利用二甲基硅油副产物合成笼状有机硅阻燃成炭剂的研究

Study on Cage Organosilicon Flame Retardant Carbonization Agent Synthetized from the By-products of Dimethyl Silicone Oil

以甲基三氯硅烷和季戊四醇为原料合成新型笼状有机硅阻燃成炭剂1-甲基-4-羟甲基-1-硅杂-2,6,7-三氧杂双环-[2,2,2]-辛烷。探讨了反应温度、反应时间、溶剂等对收率的影响,优化的工艺条件为:甲基三氯硅烷与季戊四醇的物质的量比为1∶1,反应温度为150℃,反应时间为4h,产品收率为96%,分解温度达310℃;采用IR、1 H NMR、差热、极限氧指数等技术表征了产品的结构及阻燃等性能;应用实验表明产品有较好的阻燃成炭性。

A new caged organosilicon flame retardant carbonization agent 1-methyl-4-hydroxymethy-l-sili- conheteropoly-2,6,7-three-oxabicyclo-[2,2,2J-octane was synthesized by using methyltrichlorosilane and pentaerythritol as raw materials. The effect of reaction time, temperature and amount ratio o[ subslances on product yield was studied. The optimal conditions for preparation of 1-methyl-4-hydroxymethyl-l-sili conheteropoly-2,6,7-three-oxabicyclo-[2,2,2]-octane were as follows ： n（methyltrichlorosilane） ： n （penta erythritol）was 1 ： 1 and reaction time was 4h at 150℃. The percentage of product yield of 1-metflyl-4- hydroxymethyl-l-siliconheteropoly-2,6,7-three-oxabicyclo-[2,2,2]-octane could reach 96 %. The decompo sition temperature reached 310℃. The molecular structure of 1-methyl-4-hydroxymethyl-l-siliconhetero- poly 2,6,7-three-oxabicyelo [2,2,2]-octane was determined by means of IR and 1H NMR technique. Ap- plication results showed that the product has a good performance of flame retardant carbonization.