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Method for preparing hydrolysate of mixture of N-propyltrimethoxysilane and ethyl orthosilicate

A technology of propyltrimethoxysilane and ethyl orthosilicate is applied in the field of preparation of N-propyltrimethoxysilane and ethyl orthosilicate mixture hydrolyzate, and can solve the problem of low methanol and ethanol content, self-polymerization Cross-linking affects the activity and other problems, and achieves the effect of strong coupling activity, increased lipophilicity, and good storage stability

Active Publication Date: 2014-11-19
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of strong coupling activity, good storage stability, low content of methanol and ethanol, to solve the problem that the existing N-propyltrimethoxysilane is easy to self-polymerize and cross-link directly when used directly in the water-based system. Preparation method of hydrolyzate of N-propyltrimethoxysilane and ethyl orthosilicate mixture affecting its activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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 gla...

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...

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Abstract

The invention relates to a method for preparing hydrolysate of a mixture of N-propyltrimethoxysilane and ethyl orthosilicate and belongs to the technical field of fine chemical engineering. According to the method, a mixture of propyltrimethoxysilane and ethyl orthosilicate is subjected to prehydrolysis under certain conditions, so that most of methoxy groups and oxyethyl groups in the molecules of N-propyltrimethoxysilane and ethyl orthosilicate are hydrolyzed into silanol (Si-OH), condensation polymerization of silanol into siloxane is inhibited, and the problem that N-propyltrimethoxysilane is untimely crosslinked in an aqueous system in the prior art is solved. The product prepared by the method has the characteristics of high coupling activity, high storage stability and low methanol content and can be directly applied to glass fiber reinforcement, water-based paint tackifying and other aqueous systems.

Description

technical field [0001] The invention relates to a method for preparing a hydrolyzate of a mixture of N-propyltrimethoxysilane and ethyl orthosilicate, belonging to the technical field of fine chemicals. Background technique [0002] Propyltrimethoxysilane is a practical silane coupling agent, which can couple with resin and is an important basic raw material for processing sol-gel. It is widely used in glass fiber reinforcement, resin surface modification, surface active The lipophilicity of the material adds organic properties to the silicone network, but in some water-based systems, its actual use effect is often not ideal. If N-propyltrimethoxysilane is added to the water-based system in proportion according to the conventional use method, its storage life is very short, generally no more than one week, and it needs to be added again after a period of time, so it needs to be added immediately in the actual application process. It can be used immediately after mixing, oth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5415C08K3/36C09D7/12C07C29/09C07C31/04C07C31/08
Inventor 吴兵兵刘明锋阮少阳甘俊陈圣云甘书官
Owner JINGZHOU JIANGHAN FINE CHEM