绿色合成3-异氰酸酯基丙基三甲氧基硅烷的研究

Green Synthesis of 3-isocyanatopropyltrimethoxysilane Route

采用氰酸钾和3-氯丙基三甲氧基硅烷为原料,以氰化法合成3-异氰酸酯基丙基三甲氧基硅烷。确定了最佳工艺条件:反应温度105℃,催化剂用量1%,投料比n_(KOCN)︰n_(3-氯丙基三甲氧基硅烷)=2.5,保温时间4 h,保护试剂为己内酰胺,最佳用量n_(己内酰胺)︰n_(3-氯丙基三甲氧基硅烷)=1.6,溶剂为N-甲基甲酰胺,添加量为45%。通过气相色谱,红外光谱分析和核磁谱图分析确定了产物为3-异氰酸酯基丙基三甲氧基硅烷及其纯度。在最佳条件下产品收率为92.38%,纯度为97.26%。

Synthesis of 3-Isocyanatopropyltrimethoxysilane by cyanidation using potassium cyanate and(3-chloropropyl)trimethoxysilane as raw materials.The optimum process conditions were determined:the reaction temperature was 105℃,the catalyst dosage was 1%,the feed ratio was n_(KOCN)︰n_(1,6-dichlorohexane)=2.5,the holding time was 4 h,the protective reagent was caprolactam,the optimal amount was n_(caprolactam)︰n_(1,6-dichlorohexane)=1.6,the solvent was N-methylformamide was added in an amount of 45%.The product was determined by gas chromatography,infrared spectroscopy and nuclear magnetic spectrum analysis,the product was 3-isocyanatopropyltrimethoxysilane and its purity.Under the optimal conditions,the product yield was 92.38%and the purity was 97.26%.