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Method for preparing 3-aminopropyl triethoxy silane hydrolysate

A technology of aminopropyltriethoxysilane and hydrolyzate, which is applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of self-polymerization crosslinking failure and poor storage stability, and achieve coupling Strong activity, low ethanol content, good storage stability

Active Publication Date: 2014-03-12
JINGZHOU JIANGHAN FINE CHEM
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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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  • Method for preparing 3-aminopropyl triethoxy silane hydrolysate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 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 heat up to 20°C, then start stirring at a stirring speed of 80 rpm. Under the condition of revolutions per minute, 400 g of 3-aminopropyltriethoxysilane with a content of 98.5% and a colorless and transparent appearance was added dropwise into a four-necked flask for hydrolysis reaction, and the dropping time was controlled at 2 hours. After the dropwise addition, the temperature was raised to 60° C. to continue the reaction for 2 hours, and the temperature was lowered to below 30° C. after the reaction was completed.

[0021] Add the material obtained by the reaction into a 2000ml three-necked flask with a fractionating tower, a thermometer and oil bath heating. The fractionating tower is a glass packed tower with a length of 400 mm and an inner diameter of 10 mm, filled with glass spring packing. Under the ...

Embodiment 2

[0024] 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 heat up to 60°C, then start stirring at a stirring speed of 300 rpm. Under the stirring condition of 300 rpm, 500 g of 3-aminopropyltriethoxysilane with a content of 98.5% and a colorless and transparent appearance was added dropwise into a four-necked flask, and the dropping time was controlled to be 6 hours. After the dropwise addition, the temperature was raised to 80° C. to continue the reaction for 3 hours, and the temperature was lowered to below 30° C. after the reaction was completed.

[0025] Add the material obtained by the reaction into a 2000ml three-necked flask with a fractionating tower, a thermometer and oil bath heating. The fractionating tower is a glass packed tower with a length of 400 mm and an inner diameter of 10 mm, filled with glass spring packing. Under the condition of normal pressu...

Embodiment 3

[0028] 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 heat up to 50°C, then start stirring at a stirring speed of 200 rpm. 600 g of 3-aminopropyltriethoxysilane with a content of 98.5% and a colorless and transparent appearance was added dropwise into a four-necked flask, and the dropping time was controlled to be 5 hours. After the dropwise addition, the temperature was raised to 70° C. to continue the reaction for 2 hours, and the temperature was lowered to below 30° C. after the reaction was completed.

[0029] Add the material obtained by the reaction into a 2000ml three-necked flask with a fractionating tower, a thermometer and oil bath heating. The fractionating tower is a glass packed tower with a length of 400 mm and an inner diameter of 10 mm, filled with glass spring packing. Under the condition of normal pressure 101.3Kpa, the by-product ethanol produ...

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Abstract

The invention relates to a method for preparing 3-aminopropyl triethoxy silane hydrolysate and belongs to the technical field of fine chemical engineering. The method comprises the following steps of: performing prehydrolysis on 3-aminopropyl triethoxy silane under a certain condition to ensure that most oxethyls in 3-aminopropyl triethoxy silane molecules are hydrolyzed to form silanol (Si-OH), and the polycondensation of silanol into siloxane can be inhibited. The problem that the conventional 3-aminopropyl triethoxy silane is crosslinked too early in an aqueous system can be solved; and a product prepared by the method has the characteristics of strong coupling activity, high storage stability and low ethanol content, can be directly applied to aqueous systems that glass fibers are enhanced, waterborne polyurethane is modified, and water-based paint is tackified.

Description

technical field [0001] The invention relates to a method for preparing a 3-aminopropyltriethoxysilane hydrolyzate, belonging to the technical field of fine chemicals. Background technique [0002] 3-Aminopropyltriethoxysilane (KH550) is a general-purpose silane coupling agent, which can almost 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 directly added to the water-based system in proportion according to the conventional use method, its storage life is very short, generally not 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 be gradually lost with the prolongation of storage time, which will bring difficulties to the application o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/00
Inventor 阮少阳陈圣云刘明锋吴兵兵王欣胡江华王灿甘书官
Owner JINGZHOU JIANGHAN FINE CHEM