Study On The Preparation Of 1-Chloromethylsilatrane From Methyltrichlorosilane

Methyltrichlorosilane (CH3SiCl3) is one of the main by-products for the synthesis of methyl chlorosilane by "direct method", accounting for 5%～15% of the total products. Currently, methyltrichlorosilane is mainly used to prepare silica or transformed into other useful silane at home and abroad. Some domestic enterprises also used methyl trichlorosilane for the preparation of silane coupling agent, methyl silicone resin and water-proofing agent and so on.In this paper,1-chloromethylsilatrane, which posses broad spectrum of biological activities, was prepared from methyltrichlorosilane by chloration. Also, a series of studies on the optimization of technological conditions were investigated, which laying the foundation for broadening the applications of methyl trichlorosilane. The main work of this paper is as follows:1. In order to increase the yields of the products and transform the by-product into raw materials or environmentally-friendly materials, the hydrogen chloride gas absorption device were designed.2. The chlorination reaction of methyltrichlorosilane was optimized and the effects of reaction conditions on the yield of 1-chloromethyl silatrane were studied. The optimum condition of the reaction was obtained as follow:the reaction temperature of the chlorination reaction should be controlled at 68～72℃and the reaction time should be 12 hours; Ethanol was added after the reaction and the appropriate molar ratio of ethanol to methyltrichlorsilane was 2.5:1; When 151g (lmol) methyltrichlorosilane was added to the reaction flask, the highest yield of 1-chloromethyl silatrane of 64.5% can be obtained while 0.75 mol triethanolamine was added.3. Hydrogen chloride gas produced from the alcoholysis reaction can be made into chlorine gas after chlorination and oxidation reaction. The reaction conditions of the chlorination and oxidation reaction were studied. Also, the effects of the category of catalysts and reaction conditions on the reaction behaviors were investigated. 4. The white solid powder which has a melting point of 221～223℃was obtained after recrystallization and the drying procedure. IR,'HNMR and other measurements were used to verify the structure of the product which confirm that 1-chloromethyl silatrane was obtained. Biological activity of the product was further investigated and studied in some degree.