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ChemicalBook CAS DataBase List Tetramethyl orthosilicate
681-84-5

Tetramethyl orthosilicate synthesis

14synthesis methods
Silica aerogels are usually prepared by base-catalyzed reaction of tetramethoxysilane or tetraethoxysilane, mostly with ammonia as the catalyst. A modification of this procedure is to prehydrolyze Si(OR)4 with a small amount of water under acidic conditions.
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Yield:681-84-5 96.8%

Reaction Conditions:

with nickel(II) sulphate;tetrachlorosilane;trichlorosilane in tetrachloromethane at 55 - 60; for 3 h;Large scale;

Steps:

3 Example 3

In 3000L, with DN400*14000 glass-lined tower (tower filling), with circulating water cooling,In a glass-lined reactor with steam heating and stirring,Add the main components of 25% trichlorosilane, 60% silicon tetrachloride,1400 kg of organic silicon by-product of 15% carbon tetrachloride is added, and 1000 ppm of catalyst nickel sulfate is added. Keep the tail gas system pressure at -5kPa, and add 1100kg of methanol to the kettle through the bottom of the kettle.Control the dripping rate of 340kg/hr, and control the temperature to 55 during the dripping process. After the dripping is completed,The temperature was raised to 60°C and the reaction was continued for 3 hours. The by-product hydrogen chloride in the dropping reaction process enters the falling film absorption system to produce hydrochloric acid. After the reaction, the materials are neutralized,There is no trimethoxyhydrosilane in the detected product, and the dehydrogenation of trichlorosilane is complete;After rectification, 1110 kg of tetramethoxysilane product with a purity of 98.4% was obtained, with a yield of 96.8%.200 kg of carbon tetrachloride with a purity of 98% was obtained.

References:

CN111303198,2020,A Location in patent:Paragraph 0024

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