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与以二茂铁,4-氯丁酰氯为原料的传统合成方法不同,直接以γ-二茂铁丁酸为原料,采用NaBH4-I2-THF体系代替有毒的锌汞齐作为还原剂,以SOCl2为氯代试剂,制备了4-氯丁基二茂铁,将其与镁粉反应制得格式试剂,再与二甲基氯硅烷反应合成4-二茂铁丁基二甲基硅烷,在高效可重复使用铂催化剂(二氧化硅负载壳聚糖络合氯铂酸SiO2-CS-Pt)催化下与端羟基聚丁二烯(HTPB)硅氢加成得到高收率的巴特辛(Butacene).采用1H-NMR和FTIR对其化学结构进行了表征,采用TGA分析了产物的热性能,并测定了接枝率和羟值.研究结果表明,所得产物与目标产物相符,初始热分解温度提前,热敏感度增加,热稳定性增加,具有良好的催化性能。
Different from the traditional synthesis method using ferrocene and 4-chlorobutyryl chloride as raw materials, γ-ferrocenebutyric acid is directly used as a raw material, NaBH4-I2-THF system is used instead of toxic zinc amalgam as a reducing agent, and SOCl2 As chlorination reagent, 4-chlorobutyl ferrocene was prepared, which was reacted with magnesium powder to obtain a format reagent, and then reacted with dimethylchlorosilane to synthesize 4-ferrocene butyldimethylsilane, Reusable hydrosilylation with terminal hydroxyl polybutadiene (HTPB) catalyzed by a platinum catalyst (silica loaded chitosan complexed with chloroplatinic acid, SiO2-CS-Pt) resulted in a high yield of Butacene The chemical structure was characterized by1H-NMR and FTIR, the thermal properties of the product were analyzed by TGA, and the grafting ratio and hydroxyl value were determined.The results show that the obtained product is consistent with the target product, the initial thermal decomposition temperature is advanced , Thermal sensitivity increases, thermal stability increased, with good catalytic performance.