A kind of preparation method of n-propyltrimethoxysilane and ethyl orthosilicate mixture hydrolyzate
A technology of propyltrimethoxysilane and ethyl orthosilicate, which is applied in the field of preparation of the hydrolyzate mixture of N-propyltrimethoxysilane and ethyl orthosilicate, can solve the problem of self-polymerization crosslinking affecting activity, Solve problems such as low content of methanol and ethanol, achieve the effect of increasing lipophilicity, strong coupling activity, and good storage stability
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Embodiment 1
[0015] In a 2000m1 glass four-neck reaction flask with mechanical stirring, spherical reflux condenser, thermometer and oil bath heating, add 1000g of distilled water and raise the temperature to 20°C, then start stirring at a stirring speed of 80 rpm. Under the condition of revolution per minute, according to the molar ratio of 4:6mol, 500g of colorless and transparent N-propyltrimethoxysilane and tetraethyl orthosilicate mixture was added dropwise into a four-necked flask for hydrolysis reaction. Control is 2 hours. After the dropwise addition, heat up to 60°C to continue the reaction for 2 hours, and then lower the temperature to below 30°C after the reaction to obtain a first-grade crude product of the hydrolyzate of the mixture of N-propyltrimethoxysilane and ethyl orthosilicate.
[0016] Add the primary crude product obtained by the reaction into a 2000m1 three-neck flask with a fractionating tower, a thermometer and oil bath heating. The fractionating tower is a glass p...
Embodiment 2
[0019] In a 2000ml glass four-necked reaction flask with mechanical stirring, spherical reflux condenser, thermometer and oil bath heating, add 1000g of distilled water and raise the temperature to 60°C, then start stirring at a stirring speed of 300 rpm. According to the molar ratio of 4:6mol, 400g of colorless and transparent N-propyltrimethoxysilane and tetraethyl orthosilicate mixture was added dropwise to the four-necked flask under the stirring condition of 300 rpm, and the dropping time Control is 6 hours. After the dropwise addition, heat up to 80°C to continue the reaction for 3 hours, and then cool down to below 30°C after the reaction to obtain a first-grade crude product of the hydrolyzate of the mixture of N-propyltrimethoxysilane and ethyl orthosilicate.
[0020] Add the primary crude product obtained by the reaction into a 2000m1 three-neck flask with a fractionating tower, a thermometer and oil bath heating. The fractionating tower is a glass packed tower with ...
Embodiment 3
[0023] In a 2000ml glass four-neck reaction flask with mechanical stirring, spherical reflux condenser, thermometer and oil bath heating, add 1000g of distilled water and raise the temperature to 50°C, then start stirring at a stirring speed of 200 rpm. According to the molar ratio of 4:6mol, 600g of a colorless and transparent mixture of N-propyltrimethoxysilane and ethyl orthosilicate was added dropwise into a four-necked flask, and the dropping time was controlled to be 5 hours. After the dropwise addition, heat up to 70°C to continue the reaction for 2 hours, and then lower the temperature to below 30°C after the reaction to obtain a primary crude product of the hydrolyzate of the mixture of N-propyltrimethoxysilane and ethyl orthosilicate.
[0024] Add the primary crude product obtained by the reaction into a 2000m1 three-neck flask with a fractionating tower, a thermometer and oil bath heating. The fractionating tower is a glass packed tower with a length of 400mm and an ...
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