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Technology for preparing terminated-type sulfur-containing silane coupling agent through hydrosilation method

A technology of sulfur silane coupling agent and hydrosilicon addition, which is applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., can solve the problems affecting storage stability, alkoxysilane Unstable water, prone to hydrolysis and other problems, to achieve the effect of improving raw material utilization, improving storage stability, and inhibiting hydrolysis

Active Publication Date: 2014-04-09
江西晨光新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the current common preparation methods of end-capped sulfur-containing silane coupling agents, the organic solvent method needs to use 3-mercaptopropyltrialkoxysilane as a raw material, but the production yield of 3-mercaptopropyltrialkoxysilane is low , relatively cumbersome; on the other hand, the end-capped sulfur-containing silane coupling agent can also be synthesized by hydrolysis, but the alkoxysilane is unstable to water and is prone to hydrolysis, and it is also easy to bring water into the product, affecting its storage stability

Method used

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  • Technology for preparing terminated-type sulfur-containing silane coupling agent through hydrosilation method
  • Technology for preparing terminated-type sulfur-containing silane coupling agent through hydrosilation method
  • Technology for preparing terminated-type sulfur-containing silane coupling agent through hydrosilation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) Preparation of allyl thiooctanoate (C 7 h 15 COSCH 2 -CH=CH 2 )

[0025] In a 2L three-neck flask protected by nitrogen, add 240g (1mol) of sodium sulfide nonahydrate solid, add 150g of water, and dissolve to obtain a sodium sulfide solution with a concentration of 20%. Under mechanical stirring, 162.5g (1mol) of octanoyl chloride is added from The constant pressure dropping funnel was added dropwise, and the dropwise addition was completed in about 30 minutes. With the addition of octanoyl chloride, the temperature in the bottle rose to about 70°C. The system was naturally cooled to room temperature, and after stirring for 4 hours, a slightly viscous mixture was obtained. Thick aqueous solution of sodium lipoate. Add 3g of saturated methyltrioctylammonium chloride solution to the above solution, add 80.3g (1.05mol) of 3-chloropropene into the bottle under mechanical stirring, after completion, raise the temperature and keep it at a slight reflux for 5 hours, and...

Embodiment 2

[0029] 1) Preparation of allyl thiohexanoate (C 7 h 15 COSCH 2 -CH=CH 2 )

[0030] In a 2L three-necked flask protected by nitrogen gas, 622g of 18% sodium hydrosulfide aqueous solution (containing 102g of sodium hydrogensulfide, 2mol), under mechanical stirring, 134.5g (1mol) of hexanoyl chloride was dropped from a constant pressure dropping funnel to produce The hydrogen sulfide gas was absorbed with sodium hydroxide solution, and the dropwise addition was completed in about 30 minutes. After stirring at 60° C. for 3 hours, it was cooled to room temperature to obtain a slightly viscous aqueous solution of sodium thiohexanoate. Add 0.5 g of tetrabutylammonium bromide to the above solution, add 80.3 g (1.05 mol) of 3-chloropropene into the bottle under mechanical stirring, control the heating temperature, keep a slight reflux for 5 hours, and detect the organic phase by gas chromatography. - The chloropropene content is less than 3%, stop stirring, separate the upper organ...

Embodiment 3

[0034] 1) Preparation of allyl thiolaurate (C 11 h 23 COSCH 2 -CH=CH 2 )

[0035] In a 2L three-neck flask protected by nitrogen, add 130g (1mol) of sodium sulfide solid with a sodium sulfide content of 60%, add 520g of water, and dissolve to obtain a sodium sulfide solution with a concentration of 12%. Under mechanical stirring, mix 218.5g (1mol) ) Lauroyl chloride was added dropwise from a constant pressure dropping funnel, and the dropwise addition was completed in about 40 minutes, stirred at 75°C for 3 hours, cooled to room temperature, and a slightly viscous aqueous solution of sodium thiolaurate was obtained. Add 2g of trimethyldodecyl ammonium chloride to the above solution, and add 80.3g (1.05mol) of 3-chloropropene into the bottle under mechanical stirring. After completion, raise the temperature and maintain a slight reflux for 5 hours. The 3-chloropropene content is less than 3%, stop stirring, separate the upper organic layer, remove the low boiling point unde...

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Abstract

Provided is a technology for preparing a terminated-type sulfur-containing silane coupling agent through a hydrosilation method. First, acyl chloride and sodium sulfide or sodium bisulfide are reacted in a water phase to prepare an aqueous solution of sodium thiocarboxylate; under catalysis of phase-transfer catalysts, the aqueous solution of sodium thiocarboxylate is reacted with chloropropene, and thiocarboxylate allyl ester, liquid separation is carried out, after low-boiling-point substance removal, thiocarboxylate allyl ester and trialkoxysilane are subjected to a hydrosilation reaction under action of platinum catalysts, and after the reaction is over, a finished product silane coupling agent is obtained after low-boiling-point substance removal and decolouring steps. The raw material utilization rate is raised, The hydrosilation reaction process keeps anhydrous state, hydrolysis of alkoxy silane is inhibited, and the storage stability of the silane coupling agent is raised.

Description

technical field [0001] The invention relates to a process for preparing end-blocking sulfur-containing silane coupling agent by a hydrosilylation method. Background technique [0002] Sulfur-containing silane coupling agents are widely used in the rubber industry. With the development of the automobile industry, the demand for silane coupling agents is also increasing year by year. At present, the sulfur-containing silane coupling agent that has been widely used is polysulfide silane. Such as bis-[3-(triethoxysilyl)propyl]-tetrasulfide (trade name Si-69), these sulfur-containing silane coupling agents can significantly improve the tensile strength, wear resistance, However, the polysulfide bond of polysulfide silane is easy to break at high temperature, especially in the mixing stage of rubber, polysulfide silane is easy to break early and cause rubber vulcanization in advance, resulting in a decline in rubber performance. Blocked sulfur-containing silane coupling agents ca...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 丁建峰梁秋鸿葛利伟周煜华
Owner 江西晨光新材料股份有限公司
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