摘要
以丙基三甲氧基硅烷与笼状磷酸酯为原料,合成了一种含磷量、含硅量高的阻燃剂丙基硅酸三环膦酸脂。研究得出的最佳工艺条件是:笼状膦酸脂和丙基三甲氧基硅烷的物质的量之比为3.4∶1,先在65℃下,将丙基三甲氧基硅烷与笼状膦酸脂混合,加热至170℃,保温反应17h,冷却至室温,加入乙醚洗涤,搅拌0.5h,抽滤后烘干,最终产物收率为86.2%。利用傅立叶变换红外光谱、核磁共振、热重分析及极限氧指数等技术手段对该产物的结构以及性能进行表征。结果表明,产物有较好的热稳定性,当产物丙基硅酸三环膦酸脂添加到191不饱和树脂当中,添加量达到20%时,其极限氧指数达到29%,达到难燃级别:当产物添加到聚丙烯(PP)当中,添加量达到25%时,其极限氧指数达到26%,燃烧时样条成炭不滴落。这说明产物丙基硅酸三环膦酸脂表现出了良好的阻燃成炭效果。
Propyl trimethoxy silane and caged phosphate were used as raw materials to synthesize a kind of flame retardant propyl silicic acid tricyclic phosphonate containing high phosphorus content and high silicon content.The optimum conditions are:the molar ratio of glycidoxypropyltrimethoxysilane and cage phosphonic acid lipid 1∶3.4,first at 65℃,the propyl trimethoxysilane and cage phosphonic acid ester are mixed,and then heated to 170℃,the reaction of 17 h,cooling to 40℃,adding ether washing,stirring 0.5 h,filtration after drying,the final product yield is 86.2%.The structure and properties of the product were characterized by means of fourier transform infrared spectroscopy and nuclear magnetic resonance,thermogravimetric analysis and the limit oxygen index.The results show that the product has good thermal stability.When the product is added to 191 unsaturated resin with 20%propylsilicate tricyclic phosphonate,the oxygen index reached 29%and the flame retardant level reach.When the product is added to polypropylene with 25%propylsilicate tricyclic phosphonate,the limiting oxygen index reach 26%and the spline charring does not drop during combustion.This indicates that propylsilicate tricyclic phosphonate has good flame retardant and charring effect.
作者
仲柿成
李果
王彦林
Zhong Shicheng;Li Guo;Wang Yanlin(School of Chemistry Bioligy and Material Engineering,Suzhou University of Science and Technology,Suzhou 215009,China)
出处
《工程塑料应用》
CAS
CSCD
北大核心
2019年第8期124-127,134,共5页
Engineering Plastics Application
关键词
丙基三甲基硅烷
笼状膦酸脂
高含磷量
阻燃剂
propyl three methyl silane
caged phosphonate
high phosphorus content
flame retardant
