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New Transition Metal Catalyst Synthesis And Applied Research In The Hydrosilylation Reaction

Posted on:2011-05-12Degree:MasterType:Thesis
Country:ChinaCandidate:F YuFull Text:PDF
GTID:2191360305968596Subject:Organic Chemistry
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Organosilicon chemistry is a study of structure, properties and uses of organic silicon compounds.In addition to the compounds containing C, N, O, P, Organosilicon is the most studied compounds. The special composition and molecular structure makes Silicone Products have the characteristics of organic compounds and inorganic compounds. It is widely used in aerospace, electrical and electronic, textile, light industry, building, machinery, medical, food, transportation and other industrial sectors.Hydrosilylation is an important method to prepare the silane coupling agent. Hydrosilylation is the most studied and most widely used response in organosilicon chemistry. At present, the widely used catalyst system in industry is the platinum complexes. But there are two major disadvantages. Firstly, the catalysts are very expensive. The recovery of catalysts is not easy. Secondly, in the case of olefins with electron-drawing substituents, conventional platinum catalysts are not effective. In order to reduce the cost of industrial production and increase the catalytic activity of catalysts, in this paper, we try to synthesize several types of palladium catalysts and nickel catalysts, and apply it to hydrosilylation reaction.1.2-(3,4-Epoxycyclohexyl)ethyl trimethoxysilane were synthesized by the platinum complexes catalyzed hydrosilation reaction of Trimethoxysilane and 1,2-epoxy-4-vinylcyclohexane. The products were analyzed by means of GC-MS and HNMR, and the effects of reaction temperature, the amount of catalyst, the type of catalyst-assisted and the amount of solvent on the production rate were discussed. The self-made catalyst has higher catalytic activity. The most reasonable amount of catalyst is 40ppm. The best ratio of solvent and 1,2-epoxy-4-vinylcyclohexane is 1:1.Yield of the addition product can reach 80% under the temperature 80℃-90℃. The same method is used in the Preparation of 2-(3,4-Epoxycyclohexyl)ethyl methyldiethoxysilane. The best ratio of solvent and 1,2-epoxy-4-vinylcyclohexane is 0.25:1. When the temperature be kept between 60℃to 70℃, yield of the addition product can reach 84%.2. Under the catalyzation of platinum complexes, Octylmethyldiethoxysilane has been synthesized. The products were analyzed by means of GC-MS. and the effects of reaction temperature, the amount of catalyst and the amount of solvent on the production rate were discussed. The most reasonable amount of catalyst is 45ppm. Yield of the addition product is highest under the temperature 80℃-90℃without solvent.3. In this paper, two palladium complexes-salicylaldehyde-Pd complexes and 5-methyl-2-hydroxyacetophenone oxime-Pd complexes are synthesized. When we apply these two kinds of catalyst to the addition reaction of Chloropropene and Trichlorosilane,The study found that the catalytic activity of two palladium complexes is less than that of the classic "Speier catalyst",and it is to be further studied for other hydrosilylation.4. Two nickel complexes-nickel complexes of Schiff base and 2,5-dihydroxyacetophenone-Ni complexes are synthesized.We apply them to the addition reaction of 3-Chloropropene and Methyldichlorosilane. The study found that the catalytic activity of two nickel complexes is less than that of the classic "Speier catalyst",and in this addition reaction, adding triethylamine "Speier catalyst" can get the best catalytic effect.
Keywords/Search Tags:hydrosilylation, palladium complexes, nickel complexes, catalytic activity, silane coupling agents, 2-(3,4-epoxycyclohexyl)ethyl trimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyl methyldiethoxysilane, Octylmethyldiethoxysilane
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