有机硅、硫、磷阻燃成炭剂的合成与应用研究  

Synthesis and Application of Organic Silicon, Sulfur, Phosphorus Flame Char-forming Agent

作　　者：贺婧[1] 杨海军[1] 沈东杰[1] 王彦林[1] 

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：《塑料科技》2017年第1期89-93,共5页Plastics Science and Technology

摘　　要：以丙基三甲氧基硅烷(PTMO)和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,合成了一种笼状硫代磷酸酯阻燃剂——丙基硅酸三-1-硫基磷杂-2,6,7-三氧杂双环[2.2.2]辛基-4-甲酯(PSTSPE)。同时探讨了溶剂、反应温度、反应时间及物料比等对产率的影响,并得到合成反应的最佳条件:SPEPA与PTMO的物质量比为3.3:1,第一步在130℃下反应2 h,第二步在150℃下反应8 h。该条件下,产物的产率可达到94.3%。另外通过红外光谱(FTIR)、核磁共振氢谱(1H-NMR)、热分析(TG/DTA)及极限氧指数(LOI)测试等对产物的结构及性能进行了表征。测试结果表明:产物具有良好的热稳定性,其可对聚对苯二甲酸丁二醇酯(PBT)产生良好的阻燃及成炭、防滴落效果;当其与三聚氰胺聚磷酸盐(MPP)复配用于PBT阻燃时,表现出明显的协同阻燃效应。A kind of caged thiophosphate flame retardant, propyl silicate-methyl-1-thiophospha-2,6,7-trioxabicyclo [2.2.2] octyl-4-methyl ester（PSTSPE）, was synthesized by propyl-trimethoxysilane（PTMO） and 1-thiophospha-4-hydroxymethyl-2,6,7-trioxabicyclo [2.2.2] octane（SPEPA）. The effects of solvent, reaction temperature, reaction time and mass ratio on the yield were investigated. The optimal conditions were selected as follows： the molar ratio of SPEPA and PTMO was 3.3：1, the first step reacted at 130℃ for 2 h, the second step reacted at 150℃ for 8 h, and the yield could reach to 94.3%. Furthermore, the structure and flame retardance of the product were characterized by means of FTIR, 1H-NMR, TG-DTA analysis and LOI test. Results showed that the product had an excellent thermal stability and presented a good effect in antiflaming and anti-dripping when applied to polybutylecetere-phthalate（PBT）. Besides, when it was mixed with melamine pyrophosphate（MPP） and was applied to PBT, high synergistic flameretardance efficiency was found.

关 键 词：阻燃剂 成炭剂 防滴落 协同效应 

分 类 号：TQ314.248[化学工程—高聚物工业]