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ChemicalBook CAS DataBase List Tetraethyl orthosilicate

Tetraethyl orthosilicate synthesis

12synthesis methods
Prepared from absolute alcohol and silicon tetrachloride.
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Yield:78-10-4 99%

Reaction Conditions:

with ethyl silicate 40;silicon at 150 - 180; under 760.051 Torr;Inert atmosphere;Concentration;

Steps:

3 Example 1

General procedure: Silicon metal powder, potassium ethoxide and ethyl silicate 40 were put into a 500 ml reactor 10, and the mixture was stirred at 150 to 180 ° C for 4 hours to 8 hours under nitrogen atmosphere and 1 atm, . At this time, the weight of the silicon metal powder is preferably 50 g, the average particle diameter is 20 , the potassium ethoxide is 1.12 g, the number of gaseous molecules is 0.02 mol, and the amount of ethyl silicate is preferably 0.2 mol to 56 g. The ethyl silicate is also available as an alkyl silicate.After the reaction is carried out by stirring the mixture, excess components in components (silicon metal powder, potassium ethoxide) composed of the mixture are removed by vacuum distillation. Thereafter, the temperature is increased up to 220 ° C, and the boiling point of the ethyl silicate 40 is 236 ° C, so that the boiling point of the ethyl silicate 40 is prevented from further boiling. Thus, ethyl silicate 40 serves to allow the mixture to withstand high temperatures. Anhydrous ethanol is synthesized in the mixture. The anhydrous ethanol is injected at a rate of 1 liter per hour using a metering pump (not shown). The boiling point of ethyl silicate is about 166 ° C. by adding anhydrous ethanol. The anhydrous ethanol is added to the mixture of the reactor 10 to proceed the synthesis, thereby preventing the solution from boiling and overflowing. The ethyl silicate produced in this manner is not overflowed and is passed to the condenser 20 formed on the side surface and the mixture delivered to the condenser 20 is condensed and accumulated in the storage tank 30. The mixture accumulated in the storage tank 30 was further separated into ethanol and ethyl silicate through the distillation column 40 to obtain 20 g of ethyl silicate. (Yield: 99%).

References:

KR2015/97319,2015,A Location in patent:Paragraph 0055; 0056

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