Butacene合成方法的改进及性能研究

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.

STUDIES ON SYNTHESIS METHOD AND PROPERTIES OF BUTACENE

4-Chlorobutylferrocene was synthesized from 4-ferrocenylbutanoic acid by typical reactions of NaBH4-I2-THF reduction and thionyl chloride chlorination,in stead of the traditional method with ferrocene and 4-chlorobutyryl chlorid as raw materials,in which NaBH4-I2-THF system replaces toxic zinc amalgam as reducing agent.(4-Ferrocene-butyl) dimethyl silane was perpared from dimethyl chlorosilane and format reagent which was produced by magnesium powder and 4-chlorobutyl ferrocene.The butacene with high yield,which was formed from hydrosilylation,was successfully obtained by reaction of(4-ferrocene-butyl) dimethyl silane and hydroxyl-terminated polybutadiene(HTPB) in the presence of the efficient and reusable platinum catalyst(silica-supported chitosan complex of chloroplatinic acid SiO2-CS-Pt).The structure of the polymer was characterized by 1H-NMR and FTIR.Thermal stability of the polymer was studied using TGA.This work also measured the rate of grafting and the hydroxyl value.The results show that the desired target product with the advanced initial decomposition temperature,increased thermal sensitivity,increased thermal stability and excellent catalytic performance was obtained.