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Preparation method of silazane containing thioester bond

A nitrogen silane and ester bond technology, applied in the field of organosilicon fine chemicals synthesis, can solve the problems of large rubber porosity and high VOC, and achieve the effects of improving vulcanization performance, good product wear resistance and low rubber porosity

Inactive Publication Date: 2021-07-13
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above-mentioned NXT series is to modify the organic end of silane molecules, which solves the problems of sulfur-containing silane scorching and sulfur precipitation. At the same time, the reinforcement performance is better than Si75 and Si69, but it still cannot solve the problem of ethanol produced by the hydrolysis of sulfur-containing silane. High VOC and large rubber porosity

Method used

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  • Preparation method of silazane containing thioester bond
  • Preparation method of silazane containing thioester bond
  • Preparation method of silazane containing thioester bond

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Under nitrogen protection conditions, 364 g of 3-octyl thiopropyltriethoxysilane was added to the reaction vessel with mechanically stirred, and 200 g of DMF was added as a solvent, and 400 g of oxylate was added as an inhibitor, 1 g of triphenzene was added. Base acid ester exchange reaction catalyst.

[0036] The temperature was raised to 105 ° C, and 150 g of tsolamine was slowly added dropwise, and the ester exchange reaction was carried out, and the reaction temperature was controlled between 105-110 ° C. As the reaction initiated, the ethanol produced by the ester exchange was constantly vaporized to depart the reaction system, and then condensed with the brine condenser. After 4 hours of reaction, the system no longer produces ethanol, stop heating, and the ethanol 135 g is recovered. The reaction keena was reduced to 50-60 ° C for subsequent operation.

[0037] The mechanical stirring was opened and 1500 g of petroleum ether was added to the reaction kettle. As the ...

Embodiment 2

[0041] Under nitrogen protection conditions, 728 g of 3-octyl thiopropyltriethoxysilane was added to a mechanically stirred reaction kettle, and 440 g of DMF was added as a solvent, 826 g of oxylate as an inhibitor, and 2 g triphenzene was added. Base acid ester exchange reaction catalyst.

[0042] The temperature was raised to 105 ° C, and 300 g of triethoxide was slowly added dropwise, and the ester exchange reaction was carried out, and the reaction temperature was controlled between 105-110 ° C. As the reaction initiated, the ethanol produced by the ester exchange was constantly vaporized to depart the reaction system, and then condensed with the brine condenser. After the reaction was carried out for 4 h, the system no longer produced ethanol, stop heating, and the ethanol was recovered 270 g. The reaction keena was reduced to 50-60 ° C for subsequent operation.

[0043] The mechanical stirring was opened, and 3000 g of petroleum ether was added to the reactor. As the petrole...

Embodiment 3

[0047] Under nitrogen protection conditions, 1456 g of 3-octyl thiopropyltriethoxysilane was added to the reaction vessel with mechanically stirred, and 800 g of DMF was added as a solvent, and 1600 g of n-optate was added as an inhibitor, 5 g of triphenzene was added. Base acid ester exchange reaction catalyst.

[0048] The temperature was heated to 105 ° C, slowly added 600 g of triethylamine, and the ester exchange reaction was carried out, and the reaction temperature was controlled between 105-100 ° C. As the reaction initiated, the ethanol produced by the ester exchange was constantly vaporized to depart the reaction system, and then condensed with the brine condenser. After 4 hours of reaction, the system no longer produces ethanol, stop heating, and the ethanol 135 g is recovered. The reaction keena was reduced to 50-60 ° C for subsequent operation.

[0049] The mechanical stirring was opened, and 6000 g of petroleum ether was added to the reaction kettle to recrystallize....

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Abstract

The invention relates to a preparation method of silazane containing a thioester bond, and belongs to the field of organic silicon fine chemical synthesis. According to the invention, 3-octanoyl thiopropyl triethoxy silane and triethanolamine are used as raw materials, triphenyl borate is used as a catalyst, DMF is used as a solvent, ethyl n-caprylate is used as an inhibitor, novel solid sulfur-containing silane containing the thioester bond is synthesized, the yield reaches 98%, and the content reaches 98.5%. Compared with common thioester bond-containing silane, the silazane containing the thioester bond has the advantages that in the rubber mixing process, low-boiling-point alcohol substances cannot be generated, the rubber porosity is low, the product wear resistance is good, and almost no VOC is discharged; and meanwhile, the triethanolamine component in the structure can be preferentially adsorbed by carbon black, plays a role of an active dispersant, can promote uniform distribution of other amine accelerators, anti-aging agents, coloring agents and the like at the same time, and improves the vulcanization performance of the rubber material.

Description

Technical field [0001] The present invention relates to a method of preparing a mixed nitrogen-containing nitric silane containing a sulfide bond; an organic silicone fine chemical synthesis field. Background technique [0002] The sulfonilan is attached to the rubber with rubber by a chemical bond to effectively improve the binding ability of white carbon black and rubber molecules to promote rubber vulcanization, and simultaneously act as a dispersant, which can significantly reduce the tire rolling resistance and tire heat. Domestic common sulfur silicon having dibly (triethoxysil silica) tetravades (Si69), bis (triethoxypropylene) disulfide (Si75), mercaptoethoxysilane, etc. . In the tire industry, Si69 is the earliest, largest silane coupling agent, which can effectively improve the tensile strength, tear strength, hardness and intensive stress of the sulfide. However, due to the large number of sulfur atoms in the molecular structure, there is a problem that is prone to cok...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18B01J31/02
CPCB01J31/0272C07F7/1804C07F7/188
Inventor 靳军王灿陈圣云甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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