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以苯基磷酰二氯、对羟基苯甲醛、对氨基苯酚及DOPO为原料成功合成了一种新型含磷阻燃剂二[4-(对羟基苯胺-磷杂菲-亚甲基)苯氧基]苯基氧化膦(DOPO-PPO),通过傅里叶红外光谱(FTIR)测试对其结构进行了表征。通过热重分析测试(TGA)研究了产物的热稳定性、热降解行为及成炭性能,结果表明:合成产物的起始热分解温度为280℃,在700℃时的残炭量为36.0%,表明该阻燃剂具有较好的热稳定性和成炭性能。将合成的阻燃剂添加到环氧树脂中,以二氨基二苯硫砜(DDS)为固化剂制备阻燃环氧树脂固化物,通过极限氧指数(LOI)和垂直燃烧(UL-94)测试研究了材料的阻燃性能,通过TGA测试研究了材料的热稳定性及成炭性能,通过耐水测试研究了材料的耐水性能,通过扫描电镜(SEM)研究了炭层的形貌。测试结果表明:当阻燃剂的添加量为14%时,此时材料中含磷质量分数仅为1.1%,材料通过了垂直燃烧测试的UL-94 V-0级,氧指数达到了33.5%,表现出良好的阻燃效率。热重分析测试结果表明:阻燃剂的加入促使材料提前降解,同时提高了材料的成炭性能,在700℃时材料的残炭量由14.1%提高到了27.8%。耐水测试表明:阻燃剂的加入降低了材料的吸水率,耐水测试后材料依然保持良好的阻燃性能。SEM测试表明:阻燃剂的加入使材料在燃烧过程中形成了更加均一、致密的炭层,很好地保护了下层材料,从而提高了环氧树脂材料的阻燃性能。
A novel phosphorus-containing flame retardant bis [4- (p-hydroxyaniline-phosphaphenanthrene-methylene) phenoxy] phenylphosphonic dichloride, p-hydroxybenzaldehyde, p-aminophenol and DOPO was successfully synthesized. Phenyl] phosphine oxide (DOPO-PPO), its structure was characterized by Fourier transform infrared spectroscopy (FTIR). The thermal stability, thermal degradation behavior and carbon formation behavior of the product were investigated by thermogravimetric analysis (TGA). The results showed that the initial thermal decomposition temperature of the product was 280 ℃, the carbon residue at 700 ℃ was 36.0% , Indicating that the flame retardant has good thermal stability and carbon formation. The flame retardant epoxy resin was added into the epoxy resin, and the cured epoxy resin was prepared by using diaminodiphenyl sulfone (DDS) as curing agent. Through limiting oxygen index (LOI) and vertical burning (UL-94) The flame retardancy of the material was tested and studied. The thermal stability and charring performance of the material were studied by TGA. The water resistance of the material was studied by water resistance test. The morphology of carbon layer was studied by scanning electron microscopy (SEM). The test results show that when the amount of flame retardant added is 14%, the content of phosphorus in the material is only 1.1%, the material passes UL-94 V-0 of vertical burning test, the oxygen index reaches 33.5% , Showing a good flame retardant efficiency. Thermogravimetric analysis results show that the addition of flame retardant accelerates the premature degradation of the material and improves the carbon formation of the material. The residual carbon content of the material increases from 14.1% to 27.8% at 700 ℃. The water resistance test showed that the addition of flame retardant reduced the water absorption of the material, and the material still maintained good flame retardancy after the water resistance test. The SEM test shows that the addition of flame retardant makes the material form a more uniform and dense carbon layer during combustion, which protects the underlying material well and improves the flame retardancy of the epoxy resin material.