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以二甲基二氯硅烷和季戊四醇为原料,首次合成了一种无卤环保阻燃剂季戊四醇双二甲基硅酸酯,同时确定了该合成反应的最佳工艺条件,并通过傅里叶变换红外光谱(FTIR)、核磁共振氢谱(1H-NMR)和热重分析表征了产物的结构及热稳定性能。随后将该产物用于聚对苯二甲酸丁二醇酯(PBT)的阻燃,并利用极限氧指数(LOI)测试考察了材料的阻燃性能。结果表明:成功合成了目标产物季戊四醇双二甲基硅酸酯,最佳反应条件下(二乙二醇二甲醚为溶剂、二甲基二氯硅烷和季戊四醇的物质量比为2:1),其产率可达97.6%。该产物具有较好的热稳定性,对PBT具有良好的阻燃效果,且能与聚磷酸铵(APP)、三聚氰胺聚磷酸盐(MPP)产生协同阻燃效应。
Using dimethyl dichlorosilane and pentaerythritol as raw materials, a kind of non-halogen environment-friendly flame retardant pentaerythritol bis-dimethylsilicate was synthesized for the first time. At the same time, the optimum technological conditions of the synthesis reaction were determined and analyzed by Fourier transform The structure and thermal stability of the product were characterized by FTIR, 1H-NMR and TG. The product was then used for the flame retardancy of polybutylene terephthalate (PBT) and the flame retardancy of the material was investigated using the limit oxygen index (LOI) test. The results showed that the target product, pentaerythritol bis-dimethylsilicate, was successfully synthesized under the best reaction conditions (the molar ratio of diethylene glycol dimethyl ether to dimethylsilyl chloride and pentaerythritol was 2: 1) , Its yield can reach 97.6%. The product has good thermal stability, good flame retardant effect on PBT, and synergistic flame retardant effect with ammonium polyphosphate (APP) and melamine polyphosphate (MPP).