,AlCP 与 PBT 具有良好的相容性。微量燃烧热量计、TG-傅立叶变换红外光谱和扫描电镜结果表明,AlCP 能抑制燃烧过程中的热量释放并促进炭的形成,且主要作用于凝聚相。