新型含硫有机膦阻燃剂的合成与应用分析-synthesis and application analysis of novel sulfur-containing organophosphine flame retardants.docxVIP

苏州科技学院硕士学位论文摘要摘要有机磷系阻燃剂以其优异的阻燃性能和环保优势，符合人们对阻燃剂无卤化的 要求，成为了当今世界阻燃剂行业的研究热点之一。目前有机磷系阻燃剂的研究主 要集中在：提高含磷量，增大分子量，多元素协同阻燃，改善与材料相容性等方面。本论文依据这一思路，以苯基硫代膦酰二氯为基本原料，设计合成了三种新型 含硫有机膦阻燃剂：聚苯基硫代膦酸（10-(2,5-二羟基苯基)-9-氧杂-10-磷酰杂菲）酯（PDPTP），苯基硫代膦酸二（1-氧基磷杂-2,6,7-三氧杂双环[2.2.2]辛烷基-4-甲）酯（PPS-PEPA），聚苯基硫代膦酸乙二醇酯（PPSET）。并对反应时间、反应温度、原 料配比、提纯溶剂的选择等方面进行了详细的探讨，得到了最佳的合成工艺条件。 利用红外光谱仪，核磁共振 1H NMR 和元素分析仪对其结构进行了表征，结果证明 所合成的化合物为目标产物。用热重/差热联用分析仪（TG /SDTA）分别对三种产 物的热稳定性进行了考察，结果表明三种产物均有较好的热稳定性能，热分解温度 均大于 270℃。运用极限氧指数法测定了它们的阻燃性能，结果显示三种产物对聚 对苯二甲酸乙二醇酯（PET）均具有较好的阻燃性能，当添加量为 20 wt%时，LOI 值达到了 28%以上。同时产物 PDPTP 和 PPS-PEPA 无论是单独使用还是复配，对工 程塑料聚对苯二甲酸丁二醇酯（PBT）也都有较好的阻燃效果。关键词：苯基硫代膦酰二氯，合成，含硫有机膦阻燃剂，阻燃性能Master Dissertation of Suzhou University of Science and TechnologyAbstractAbstractBased on its excellent flame retardant properties, environmental advantages and meeting the requirements for non-halogenated flame retardants, organic phosphorus flame retardants has become one of the hot study topics in the flame retardant industry around the world. The research to organic phosphorus flame retardants is mainly concentrated in the following areas: to improve the phosphorus content , to increase the molecular weight, multi-element retardants, to better the compatibility with materials, and so on.According to this idea, three new sulfur-containing organic phosphine flameretardants were designed and synthesized using the phenyl dichloride as the basic raw materials in the paper, they are poly phenyl acid phosphonothioic (10-(2,5-dihydroxyphenyl)-9-xa-10-phosphoryl hybrid-philippines) ester (PDPTP), diethyl phenyl phosphine (1-oxy phosphorus miscellaneous 2,6,7-three oxygen miscellaneous bicyclo [2.2.2] octane-4-methyl) ester (PPS-PEPA) and poly phenyl thio phosphonic acid ethylene glycol ester (PPSET). Moreover, by discussing the reaction time, reaction temperature, the ratio of raw materials, the selection of solvents and so on in detail, we acquired the optimal synthesis conditions. The chemical structures ofthe products were co