A kind of 3-cyclohexylthio-1-propyl-triethoxysilane and its preparation method and application

A technology of chloropropyl triethoxy silane and triethoxy silane, which is applied in the field of multifunctional rubber additives, can solve the problem of not improving the chemical bonding effect between silica and rubber matrix to a certain extent, and achieves synthesis The method is simple, the process flow is short, and the cost is reduced.

Active Publication Date: 2018-11-23
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The surface modification of silica currently used includes the use of chlorosilanes, alcohol compounds and silane coupling agents, surface chlorination, surface grafted polymers, Grignard reaction and etherification reaction with epoxides, etc. However, these modification methods can only improve the compatibility between silica and non-polar rubber. This compatibility is a physical effect and does not improve the compatibility between silica and rubber matrix to a certain extent. chemical bonding

Method used

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  • A kind of 3-cyclohexylthio-1-propyl-triethoxysilane and its preparation method and application
  • A kind of 3-cyclohexylthio-1-propyl-triethoxysilane and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0025] Put 11.6g of cyclohexanethiol, 24g of 3-chloropropyltriethoxysilane, 4.1g of sodium hydroxide, and 200g of petroleum ether into a 1000mL three-necked flask, stir and react at 40°C for 2 hours, filter after reaction, and obtain a white Sodium chloride solid 4.7g, filtrate 208g, after filtrate is concentrated to dryness, obtain product 26.4g, measure by HPLC, 3-cyclohexylthio-1-propyl-triethoxysilane content is 95.1% in the product, yield The yield is 82.4%, and the calculation method of the yield is: the quality of the obtained product / theoretical quality of the product, the same below.

Embodiment 2

[0027] Put 11.6g of cyclohexanethiol, 28.9g of 3-chloropropyltriethoxysilane, 4.9g of sodium hydroxide, and 200g of toluene into a 1000mL three-neck flask, stir and react at 60°C for 2 hours, filter after reaction, and obtain a white Sodium chloride solid 4.9g, filtrate 209g, obtain product 27.1g after filtrate is concentrated to dryness, through HPLC measurement, 3-cyclohexylthio-1-propyl-triethoxysilane content is 95.9% in the product, yield The rate is 84.6%.

Embodiment 3

[0029] Put 11.6g cyclohexanethiol, 24g 3-chloropropyltriethoxysilane, 4.1g sodium hydroxide, 0.3g catalyst KI, 200g petroleum ether into a 1000mL three-necked flask, stir and react at 40°C for 2 hours, the reaction After filtration, obtain white sodium chloride solid 5.2g, filtrate 210g, obtain product 28.3g after filtrate is concentrated to dryness, through HPLC determination, 3-cyclohexylthio-1-propyl-triethoxysilane content in the product It was 95.7%, and the yield was 88.3%.

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Abstract

The present invention provides 3-cyclohexyl thio-1-propyl-triethoxysilane, a preparation method therefor and an application thereof. The preparation method comprises: mixing cyclohexyl mercaptan, 3-chloropropyl silane and sodium hydroxide in an organic solvent to be stirred to react so as to generate the 3-cyclohexyl thio-1-propyl-triethoxysilane. The synthesis method disclosed by the present invention is simple, the process is short, very little waste water is generated, environmental pollution is small, and the obtained product is high in yield, and high in purity, so that dispersion and compatibility in rubber products of the white carbon black are improved, a chemical bonding function between silica and the rubber matrix can be improved to a certain extent, overall performance of the rubber products is improved, and when the obtained product is taken as a rubber assistant or a white carbon black modifier, a good application prospect can be ensured.

Description

technical field [0001] The invention relates to a multifunctional rubber auxiliary agent, in particular to a 3-cyclohexylthio-1-propyl-triethoxysilane, a preparation method thereof and an application as a multifunctional rubber auxiliary agent. Background technique [0002] Silica is an important reinforcing filler in the rubber industry, and has obvious advantages over carbon black. Due to the presence of a large number of silanol hydroxyl groups on the surface of silica, it will produce strong moisture absorption and easy to cluster, and has poor compatibility with hydrocarbon rubber, resulting in poor dispersion. Therefore, the surface modification of silica has become a research hotspot in the field of rubber. The surface modification of silica currently used includes the use of chlorosilanes, alcohol compounds and silane coupling agents, surface chlorination, surface grafted polymers, Grignard reaction and etherification reaction with epoxides, etc. However, these mod...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C08K5/548
Inventor 张琳李剑波王才朋
Owner SHANDONG YANGGU HUATAI CHEM
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