含双螺环阻燃剂的制备及其在聚丙烯中的应用

Preparation of Schiff Base Type Flame Retardant Based on Double Spiral Ring and Its Application in PP

采用季戊四醇和三氯氧磷作为反应原料,制备了中间体二氯双螺环季戊四醇二磷酯(SPDEB),然后,再以中间体、对羟基苯甲醛和乙二胺作为反应单体,三乙胺作为缚酸剂,反应生成具有席夫碱的季戊四醇磷酸酯(SPDEB)。利用FT-IR、^(1)H-NMR、^(31)P-NMR及固态^(13)C-NMR分别表征了中间体SPDEB和目标产物SPDEB的化学结构,研究结果表明,合成产物与预期一致。采用极限氧指数和锥形量热研究了不同复配比的聚磷酸铵(APP)及SPDEB在聚丙烯(PP)基体中的热降解行为及协同阻燃性。结果表明,将APP与SPDEB以3:1进行复配,当复配阻燃剂含量为PP的30%时,阻燃PP的极限氧指数(L0I)达到35%。在APP与SPDEB的协同作用下,能够明显改善PP燃烧时的熔滴缺陷,显著降低热释放速率和烟释放速率。

In this paper,the intermediate was prepared using pentaerythritol and phosphorus oxychloride as reaction raw materials,and then Schiff Alkali pentaerythritol phosphate(SPDEB)was synthesized by the reaction of the intermediate with p-hydroxybenzaldehyde and ethylenediamine,and triethylamine as acid binding agent.The chemical structures of intermediate and SPDEB were characterized by by FT-IR,^(1)H-NMR,^(31)P-NMR and solid-state 13C-NMR,respectively.Furthermore,intumescent flame retardant polypropylene composite was prepared using blending of SPDEB and APP by melt compounding method.The results showed that the LOI value of flame retardant PP was 35%while the intumescent flame retardant loading was 30%,when the APP and SPDEB were compounded at 3:1.Meanwhile,the flame retardant PP could reach a V-0 rating in the UL 94 tests.Cone calorimetry results indicated that heat release rate,total heat release,smoke produce rate and total smoke production were reduced dramatically.