含硫有机硅磷阻燃成炭剂的合成与应用研究
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Synthesis and Application of Sulfur-containing Organic Silicon Phosphorus Flame Char-forming Agent
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    摘要:

    以二苯基二甲氧基硅烷(DMDPS)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Si、P、S三元素协同阻燃成炭剂二苯基硅酸双-1-硫基磷杂-2,6,7-三氧杂双环[2.2.2]辛基-4-甲酯(DPSSPE)。探讨了溶剂、反应温度、反应时间及摩尔比等对产率的影响。其最佳反应条件:DMDPS和SPEPA摩尔比为1:2.2,升温至140℃,分馏反应7h,产率为92.7%。通过FTIR、1H-NMR、热重分析及极限氧指数测试等对产物的结构及性能进行了表征。测试结果表明:该化合物热稳定性好,分解温度达350℃,应用于聚对苯二甲酸丁二醇酯(PBT)中有良好的阻燃及成炭防滴落效果,并且其与三聚氰胺聚磷酸盐(MPP)复配用于PBT阻燃时表现有协同增效性。

    Abstract:

    A caged phosphorothioate flame retardant synergistic with silicon, phosphorus and sulfur three elements, diphenyl silicic acid bis-1-phosphorus heteroaryl thio-2,6,7-trimethyl- oxabicyclo [2.2.2] octyl-4-methyl ester, was synthesized by dimethoxydiphenylsilane (DMDPS) and 1- phosphorus heteroaryl thio-4-hydroxymethyl-yl-2,6,7-trimethyl- oxabicyclo [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: n(DMDPS): n(SPEPA) is 1:2.2, kept the reaction going at 140℃ , then fractionating for 7h and the yield can reach to 92.7%.The structure and flame retardance of the product were characterized by means of FTIR, 1H -NMR, TG-DTA analysis and LOI technique. Results showed that the product have a good thermal stability and high flame-retardant and anti-dripping efficiency for polybutylece terephthalate (PBT). Besides, when it was mixed with MPP and was applied to PBT, high synergistic flame-retardance efficiency was found.

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王彦林,贺婧,杨海军.含硫有机硅磷阻燃成炭剂的合成与应用研究[J].精细化工,2017,34(6):

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  • 收稿日期:2016-09-28
  • 最后修改日期:2016-12-13
  • 录用日期:2017-01-24
  • 在线发布日期: 2017-05-04
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