含硫有机硅磷阻燃成炭剂的合成与应用  

Synthesis and Application of Sulfur Containing Organosilicon Phosphorus Flame Retardant Charming Agent

作　　者：王鑫[1] Wang Xin(Kunming University of Technology,Kunming Yunnan 650000)

机构地区：[1]昆明理工大学,云南昆明650000

出　　处：《山西化工》2023年第3期31-32,35,共3页Shanxi Chemical Industry

摘　　要：以1-硫基磷杂-4-羟甲基-2,6,7-三氧杂双环[2.2.2]辛烷(SPEPA)以及丙基三甲氧基硅烷(PTMO)为原料,实现对一种含硫、有机硅、磷三元素协同阻燃成炭剂——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)的合成。考虑反应温度、溶剂、反应时间和物料比对PSTSPE产率的影响。结果表明,最佳反应条件是:n(SPEPA)∶n(PTMO)=3.3∶1。先在130℃下反应,分馏时间2 h,之后升温至150℃反应,分馏时间8 h,此时PSTSPE的产率能达到94.3%。此外,通过1H-NMR、FTIR、TG/DTA以及LOI对PSTSPE的结构和性能进行表征测试。测试结果表明,该化合物具有良好的热稳定性,当分解温度在325℃,PSTSPE与MPP的复配比为1.5时,化合物的LOI能达到34%,且不低落。由此可见,化合物PSTSPE的阻燃和成炭防滴落效果良好,并且同MPP复配后表现出明显的协同增效性。Using 1-thiophospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane(SPEPA)and propyltrimethoxysilane(PTMO)as raw materials,a synergistic flame retardant charring agent of sulfur,organosilicon and phosphorus-propylsilicate-tria-1-thiophospha-2,6,7-trioxabicyclo[2.2.2]octyl-4-methyl ester(PSTSPE)was synthesized.The effects of reaction temperature,solvent,reaction time and material ratio on the yield of PSTSPE were considered.The results showed that the optimum reaction condition was n(SPEPA)∶n(PTMO)=3.3∶1.The reaction was conducted at 130℃for 2 h,and then heated to 150℃for 8 h.At this time,the yield of PSTSPE could reach 94.3%.In addition,the structure and properties of PSTSPE were characterized by 1H-NMR,FTIR,TG/DTA and LOI.The test results show that the compound has good thermal stability.When the decomposition temperature is 325℃and the composite ratio of PSTSPE and MPP is 1.5,the LOI of the compound can reach 34%without dropping.It can be seen that the compound PSTSPE has good flame retardancy and charring and anti-dripping effect,and it shows obvious synergistic effect when compounded with MPP.

关 键 词：阻燃剂 成炭剂 协同效应 功能材料 

分 类 号：TQ314.248[化学工程—高聚物工业]