摘要
以二氯二甲基硅烷(DMDCS)和三羟甲基氧化磷(THPO)为原料,制备得到一种反应型阻燃剂环状有机膦硅酸酯,即1,1-二甲基-1-硅杂-2,6-二氧杂-4-氧基-4-膦杂-4-羟甲基环己烷。以二乙二醇二甲醚为溶剂,二氯二甲基硅烷和三羟甲基氧化磷的摩尔比为1∶1,最佳工艺条件为在40℃以下,缓慢滴加二氯二甲基硅烷,滴加完成后,在1 h内将温度升至70℃,保温反应8 h,然后,升温至130℃,保温反应6 h,采用碳酸钠水溶液纯化处理产物,收率为95.2%,采用红外光谱、核磁共振、元素分析和极限氧指数等方法对产物的结构及性能进行分析可知,产品可以应用于环氧树脂材料中,具有良好的成炭性和阻燃效果。产物是一种含有活性羟基官能团的反应型有机磷硅协同阻燃剂,也可以作为有机合成中间体具有更广泛的应用。
A novel reactive flame retardant,Monocyclic organophosphorus silicate estero,which was in effect 1,1-dimethyl-1-sila-2,6-dioxa-4-oxy-4-phospha-4-hydroxymethyl hydroxymethyl was synthesized by using Dichlorodimethylsilane(DMDCS)and Tris(hydroxymethyl)phosphine oxide(THPO)as raw material.Theoptimal conditions were selected as follows,n(DMDCS)∶n(THPO)=1∶1 while Diethylene glycol dimethyl ether as the solvent.DMDCS was added dropwise below 40℃,and reacted for 8 h at 70℃,then warm to 130℃and keep warm for 6 h,finally purified with aqueous solution of Sodium carbonate,the percentage of reaction yield could reach 95.2%.The structure and properties of the product was characterized by FT-IR,^(1)H NMR,elemental analysis and the limit oxygen index(LOI)technique.Results showed that the product presented a good effect on antiflaming charring performance when it was applied to epoxy resin.The product was a reactive organophosphorus-silica synergistic flame retardant which containing active hydroxyl functional groups,and could also be used as an organic synthesis intermediate.
作者
娄帅
王世杰
陈舒波
王彦林
LOU Shuai;WANG Shijie;CHEN Shubo;WANG Yanlin(School of Chemistry,Biology and Material Engineering,Suzhou University of Science and Technology,Suzhou,Jiangsu 215009,China)
出处
《塑料》
CAS
CSCD
北大核心
2021年第1期84-87,共4页
Plastics
关键词
二氯二甲基硅烷
三羟甲基氧化磷
反应型阻燃剂
环状有机膦硅酸酯
成炭
dichlorodimethylsilane
tris(hydroxymethyl)phosphine oxide
reactive flame retardant
monocyclic organophosphorus silicate estero
charring
