硅氢化反式-1,4-聚异戊二烯的制备与结构研究

摘要

研究硅氢化反式-1,4-聚异戊二烯(HsTPI)的制备与结构.反式-1,4聚异戊二烯(TPI)的最佳硅氢化反应工艺参数为:反应温度105℃,反应时间12h,催化剂相对TPI质量分数0.07,三乙基硅烷与TPI中乙烯基等摩尔.采用核磁共振氢谱和核磁共振硅谱表证HsTPI的结构,确认三乙基硅烷接枝在TPI的碳-碳主链上.热重分析表明,HsTPI的分解温度随着硅氢化度的增大而逐渐提高,热质量损失由TPI的一阶变为两阶.差示扫描量热分析表明,HsTPI的玻璃化温度随着硅氢化度的增大而提高.X射线衍射分析表明,随着硅氢化度的增大,HsTPI的晶型发生转变,随后结晶能力变小.HsTPI的力学性能随着氢化度的增大而变差.%The preparation and structure of hydrosilated trans-1,4-polyisoprene (HsTPI) were studied.The best hydrosilylation process of trans-1,4-polyisoprene (TPI) was obtained as follows:reaction temperature was 105 ℃,reaction time was 12 h,mass fraction of catalyst relative to TPI was 0.07,and the molar quantities of triethyl silane and vinyl group in TPI were equal.1H-NMR and Si-NMR were carried out to confirm that triethyl silicane group was grafted into TPI C-C main molecular chain.Thermogravimetric analysis showed that the decomposition temperature of HsTPI gradually increased along with degree of hydrosilation increasing,and the thermal mass loss of HsTPI changed from one-stage decomposition to two-stage decomposition.DSC test result showed that the glass-transition temperature of HsTPI increased along with degree of hydrosilation increasing.X-ray diffraction analysis showed that with the increase of the degree of hydrosilation,the crystal form of HsTPI changed and the crystallization ability was weakened.The mechanical properties of HsTPI deteriorated with the increase of hydrosilation degree.