3种4-甲氧基二氯化磷酸苯酯衍生聚合物型阻燃剂的合成及其对环氧树脂改性探究

Synthesis of three of MOPO derived polymeric flame retardant and its application in EP

以4-甲氧基苯酚和三氯氧磷为原料合成4-甲氧基二氯化磷酸苯酯(MOPO),再将其分别与10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)、4,4-二羟基联苯和双酚A(BPA)聚合得到4-甲氧基苯基(4-甲基-3-(6-氧代-6H-二苯并[c,e][1,2]氧杂膦-6-基)苯基)甲基膦酸酯(MODOP)、4-甲氧基苯基(4′-甲基-[1,1′-联苯基]-4-基)甲基膦酸酯(MOBOP)和4-甲氧基苯基(4-(2-(对甲苯基)丙-2-基)苯基)甲基膦酸酯(MOPOP)这3种阻燃剂。将这3种阻燃剂用于环氧树脂(EP)改性研究,对其极限氧指数(LOI)、垂直燃烧(UL-94)和热学性能进行比较研究。结果表明:MODOP阻燃体系对EP阻燃效果最为明显,添加量达到10%时,阻燃改性EP的LOI值达到24.4%,垂直燃烧等级达到UL-94V-0级。从环保、经济的角度来说,MODOP阻燃剂是3种新型阻燃剂中阻燃效果最好的。

4-Methoxydichlorophosphoric acid phenyl ester(MOPO) were firstly synthesized from 4-methoxyphenol and phosphorus oxychloride.Combining with 10-hydro-9-oxa-10-phospha-phenanthrene-10-oxide(ODOPB),4,4-dihydroxybiphenyl and bisphenol A(BPA),4-methoxyphenyl(4-Methyl-3-(6-oxo-6 H-dibenzo[c,e][1,2]oxaphosphino-6-yl)phenyl)methyl-phosphonate(MODOP),4-methoxy Phenylphenyl(4′-methyl-[1,1′-biphenyl]-4-yl)methylphos-phonate(MOBOP)and 4-methoxyphenyl(4-(2-(p-toluene)were prepared.By blending in epoxy resin(EP),a serials of flame retarded EP(FR-EP)were made.The limited oxygen index(LOI),vertical combustion(UL-94)and thermal properties of these samples were investigated by appropriate instrument.The results shown that MODOP had the most obvious flame retardant effect in EP.When the added amount reached 10%,the LOI value of FR-EP reached 24.4%,and the vertical burning grade reached UL-94 V-0.From the perspective of environmental protection and economy,MODOP had the best flame retardant effect among the three new flame retardants.