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硅氢加成反应合成KH-540的研究

Research on Hydrosilylation Reaction for the Synthesis of KH-540

【作者】 刘红艳

【导师】 吕连海;

【作者基本信息】 大连理工大学 , 精细化工, 2010, 硕士

【摘要】 有机硅化学是一门研究有机硅化合物的合成、结构、性能和用途的科学。有机硅化合物是除含C、N、O、P化合物以外研究最多的一种化合物,由其制得的有机硅材料,品种众多,性能优异,并已在工农业生产、新兴技术、国防军工、医疗卫生、食品等各种工业部门,已成为化工新材料中发展最快的品种之一硅烷偶联剂是有机硅产品的一种,几种基本单体可生产出上千种有机硅产品,因此其本身可获得广泛应用。合成有硅烷偶联剂的重要反应-硅氢加成反应是有机硅化学中应用最广、研究最多的一个反应。目前工业上广泛使用的催化体系为铂的配合物和负载体,但是这些催化剂存在一些缺点,比如催化剂不稳定、易产生凝胶化物质、烯烃异构化严重等。本论文研究了Pt-三乙胺络合物对于3-氨基丙烯与三甲氧基硅烷(TMOS)的硅氢加成一步合成γ-氨基丙基三甲氧基硅烷的合成,结果发现此种催化剂催化活性高、选择性强、催化剂使用量很低,具有很高的工业价值。利用气质连用定性分析了主、副产物的结构,利用气相色谱内标法监控反应过程并进行定量分析。本论文考察了反应温度、时间、催化剂用量、原料配比和初始压力等因素对硅氢加成反应的影响,结果表明在优化条件下,3-氨基丙烯的转化率可达87.9%,KH-540的选择性可达81.7%,产品无色透明且不容易产生高聚物。

【Abstract】 Organosilicon is one of the most versatile groups of chemicals on the world, they can share some common features that give them special advantages over other materials. Organosilicon materials become the important branch of chemicals industry and hold a very important status in our country’s economy. They are widely used in aerospace, electrical and electronic, textile, light industry, and other industrial sectors.The catalytic hydrosilylation of unsaturated compounds is one of the most elegant methods for the synthesis of organosilicon compounds. Although the hydrosilylation of olefins predominantly uses platinum catalyst in industry at present, the deficiencies are obvious. All the drawbacks often resulted in undesired side reactions. To overcome some of these undesired side reactions, there has been a marked interest in the development of newer and different catalysts for the hydrosilylation reaction.In this paper, Pt-triethylamine complexes were studied as catalysts for the one-pot synthesis of y-aminopropyltrimethoxysilane(KH-540) by hydrosilylation of 3-aminopropene with trimethoxysilane(TMOS). Pt-triethylamine complexes were proved to be active and effective homogeneous catalyst for the hydrosilylation reaction. GC-MS was used to analyze the structures of products qualitatively. The reaction course was monitored by GC, and the products were quantitatively analyzed using internal standard method. Effects of reaction temperature, reaction time, the amount of catalyst, n(TMOS):n(3-aminopropene) ratio, initial pressure on the hydrosilylation were investigated. Under the optimal conditions, the conversion of 3-aminopropene is 87.9%, the selectivity of KH-540 reaches 81.7% and no polymer is found during the whole reaction course of the hydrosilylation.

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