Method for manufacturing phenoxy trimethyl silicone hydride compounds
A phenoxytrimethylsilane, a technology for a manufacturing method, applied in chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, organic compounds/hydrides/coordination complex catalysts, etc. Problems such as the production method of phenoxytrimethylsilane compound to achieve the effect of high productivity, simple process and stable quality
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Embodiment 1
[0029] Preparation of Phenoxytrimethylsilane from Phenol
[0030] Add 147g of phenol into the reaction vessel equipped with constant temperature circulating oil heating in the jacket, mechanical stirring, dropping device, tail gas absorption tower, and overhead reflux device, then raise the temperature to 80°C, and add 140g of hexamethyldisilazane dropwise , the ammonia gas generated enters the tail gas absorption tower through the reflux device, and the reaction system is slightly positive pressure in the whole process. After the dropwise addition, it is kept warm for 6 hours, and it is found that 60% of the phenol has no reaction, and the heat preservation is continued for 5 hours. 58% of the phenol did not react, and the temperature was increased to 120-130° C. for 5 hours, and 50% of the phenol remained unconverted. Further prolonging the time, increasing the amount of hexamethyldisilazane and increasing the reaction temperature cannot significantly increase the conversion...
Embodiment 2
[0033] Phenoxytrimethylsilane was prepared from phenol, and the whole reaction process was carried out under the protection of nitrogen.
[0034] Add 147g phenol in the reaction vessel equipped with constant temperature circulating oil heating in the jacket, mechanical stirring, dripping device, tail gas absorption tower, tower top reflux device, then heat up to 80 ° C, add 3g strong acid type cation exchange resin as a catalyst, Stir evenly, then add 140g of hexamethyldisilazane dropwise, and the generated ammonia gas enters the tail gas absorption tower through the reflux device. During the whole process, the reaction system is under a slight positive pressure. After the dropwise addition, react at 120-130°C for 5 Hours, the phenol conversion rate was 100%, but the product was neutral. After the resin was filtered out, the reaction solution was flash evaporated. The content of the product obtained was 99.5%, and the quality of the product was 235g.
[0035] This example prov...
Embodiment 3
[0037] Preparation of phenoxytrimethylsilane from p-methylphenol.
[0038] Add 165g of p-cresol to the reaction vessel equipped with constant temperature circulating oil heating in the jacket, mechanical stirring, dropping device, tail gas absorption tower and tower top reflux device, then heat up to 70-80°C, and add 3g of strong acid cation The exchange resin is used as a catalyst, stirred evenly, and then 140g of hexamethyldisilazane is added dropwise, and the ammonia gas generated enters the tail gas absorption tower through a reflux device. During the whole process, the reaction system is under a slight positive pressure. After reacting at -80°C for 5 hours, the conversion rate of p-cresol was 100%. After the resin was filtered off, the reaction solution was flash evaporated to obtain 241 g of finished product with a purity of 99.5%.
[0039] This example proves that if the exchange resin is used as a catalyst, the reaction for preparing phenoxytrimethylsilane from p-creso...
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