新型硫氮阻燃剂的合成及其环氧树脂应用

Synthesis of novel sulfur-nitrogen flame retardant and its application in epoxy resin

通过苯与1-溴金刚烷的傅-克反应制备了1,3,5,7-四苯基金刚烷,经氯磺化反应与水解中和反应,与鸟嘌呤反应合成了四臂星状硫氮阻燃剂1,3,5,7-四(鸟嘌呤对苯磺酸盐)金刚烷(FRSG)。采用核磁共振光谱和傅里叶变换红外光谱手段对其结构进行了表征。将FRSG与4-羟基甲基-2,6,7-三恶-1-磷酸二环[2.2.2]辛烷1-氧化物(PEPA)复配加入环氧树脂(EP),通过极限氧指数(LOI)、UL94评级以及热重分析研究了EP/FRSG/PEPA的阻燃性能。结果表明,添加质量分数20%的FRSG与PEPA物质的量比1∶2的混合物后体系的LOI可达到30.8%,阻燃等级达到V-0级,继续添加有望进一步提高阻燃性能。

The 1,3,5,7-tetraphenyladamantane was prepared by Friedel-Craft reaction of benzene and 1-bromoadamantane,which was combined with guanine to synthesize the four-arm star-shaped sulfur-nitrogen flame retardant 1,3,5,7-tetrakis(phenyl-4-guanine sulfonate)adamantane(FRSG)after chlorosulfonation reaction and hydrolysis neutralization reaction.The structure of FRSG was characterized by1 H-NMR and FTIR.The FRSG was compounded with 1-oxo-4-hydroxymethyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane(PEPA)and added to the epoxy resin(EP).The flame retardancy of EP/FRSG/PEPA was investigted by the limiting oxygen index(LOI),UL 94 rating and thermogravimetric analysis.The results showed that adding 20 wt%of the mixture(molar ratio of FRSG to PEPA1∶2),the LOI and flame retardant grade of the system reached 30.8%and V-0 grade,respectively and continued addition was expected to further improve the flame retardant performance.