阻燃剂有机硅酸单环膦酸酯的合成与应用  

Synthesis and application of flame retardant organosilicic acid monocyclic phosphonate

作　　者：许梓轩 李果 王彦林 XU Zhi-xuan;LI Guo;WANG Yan-lin(School of Chemistry Bioligy and Material Engineering,Suzhou University of Science and Technology,Suzhou 215009,China)

机构地区：[1]苏州科技大学化学生物与材料工程学院,江苏苏州215009

出　　处：《化学研究与应用》2019年第4期658-662,共5页Chemical Research and Application

摘　　要：以笼状亚磷酸酯4-乙基-2,6,7-三氧杂-1-磷杂双环[2.2.2]辛烷和甲基三甲氧基硅烷为原料,合成一种有机硅磷协同效应的阻燃剂,即有机硅酸单环膦酸酯(MSAMP)。探究不同物质的量比、反应温度以及反应时间对产率的影响,得出最佳反应条件:n(笼状亚磷酸酯):n(甲基三甲氧基硅烷)=1:1.2,在反应温度155℃的条件下反应17h,产品得率为87.5%。通过FTIR、~1H-NMR、TG-DTA对产物的结构及性能进行了表征,将产物应用于191不饱和树脂和PBT,通过极限氧指数法来测试其阻燃性能。结果表明,该产物具有较好的热稳定性及良好的阻燃效果。A phosphorus,silicon element dual synergistic flame retardant,methyldimethoxy silicic acid monocyclic phosphonate,was synthesized by caged phosphite-4-ethyl-2,6,7-trioxa-1-phosphorus oxabicyclo[2.2.2]octane and mthyltrimethoxysilane.The effects of different mass ratio,reaction temperature and reaction time on yield were investigated,and the best reaction conditions were obtained:With dimethyl sulfate as catalyst,n(cage phosphate):n(methyltrimethoxy silane)=1:1.2,and the reaction yield was 87.5%at 155℃for 17h.The structure of the product was characterized by FTIR,1H-NMR and TG-DTA.The structure of the product was characterized by FTIR,1H-NMR and TG-DTA.The flame retardancy was tested by limiting oxygen index to 191 unsaturated resin and PBT.The results show that the product has good thermal stability and shows good flame retardant effect.

关 键 词：甲基三甲氧基硅烷 笼状亚磷酸酯 有机硅膦阻燃剂 阻燃剂 

分 类 号：O624.4[理学—有机化学] O634.41[理学—化学]