γ-叔丁基过氧丙基三甲氧基硅烷的制备及表征

Synthesis and characterization of γ-tert-butyl peroxide propyltrimethoxysilane

以过氧化氢叔丁醇和3-氯丙基三甲氧基硅烷为原料,以三氯化铁为催化剂在甲苯溶剂中首次了合成γ-叔丁基过氧丙基三甲氧基硅烷。利用红外吸收光谱、1H核磁共振谱以及质谱对产物表征,确定其结构。通过研究催化剂种类、反应物配比、反应时间以及反应温度等因素对合成反应的影响,探讨出实验最佳方案为:反应时间8h,反应温度40℃,n(过氧化氢叔丁醇)∶n(3-氯丙基三甲氧基硅烷)=1.2∶1,催化剂用量为3-氯丙基三甲氧基硅烷质量的1.5%。在此条件下,产物产率最高为42%。

The γ-tert-butyl peroxide propyltrimethoxysilane was synthesized with tert-butyl hydroperoxide and 3-chloropropyltrimethoxysilane,catalyzed by ferric chloride in toluene for the first time. The product was characterized by IR、1H NMR and mass spectra,and its structure was determined. Synthetic conditions such as the catalyst species,the reactants ratio,the reaction temperature and time were discussed. The optimal conditions were determined as follows ： n（tert-butyl hydroperoxide） ∶n（3-chloropropyltrimethoxysilane）=1.2∶1,m（catalyst）∶m（3-chloropropyltrimethoxysilane） =0.015∶1,reaction temperature of 40℃ and reaction time of 8h. The yield of the product could reach 42% under the optimal reaction condition.