长链烷基硅烷的合成及催化体系研究
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摘要
随着工业的发展,有机硅产品在人们的生活和生产中起到越来越重要的作用,成为不可或缺的化工材料。以过渡金属为催化剂的硅氢加成反应是合成硅-碳官能团有机硅的主要途径,因此催化剂的开发研究对于工业生产具有重要的理论意义和实际应用价值。本文主要研究内容如下:
1、研究了一种液态位阻胺作为助催化剂,在铂催化剂催化合成长链烷基三烷氧基硅烷时,使反应产率从60%提高到90%,且该方法具有催化剂用量少(以贵金属Pt计仅为5mg/kg)、反应条件温和(常压、30~80℃)等特点。同时,对铂催化硅氢加成反应机理作了验证性研究。
2、自制羰基氯化钌配合物作为硅氢加成反应的催化剂,经红外光谱(IR)、X射线光电子能谱(XPS)、能谱(EDS)表征确定其结构为[RuCl2(CO)3]2。该催化剂可以在常温下催化硅氢加成反应合成长链烷基三烷氧基硅烷,产率可以达到90%以上,且反应完成后贵金属钌的回收率可以达到80.5%,很大程度上降低了硅氢加成反应的成本,常温反应也使得工业化生产更安全,该方法具有很好的工业应用前景。另外,对羰基氯化钌的催化性能、反应前后的结构变化进行了研究。
3、采用以上铂催化剂和钌催化剂方法进行催化硅氢加成,反应副产物少,只要经过简单精馏就可以得到纯度99%的产品。实验采用质谱、核磁共振和气相色谱对产物进行表征和定量分析,结果表明,产物皆为β-加成产物。
With the development of the industry, organic silicon products become an indispensable chemical material,which play a more and more important role in people's life and industrial production.The hydrosilylation of synthetic silicon - carbon functional groups silicone with the transition metal as catalysts is one of the mainmethods, so it has important theoretical significance and practical value to research the catalyst for the industrial production. The main results of study in this paper are summarized as follows:
1、A liquid sterically hindered amine as a sub-catalyst is developed, and the yield of synthesis of long chain alkyl trialkoxysilane by platinum catalyst was improved from 60% to 90%. This method has the advantage of using less catalyst (the concentration of Pt is only 5mg/kg), mild reaction conditions (atmospheric pressure, 30 ~ 80℃) and so on. Meanwhile, mechanism of platinum catalyzed hydrosilylation reaction was studied.
2, The carbonyl chloride ruthenium complexes is used as hydrosilylation catalysts, and the structure is [RuCl2(CO)3]2 which determined by IR, XPS and EDS. The catalyst can be used to catalyze hydrosilylation reaction of long chain alkyl trialkoxysilane at room temperature, the yield is more than 90%, and the recovery of precious metal ruthenium can reach 80.5%, which largely reducing the cost of the hydrosilylation reaction,and it also makes industrial production more secure when reaction at room temperature. This method has good prospects for industrial applications. In addition, the catalytic properties of carbonyl-chloride ruthenium and structural changes before and after reaction were studied.
3, The above method of using platinum catalyst and ruthenium catalyst for catalytic hydrosilylation makes less by-products, and you can obtain the product of with the purity of 99% just through a simple distillation. Mass spectrometry, nuclear magnetic resonance and gas chromatography are used in the experiments to characterize and quantitative analysis the products, the results show that the products are allβ-addition product.
1、研究了一种液态位阻胺作为助催化剂,在铂催化剂催化合成长链烷基三烷氧基硅烷时,使反应产率从60%提高到90%,且该方法具有催化剂用量少(以贵金属Pt计仅为5mg/kg)、反应条件温和(常压、30~80℃)等特点。同时,对铂催化硅氢加成反应机理作了验证性研究。
2、自制羰基氯化钌配合物作为硅氢加成反应的催化剂,经红外光谱(IR)、X射线光电子能谱(XPS)、能谱(EDS)表征确定其结构为[RuCl2(CO)3]2。该催化剂可以在常温下催化硅氢加成反应合成长链烷基三烷氧基硅烷,产率可以达到90%以上,且反应完成后贵金属钌的回收率可以达到80.5%,很大程度上降低了硅氢加成反应的成本,常温反应也使得工业化生产更安全,该方法具有很好的工业应用前景。另外,对羰基氯化钌的催化性能、反应前后的结构变化进行了研究。
3、采用以上铂催化剂和钌催化剂方法进行催化硅氢加成,反应副产物少,只要经过简单精馏就可以得到纯度99%的产品。实验采用质谱、核磁共振和气相色谱对产物进行表征和定量分析,结果表明,产物皆为β-加成产物。
With the development of the industry, organic silicon products become an indispensable chemical material,which play a more and more important role in people's life and industrial production.The hydrosilylation of synthetic silicon - carbon functional groups silicone with the transition metal as catalysts is one of the mainmethods, so it has important theoretical significance and practical value to research the catalyst for the industrial production. The main results of study in this paper are summarized as follows:
1、A liquid sterically hindered amine as a sub-catalyst is developed, and the yield of synthesis of long chain alkyl trialkoxysilane by platinum catalyst was improved from 60% to 90%. This method has the advantage of using less catalyst (the concentration of Pt is only 5mg/kg), mild reaction conditions (atmospheric pressure, 30 ~ 80℃) and so on. Meanwhile, mechanism of platinum catalyzed hydrosilylation reaction was studied.
2, The carbonyl chloride ruthenium complexes is used as hydrosilylation catalysts, and the structure is [RuCl2(CO)3]2 which determined by IR, XPS and EDS. The catalyst can be used to catalyze hydrosilylation reaction of long chain alkyl trialkoxysilane at room temperature, the yield is more than 90%, and the recovery of precious metal ruthenium can reach 80.5%, which largely reducing the cost of the hydrosilylation reaction,and it also makes industrial production more secure when reaction at room temperature. This method has good prospects for industrial applications. In addition, the catalytic properties of carbonyl-chloride ruthenium and structural changes before and after reaction were studied.
3, The above method of using platinum catalyst and ruthenium catalyst for catalytic hydrosilylation makes less by-products, and you can obtain the product of with the purity of 99% just through a simple distillation. Mass spectrometry, nuclear magnetic resonance and gas chromatography are used in the experiments to characterize and quantitative analysis the products, the results show that the products are allβ-addition product.
引文
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