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采用二步法合成3-异氰酸丙基三乙氧基硅烷。第一步以3-氨基丙基三乙氧基硅烷(224g,1.01mol)和碳酸二乙酯(132g,1.12mol)在-25℃反应,为避免硅基水解,乙醇钠需溶解在无水乙醇中(乙醇水含量要低于1%)置于滴液漏斗缓慢滴加30min,反应混合物搅拌2h,升至室温(20~25℃),加入1.3m L冰醋酸,调节p H值至中性后减压蒸出。第二步将装有40m L矿物油的圆底烧瓶加热至320~340℃,将[3-(三乙氧基硅基)丙基]氨基甲酸乙酯缓慢滴加到热油上,发生热裂解反应,利用高真空闪蒸技术得到3-异氰酸丙基三乙氧基硅烷,再次精馏得到目标产物,纯度98%(JC),收率可达74.3%。
Synthesis of 3-isocyanatopropyltriethoxysilane by a two-step method. In the first step, 3-aminopropyltriethoxysilane (224 g, 1.01 mol) and diethyl carbonate (132 g, 1.12 mol) were reacted at -25 ° C. To avoid silicon-based hydrolysis, sodium ethoxide was dissolved in anhydrous Ethanol (ethanol content of less than 1%) was placed in the dropping funnel was slowly dropped 30min, the reaction mixture was stirred 2h, warmed to room temperature (20 ~ 25 ℃), add 1.3m L glacial acetic acid, adjust pH value to After sexual decompression. The second step will be filled with 40m L of mineral oil in a round-bottomed flask heated to 320 ~ 340 ℃, the [3- (triethoxysilyl) propyl] urethane was slowly added dropwise hot oil, heat Pyrolysis reaction, using high vacuum flash distillation technology to obtain 3-isocyanatopropyl triethoxysilane, and then distillation to give the target product purity of 98% (JC), the yield of up to 74.3%.