摘要
以四氯化硅(STC)与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,合成了氯化硅酸双-1-硫基磷杂-2,6,7-三氧杂双环[2.2.2]辛基-4-甲酯(SDSPEC),而后经水解得到二羟基硅酸双-1-硫基磷杂-2,6,7-三氧杂双环[2.2.2]辛基-4-甲酯(SDSPE)。探讨了反应温度、反应时间及物料比对产率的影响,得到的最优工艺条件为:二氧六环作溶剂,n(STC)∶n(SPEPA)=1.0∶2.1,在30℃下反应6 h,水解反应条件为:n(SDSPEC)∶n(H_2O)=1.0∶2.0,60℃下反应4 h,得到SDSPE,产率为93.9%。通过FTIR、~1HNMR、热重分析及极限氧指数测试对产物的结构及性能进行了表征。结果表明,产物有很好的热稳定性,分解温度达270℃;当SDSPE加入量达到191不饱和树脂质量的20%时,191不饱和树脂的LOI值为28%,且残炭量高达38.6%,表明应用于191不饱和树脂时,表现出了较好的阻燃成炭效果。
Dihydroxy silicate, bis-l-thiophospha-2,6,7-trioxabicyclo [ 2.2. 2 ] octyl-4-methyl ester （SDSPE） was prepared from silicon tetrachloride （ STC ） with 1-thiophospha-4-hydroxymethyl-2,6,7- trioxabicyclo [ 2.2.2 ] octane （SPEPA）. The effects of reaction temperature, reaction time and mole ratio of reactants on the yield of SDSPE were investigated. The optimal conditions were obtained as follows： dioxane was used as solvent,and the reaction was carried out at 30 ℃ for 6 h when the mole ratio of STC to SPEPA was 1：2. 1. Subsequently, treatment of the intermediate with water at 60 ℃ for 4 h afforded the targeted product SDSPE, wherein water dosage was two times of STC. Under the optimal conditions, the yield of SDSPE could reach 93.9%. The structure of product was characterized by means of FTIR and 1HNMR. And the flame retardance of product was investigated by TG-DTA analysis and limit oxygen index （LOI） test. The results showed that the product had a good thermal stability, and its decomposition temperature was 270 ℃. When the addition amount of SDSPE was 20% by mass,based on unsaturated polyester resin 191, tile LOI value of unsaturated polyester resin 191 reached 28% ,and the residual char rate could reach up to 38.6% , indicating that SDSPE had high flame retardance and char forming ability for unsaturated polyester resin 191.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2017年第8期930-934,共5页
Fine Chemicals
关键词
四氯化硅
191不饱和树脂
笼状
阻燃剂
橡塑助剂
silicon tetrachloride
unsaturated polyester resin 191
cage
flame retardant
rubber and plastics auxiliaries
