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Preparation method of 3-mercaptopropyltriethoxysilane coupling agent

A mercaptopropyl triethoxy silane coupling agent, chloropropyl triethoxy silane technology, applied in the field of preparation of 3-mercaptopropyl triethoxy silane coupling agent, can solve guanidine salts and products Great odor, high production safety risk, large environmental pollution and other problems, to achieve the effect of small product odor, safe production process, and simple production process

Active Publication Date: 2013-11-27
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The main shortcoming of above-mentioned two kinds of production methods is: the amount of by-product guanidinium salt produced by the former process is relatively large, the guanidinium salt and product odor are big, and the pollution to environment is bigger; The hydrogen sulfide gas used in the latter process is A highly toxic gas with high production safety risks and potential safety hazards

Method used

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  • Preparation method of 3-mercaptopropyltriethoxysilane coupling agent

Examples

Experimental program
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Effect test

Embodiment 1

[0021] In a 3000ml four-neck flask, install a condenser, a mechanical stirrer, a thermometer and a water bath heating pot. Put 480 g of flaky sodium hydrosulfide solids with a mass content of 70% and 600 g of tap water into a flask, and stir at room temperature for 10 minutes to dissolve the sodium hydrosulfide to form a yellow transparent sodium hydrosulfide aqueous solution. Then heat up to 60~65°C, put 95g of sodium bicarbonate powder into the flask and stir for 5 minutes, after the sodium bicarbonate is dissolved, the pH of the reaction system is 9~10. Continue to heat up to 80~85°C, add 45g of benzyltributylammonium chloride as a phase transfer catalyst, add 1450g of 3-chloropropyltriethoxysilane dropwise at 80~85°C and stir for reaction, 3- The dropping time of chloropropyltriethoxysilane is about 2 hours. After the dropwise addition, the reaction was continued for 8 hours, and the crude product of the upper organic phase was detected by gas chromatography. At this time...

Embodiment 2

[0024] In a 3000ml four-neck flask, install a condenser, a mechanical stirrer, a thermometer and a water bath heating pot. Put 480g of sodium hydrosulfide with a mass content of 73% and 700g of tap water into the flask, stir at room temperature for 10 minutes, and dissolve the sodium hydrosulfide to form a yellow transparent sodium hydrosulfide aqueous solution. Then heat up to 70~75°C, drop 110g of sodium bicarbonate powder into the flask and stir for 5 minutes, after the sodium bicarbonate dissolves, the pH of the reaction system is 9~10; continue to heat up to 85~90°C, add 50g of benzyl tri Butyl ammonium chloride is used as a phase transfer catalyst, and 1450g of 3-chloropropyltriethoxysilane is added dropwise at 85~90°C and stirred for reaction, and the dropping time of 3-chloropropyltriethoxysilane is 2.5 hours or so. After the dropwise addition, the reaction was continued for 10 hours, and the crude product of the upper organic phase was detected by gas chromatography....

Embodiment 3

[0027] In a 3000ml four-neck flask, install a condenser, a mechanical stirrer, a thermometer and a water bath heating pot. Put 480 g of sodium hydrosulfide solid with a mass content of 73% and 800 g of tap water into the flask, and stir at room temperature for 10 minutes to dissolve the sodium hydrosulfide to form a yellow transparent sodium hydrosulfide aqueous solution. Then heat up to 80~85°C, put 120g of sodium bicarbonate powder into the flask and stir for 5 minutes, after the sodium bicarbonate dissolves, the pH of the reaction system is 9~10; after continuing to heat up to 88~90°C, add 50g of hexadecane Trimethylammonium chloride was used as a phase transfer catalyst, and 1450g of 3-chloropropyltriethoxysilane was added dropwise under the condition of 88~90℃ to stir the reaction, and the dropping time of 3-chloropropyltriethoxysilane for about 3 hours. After the dropwise addition, the reaction was continued for 12 hours, and the crude product of the upper organic phase...

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Abstract

The invention relates to a preparation method of a 3-mercaptopropyltriethoxysilane coupling agent, belonging to the technical field of organic chemistry. The preparation method comprises the following steps of: with sodium hydrosulfide and 3-chloropropyltriethoxysilane as raw materials and water as a solvent, heating, stirring and reacting under the action of a phase transfer catalyst to obtain a crude product of silane; and drying the crude product, filtering and distilling to obtain the 3-mercaptopropyltriethoxysilane coupling agent product. The preparation method is simple in process, lower in production cost, high in product yield, little in odor, safe, environment-friendly and easy to realize large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of a 3-mercaptopropyltriethoxysilane coupling agent, which belongs to the technical field of organic chemistry. Background technique [0002] 3-Mercaptopropyltriethoxysilane coupling agent is a sulfur-containing silane coupling agent with mercapto functional groups. It is used for the surface treatment of gold, silver, copper and other metals, which can enhance the corrosion resistance and oxidation resistance of the surface and increase its adhesion with polymers such as resins. In the rubber industry, it is often used to treat inorganic fillers such as white carbon black, carbon black, glass fiber, and mica, which can effectively improve the mechanical properties and wear resistance of rubber. It can be used for anti-shrinkage finishing of fabrics in textile. [0003] At present, there are mainly two processes for the production of 3-mercaptopropyltriethoxysilane in China. One technique is: use the bak...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 王灿靳军王欣陈圣云甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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