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A kind of environment-friendly production method of high-quality 3-octanoylthio-1-propyltriethoxysilane

A technology of propyltriethoxysilane and chloropropyltriethoxysilane, which is applied in the field of 3-octanoylthio-1-propyltriethoxysilane and can solve harmful catalysts and catalyst decomposition products and the like Impurity residue and other problems, to achieve the effect of light appearance, high product quality and less transition layer

Active Publication Date: 2021-11-05
南京曙光新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Technical problem: The object of the present invention is to provide an environmentally friendly production method of high-quality 3-octanoylthio-1-propyltriethoxysilane, and to solve the technology of residual harmful impurities such as catalysts and catalyst decomposition products in products Problems, reduce the amount of sticky matter caused by product hydrolysis and other reasons, reduce the platinum cobalt color number of the product, improve product quality, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] The first step: prepare the crude product of sodium thiooctanoate aqueous solution

[0072] Put 276g of sodium sulfide nonahydrate (1.15mol, 0.01% iron content) and 150g of water into a four-necked flask equipped with a thermometer, a stirrer and a feeding port, raise the temperature to 50°C, and add 20% of tetrapropylene at one time 22 g of ammonium bromide aqueous solution, 162.5 g of octanoyl chloride (1 mol) was added dropwise, and kept at 48°C-50°C for 0.5h to obtain a crude aqueous solution of sodium thiooctanoate.

[0073] The second step: preparation of crude 3-octanoylthio-1-propyltriethoxysilane

[0074] The crude sodium thiooctanoate aqueous solution was heated up to 80° C., 44 g of 20% tetrapropylammonium bromide aqueous solution was added at one time, and 290 g of 3-chloropropyltriethoxysilane (1.18 mol, content of 98%, The impurity polymer is 0.9%), and kept at 80°C-82°C for 4h to obtain the crude sodium thiooctanoate aqueous solution.

[0075] Step Thre...

Embodiment 2

[0092] The sodium sulfide nonahydrate in Example 1 is replaced with a low-iron type, and the iron element content is 0.001%, and the other steps are all the same as in Example 1. In the third step of phase separation, the transition layer is a thin layer with clear boundaries between the three phases, and there is no viscous hanging on the wall in the transition layer.

[0093] The test results of the product: the appearance is light yellow transparent liquid, the content of 3-octanoylthio-1-propyltriethoxysilane monomer is 93.8%, 3-octanoylthio-1-propyltriethoxy The silane polymer content is 1.8%, the tripropylamine content is 0, the platinum cobalt color number is 75, and the ammonia nitrogen content is 0.

Embodiment 3

[0095] The 3-chloropropyl triethoxysilane in embodiment 1 is replaced with low content, wherein the 3-chloropropyl triethoxysilane content is 93.5%, the impurity polymer content is 3%, and other steps are operated with Example 1 is the same. In the third step of phase separation, the transition layer is a thin layer with clear boundaries between the three phases, and there is no viscous hanging on the wall in the transition layer.

[0096] Test results of the product: the appearance is light yellow transparent liquid, the content of 3-octanoylthio-1-propyltriethoxysilane monomer is 91.0%, 3-octanoylthio-1-propyltriethoxy The silane polymer content is 2.2%, the 3-chloropropyltriethoxysilane polymer content is 2.8%, the tripropylamine content is 0, the platinum cobalt color number is 97, and the ammonia nitrogen content is 0.

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Abstract

The invention discloses an environment-friendly production method of high-quality 3-octanoylthio-1-propyltriethoxysilane, which comprises making Sodium thiooctanoate reacts with 3-chloropropyltriethoxysilane in the presence of tetrapropylammonium bromide to produce 3-octanoylthio-1-propyltriethoxysilane reaction product, and from this reaction Part or all of the tetrapropylammonium bromide is removed from the product to obtain a light yellow transparent liquid 3-octanoylthio-1-propyltriethoxysilane, and the transition layer is less to almost no transition layer in the production process, which is easy to carry out Phase separation, no viscous by-products, high monomer purity, low polymer content, light product color, no catalyst or catalyst decomposition product residue, high product quality, is a high-quality 3-octanoylthio- Environmentally friendly production of 1‑propyltriethoxysilane.

Description

technical field [0001] The invention relates to an environment-friendly production method of high-quality 3-octanoylthio-1-propyltriethoxysilane. Background technique [0002] Sulfur-containing silane coupling agents are widely used in the rubber product industry, especially in the process of producing green tires with white carbon black and sulfur formulations, and are absolutely indispensable additives. 3-octanoylthio-1-propyltriethoxysilane is a kind of sulfur-containing silane coupling agent, which has been gradually used in the production and manufacture of tires in recent years. [0003] At present, the prior art discloses the production process of 3-octanoylthio-1-propyltriethoxysilane as follows: [0004] (1) Silane reacts with acid chloride, acid anhydride or (thio) carboxylic acid in the presence of a solvent or without a solvent. During the reaction, the by-product hydrogen chloride is generated, and the hydrogen chloride is neutralized by alkali. [0005] (2) A...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C07F7/20
CPCC07F7/1892C07F7/20
Inventor 陶再山李春华
Owner 南京曙光新材料有限公司
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