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Preparation method of 3-aminopropyl triethoxysilane

A technology of aminopropyltriethoxysilane and thermometers, applied in chemical instruments and methods, silicon organic compounds, compounds of group 4/14 elements of the periodic table, etc., can solve the problem of self-polymerization crosslinking failure and storage stability No problem, such as strong coupling activity, low ethanol content, and good storage stability

Inactive Publication Date: 2019-09-13
湖北华欣有机硅新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a kind of strong coupling activity, good storage stability, low ethanol content, to solve the existing 3-aminopropyltriethoxysilane used directly in the water-based system, which is prone to premature self-polymerization and cross-linking failure 3-Aminopropyltriethoxysilane hydrolyzate with poor storage stability and ethanol release problem and preparation method thereof

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 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 20℃, then turn on the stirring, the stirring speed is 80 revolutions per minute, when the stirring speed is 80 Under the condition of revolution per minute, 400 g of 3-aminopropyltriethoxysilane with a content of 98.5% and a colorless and transparent appearance was dropped into a four-necked flask for hydrolysis reaction, and the dropping time was controlled to 2 hours. After the dropwise addition is completed, the temperature is increased to 60°C to continue the reaction for 2 hours, and the temperature is lowered to below 30°C after the reaction is completed.

[0021] The materials obtained from the reaction are added to a 2000ml three-necked flask heated by a fractionating tower, a thermometer and an oil bath. The fractionating tower is a glass packed tower with a length of 400 mm an...

Embodiment 2

[0024] 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 turn on the stirring at 300 revolutions per minute. Under stirring conditions of 300 revolutions per minute, 500 g of 3-aminopropyltriethoxysilane with a content of 98.5% and a colorless and transparent appearance was dropped into the four-necked flask, and the dropping time was controlled to 6 hours. After the dropwise addition is completed, the temperature is increased to 80°C to continue the reaction for 3 hours, and the temperature is lowered to below 30°C after the reaction is completed.

[0025] The materials obtained from the reaction are added to a 2000ml three-necked flask heated by a fractionating tower, a thermometer and an oil bath. The fractionating tower is a glass packed tower with a length of 400 mm and an inner diameter of 10 mm, and is filled with glass spri...

Embodiment 3

[0028] In a 2000ml glass four-necked reaction flask with mechanical stirring, spherical reflux condenser, thermometer and oil bath heating, add 1000g distilled water and raise the temperature to 50°C, then turn on the stirring at 200 revolutions per minute. 600 g of 3-aminopropyltriethoxysilane with a content of 98.5% and a colorless and transparent appearance was dropped into the four-necked flask, and the dropping time was controlled to 5 hours. After the dripping is completed, the temperature is increased to 70°C and the reaction is continued for 2 hours, and the temperature is lowered to below 30°C after the reaction is completed.

[0029] The materials obtained from the reaction are added to a 2000ml three-necked flask heated by a fractionating tower, a thermometer and an oil bath. The fractionating tower is a glass packed tower with a length of 400 mm and an inner diameter of 10 mm, and is filled with glass spring packing. Under normal pressure of 101.3Kpa, heating will fra...

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Abstract

Belonging to the technical field of fine chemical industry, the invention relates to a preparation method of 3-aminopropyl triethoxysilane. Specifically, 3-aminopropyl triethoxysilane is subjected toprehydrolysis under certain condition to hydrolyze most ethoxy in 3-aminopropyl triethoxysilane molecule into silanol (Si-OH), and polycondensation of silanol into siloxane is inhibited, thus solvingthe problem of premature crosslinking of existing 3-aminopropyl triethoxysilane in an aqueous system. The product prepared by the technology provided by the invention has the characteristics of strongcoupling activity, good storage stability and low ethanol content, and can be directly applied to glass fiber reinforcement, waterborne polyurethane modification, waterborne paint tackifying and other waterborne systems.

Description

Technical field [0001] The invention relates to a preparation method of 3-aminopropyltriethoxysilane, belonging to the technical field of fine chemicals. Background technique [0002] 3-Aminopropyltriethoxysilane (KH550) is a general-purpose silane coupling agent, which can couple with various resins, and is widely used in glass fiber reinforcement, resin surface modification, textile finishing, etc. , But in some water-based systems, its actual use effect is often not ideal. [0003] If 3-aminopropyltriethoxysilane is used in the usual way and directly added to the aqueous system in proportion, 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 in the actual application process It needs to be prepared and used immediately, otherwise the coupling effect will gradually lose with the extension of storage time, which will bring difficulties to the application of the product in aqueous systems. [0004] 3-Aminoprop...

Claims

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Application Information

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IPC IPC(8): C07F7/08
CPCC07F7/0836
Inventor 夏正东李新春
Owner 湖北华欣有机硅新材料有限公司