聚苯硫醚高相容硅酸酯阻燃剂的合成及应用

Synthesis and Application of Polyphenylene Sulfide High Compatibility Silicate Flame Retardant

将甲基三氯硅烷和季戊四醇混合,首先合成了中间体甲基硅酸季戊四醇酯,在氯化十六烷基吡啶和三氯化铝的催化下,与苯磺酰氯合成了产物(1-甲基-2,6,7-三氧-1-硅烷二环[2.2.2]辛烷-4-基)苯磺酸甲酯。实验优化了原料用量、反应温度和反应时间对产物收率的影响。最佳工艺为:甲基三氯硅烷、季戊四醇和与苯磺酰氯摩尔比为1∶1∶1,二步反应的反应温度分别为150与70℃,反应时间分别为4与2 h,最终产物收率可达93.8%。采用FTIR、1HNMR、TG和极限氧指数等技术对产物进行结构和性能的表征。结果显示,产物与聚苯硫醚(PPS)的最大共混比例为40%,热分解温度为350℃,其共混材料的拉伸强度随产物含量的升高而降低,产物具有较好的阻燃抗熔滴性能。

The intermediate of 1-methyl-4-hydroxymethyl-1-silicon coheteropoly-2,6,7-three-oxabicyclo-[2,2,2]-octane(MSPTA)was synthesized from methyltrichlorosilane and pentaerythritol.Then under the catalysis of cetyl-pyridine chloride(CPC)and Al Cl3,the intermediate reacted with benzene sulfonyl chloride(BSC)to produce the target of(1-methyl-2,6,7-trioxa-1-silabicyclo[2.2.2]-octan-4-yl)methyl benzenesulfonate(MSPT-BSA).The effects of quantity of raw materials,reaction temperature and time on the productivity were optimized.The optimum process was:the ratio of methyl trichlorosilane to pentaerythritol to benzene sulfonyl chloride was 1∶1∶1.The reaction temperature and time in the two steps was 150℃,4 h and 70℃,2 h,respectively.The final yield of MSPT-BSA was 93.8%.The structure and property of MSPT-BSA was characterized by fourier transform infrared spectroscopy(FTIR),1 HNMR,thermogravimetry(TG)and limit oxygen index(LOI)techniques,and so on.The maximum ratio of MSPT-BSA in polyphenylene sulfide(PPS)was 40%,and the thermal decomposition temperature was 350℃.The tensile strength of the composite of MSPT-BSA and PPS decreased with the content increasing of MSPT-BSA.And the application results of the composite proved that the product had good flame retardant and droplet resistant ability.