摘要
以苯基三甲氧基硅烷(PhTMO)和1-硫基磷杂-4-羟甲基-2,6,7-三氧杂双环[2.2.2]辛烷(SPEPA)为原料,合成了Si、P、S三元素协同硫代磷酸酯阻燃剂苯基甲氧基硅酸双-1-硫基磷杂-2,6,7-三氧杂双环[2.2.2]辛基-4-甲酯(PSMDSPE)。探讨了溶剂、反应温度、反应时间及物质的量比等对产率的影响。其最佳反应条件:PhTMO和SPEPA物质的量比为1∶2.2,升温至150℃,分馏反应8h,产率为92.7%。通过FT-IR、1 H-NMR、热重分析及极限氧指数测试等对产物的结构及性能进行了表征。测试结果表明:该化合物热稳定性好,应用于聚对苯二甲酸丁二醇酯(PBT)中有良好的阻燃及成炭防滴落效果,并且其与三聚氰胺聚磷酸盐(MPP)复配用于PBT阻燃时表现有协同增效性。
A phosphorothioate flame retardant synergistic with silicon,phosphorus and sulfur three elements,phenyl methoxy silicic acid,bis-1-phosphorus heteroaryl thio-2,6,7-trimethyl-oxabicyclo[2.2.2]octyl-4-methyl ester,was synthesized by phenyltrimethoxysilane（PhTMO）and 1-phosphorus heteroaryl thio-4-hydroxymethyl-yl-2,6,7-trimethyl-oxabicyclo[2.2.2]octane（SPEPA）.The effects of solvent,reaction temperature and time,as well as mass ratio on the yield were investigated.The optimal conditions were selected as follows：n（PhTMO）∶n（SPEPA）was 1∶2.2,kept the reaction going at150℃,then fractionating for 8h and the yield can reach to 92.7%.The structure and flame retardance of product were characterized by FT-IR,~1H-NMR,TG-DTA analysis and LOI technique.Results showed that the product had a good thermal stability and high flame-retardance efficiency for polybutylece terephthalate（PBT）.Besides,when it was mixed with MPP and applied to PBT,high synergistic flame-retardance efficiency was found.
出处
《化工新型材料》
CAS
CSCD
北大核心
2017年第8期244-246,共3页
New Chemical Materials
关键词
阻燃剂
硫代磷酸酯
成炭
协同
flame retardant
thiophosphate
charring
synergism
