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作 者:田永畅 张雨 申克静[2] 邱小魁 孙佳丽 许立信[4] TIAN Yongchang;ZHANG Yu;SHEN Kejing;QIU Xiaokui;SUN Jiali;XU Lixin(Engineering Research Institute,Anhui University of Technology,Ma'anshan 243032,China;Analysis and Testing Center,Anhui University of Technology,Ma'anshan 243032,China;GBXF Silicones Co.,Ltd.,Ma'anshan 238251,China;College of Chemistry and Chemical Engineering,Anhui University of Technology,Ma'anshan 243032,China)
机构地区:[1]安徽工业大学工程研究院,安徽马鞍山243032 [2]安徽工业大学分析与测试中心,安徽马鞍山243032 [3]安徽硅宝有机硅新材料有限公司,安徽马鞍山238251 [4]安徽工业大学化学与化工学院,安徽马鞍山243032
出 处:《有机硅材料》2024年第2期13-19,31,共8页Silicone Material
基 金:国家自然科学基金项目(22108238,U22A20408);安徽省自然科学基金青年基金项目(1908085QB68);安徽省科技重大专项(201903a05020055);中国博士后面上项目(2019M662060)。
摘 要:以N-(2-氨乙基)-3-氨丙基三甲氧基硅烷和对氯甲基苯乙烯为原料进行亲核取代反应,成功合成了3-(N-苯乙烯基甲基-2-氨基乙基氨基)丙基三甲氧基硅烷偶联剂,并通过核磁氢谱、气相色谱质谱联用仪、高效液相色谱和傅立叶红外光谱进行表征。考察了物料比、反应温度、不同阻聚剂和缚酸剂的种类对反应的影响以及溶剂的选择对产品外观的影响。最优反应条件为:N-(2-氨乙基)-3-氨丙基三甲氧基硅烷与对氯甲基苯乙烯的物质的量之比为1.0∶1,反应温度为80℃,对苯二酚作阻聚剂,三乙胺作缚酸剂,甲苯或苯作溶剂。在最优反应条件下,反应转化率达到100%,产品透明度较好。3-(N-styrylmethyl-2-aminoethylamino)propyltrimethoxysilane coupling agent was successfully synthesized by nucleophilic substitution with N-(2-aminoethyl)-3-aminopropyl trimethoxysilane and p-chloromethylstyrene as raw materials,and characterized by hydrogen nuclear magnetic resonance,GCMS,high performance liquid chromatography and Fourier infrared spectroscopy.The effects of ratios,temperature,different types of inhibitors and acid scavengers on the reaction and the influence of solvents on the appearance of the product were investigated.The optimal conditions were that the molar ratio of N-(2-aminoethyl)-3-aminopropyl trimethoxysilane and p-chloromethylstyrene was 1.0∶1,under the temperature of 80℃,hydroquinone was used as an inhibitor,and triethylamine was used as an acid scavenger,toluene or benzene was applied as a solvent.Under the optimal conditions,the reaction conversion rate was 100%,and the product was transparent.
关 键 词:N-(2-氨乙基)-3-氨丙基三甲氧基硅烷 对氯甲基苯乙烯 亲核取代 3-(N-苯乙烯基甲基-2-氨基乙基氨基)丙基三甲氧基硅烷
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