阻燃剂赛克三硅酸二氯异丙酯的合成及应用研究

STUDY ON THE SYNTHESIS AND APPLICAYION OF FLAME RETARDANTS TRI(2-HYDROXYETHYL)ISOCYANURAT TRISILICATE DICHLORIDE ISOPROPYL ESTER

以三(2-羟乙基)异氰尿酸酯(赛克,THEIC)、四氯化硅与1,3-二氯-2-丙醇为原料,合成了有机硅酸酯阻燃剂赛克三硅酸二氯异丙酯。探讨了溶剂、反应温度与物质的量比等对产物收率的影响。优化的工艺条件是:n(四氯化硅)∶n(赛克)∶n(1,3-二氯-2-丙醇)=3∶1∶9.6,反应过程中1,3-二氯-2-丙醇分为两次加入,四氯化硅先与1,3-二氯-2-丙醇在45℃反应2h,再加入赛克保温90℃反应11h,滴入剩余1,3-二氯-2-丙醇于90℃反应9h,再加入三聚氰胺,搅拌保温1h,收率为93.2%。通过FT-IR,1 H NMR,差热分析及极限氧指数等表征产了物的结构及性能,产物阻燃效能高,适合用作聚氯乙烯等材料的阻燃剂。

Organic silicate of synergistic flame retardants tri（2-hydroxyethyl） isocyanurat trisilicate di- chloride isopropyl ester was synthesized by using tri （2-hydroxyethyl） isocyanurate （THEIC）, silicon tetrachloride and 1,3-dichloroisopropyl alcohol as raw materials. The effects of solvent, reaction temperature and amount ratio of substance on product yield were discussed. The optimal conditions were selected as follows ： n （silicon tetrachloride） ： n （THEIC） ： n （ 1,3-dichloroisopropyl alcohol） was 3 ： 1 ： 9. 6 and 1,3-dichloroisopropyl alcohol would be added twice during the reaction. The yield could be 93.2% when silicon tetrachloride was first reacted with 1,3-dichloroisopropyl alcohol for 2 h at 45 ℃, then THEIC was added at 90℃ and reacted for 11 h, finally the rest of 1,3-dichloroisopropyl alcohol was added at 90 ℃and reacted for 9 h before the acid binding agent was added for 1 h stirring insulation. The structure and properties of flame retardant products was characterized by using FT- IR, 1H NMR, DTA and limiting oxygen index techniques. The application experiments showed that the product had a good synergistic flame retardant synergism, which can be applied to polyvinyl chloride materials.