新型有机硅-氮阻燃剂的合成与应用  

Synthesis and Application of A Novel Organic Si-N Synergistic Flame Retardant

作　　者：娄帅 仲柿成 王彦林[1] Lou Shuai;Zhong Shicheng;Wang Yanlin(School of Chemistry and Life Sciences,Suzhou University of Science and Technology,Suzhou 215009,China)

机构地区：[1]苏州科技大学化学与生命科学学院,江苏苏州215009

出　　处：《工程塑料应用》2022年第7期128-132,139,共6页Engineering Plastics Application

基　　金：江苏省自然科学基金项目(BK20190943)。

摘　　要：以二甲基二氯硅烷和三聚氰胺钠盐为原料,合成了一种新型的硅-氮阻燃剂二甲基硅酰二三聚氰胺(DMSBM)。最佳工艺条件为:氮气保护下,以四氯化碳为溶剂,三聚氰胺钠盐溶解后,缓慢滴加二甲基二氯硅烷,二甲基二氯硅烷和三聚氰胺钠盐的物质的量之比为1∶2.2,70℃下保温反应7 h,降温至30℃后抽滤,蒸馏水洗涤后干燥得到产物,收率为90.1%。通过红外光谱、核磁共振氢谱对产物进行了表征,通过差热分析法分析了产物的热稳定性,将产物应用于不饱和聚酯树脂,进行了极限氧指数、垂直燃烧及拉伸性能测试,扫描电子显微镜表征分析结果表明,残炭结构能进一步起到阻燃作用。产物以硅氮共价键结合,酰胺结构稳定,具有良好的热稳定性能;将其应用于不饱和树脂材料呈现出良好的膨胀成炭性能和阻燃效果,同时还具有一定的增塑性。A novel organic Si-N synergistic flame retardant dimethylsilylacyl bismelamine(DMSBM)was synthesized from di-methyldichlorosilane and sodium melamine.The optimal conditions were:n(dimethyldichlorosilane):n(sodium melamine)=1∶2.2 while carbon tetrachloride as solvent.Dimethyldichlorosilane was added dropwise after sodium melamine was dissolved and reacted for 7 h at 70℃under nitrogen atmosphere,and filtered after cooling to 30℃.The yield was 90.1%after washed with distilled water and dried.The product was characterized by Fourier Transform Infrared(FTIR),1 H Nuclear Magnetic Resonance(NMR).The thermal stability of the product was tested by thermogravimetry(TG)-differential thermal analysis(DTA).The limit oxygen index(LOI),vertical flammability and mechanical property was tested when it was applied to unsaturated polyester resin.The SEM characterization analysis results show that the residual carbon structure could further play a flame retardant effect.The amide structure of the product is stable,and silicon nitrogen is bound by covalent bond.The product has an excellent thermal stability and presented certain plasticization and a good effect on antiflaming when it was applied to 886 unsaturated resin.

关 键 词：有机硅-氮阻燃剂 三聚氰胺 二甲基二氯硅烷 二甲基硅酰二三聚氰胺 成炭剂 

分 类 号：TQ314.248[化学工程—高聚物工业]