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The preparation method of two [propyltriethoxysilane] disulfide

A technology of propyltriethoxysilane and chloropropyltriethoxysilane is applied in the production field of bis[propyltriethoxysilane] disulfide, and can solve the problem of increasing the output of three wastes of raw materials, toxic and harmful Substances, by-products are difficult to handle, etc., to achieve the effect of reducing the risk of polymerization, reducing the generation of three wastes, and reducing the input of raw materials

Active Publication Date: 2016-03-02
南京曙光新材料有限公司
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AI Technical Summary

Problems solved by technology

[0003] At present, there are generally two large-scale industrial production methods of bis[propyltriethoxysilane] disulfide. The first one is the synthesis method of organic solvent technology such as using alcohol solvent, hydrogen sulfide, alkali metal alcoholate, etc. as raw materials. , this method has the problems of flammable, explosive, toxic and harmful substances as raw materials, unsafe production, high cost of raw materials, difficult to handle by-products, exhaust emissions and other problems; the second is the phase transfer catalytic aqueous phase using a buffer method, such as the production method using alkali metal sulfide or hydrogen sulfide or hydroxide, water, buffering agent, etc. as raw materials, a buffering agent must be added in the production method, and the buffering agent is required for useless substances in subsequent production It is treated as the three wastes, which undoubtedly increases the input of raw materials and the output of the three wastes
[0004] In addition, the inventor's literature search and practical operation prove that there is no successful case of synthesizing bis[propyltriethoxysilane] disulfide in the phase-transfer catalytic aqueous phase method without buffer

Method used

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Embodiment 2

[0050]Into a 1000mL three-necked flask equipped with a stirring and heating device, put 60g of sodium hydrosulfide aqueous solution with a mass fraction of 46%, 38g of an aqueous sodium hydroxide solution with a mass fraction of 48%, and 20g of sulfur powder, and heat up to 70°C. ℃-80 ℃ to react until there is no solid, keep warm for half an hour. 10g of tetrabutylammonium bromide was dissolved in 120g of n-heptane, and then added to aqueous sodium polysulfide solution. Raise the temperature of the above mixed solution to 75°C, start dropwise adding 230g of 98% chloropropyltriethoxysilane to reflux reaction, keep the temperature at 75°C-95°C, and keep warm for half an hour after the addition. Separating the water phase of the lower floor, transferring the upper organic phase to the short-range molecular distillation device, collecting fractions in sections, reclaiming the solvent n-heptane, obtaining the product 193g of the light yellow transparent liquid as the substrate, aft...

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Abstract

The object of the present invention is to provide a kind of method that does not contain buffering agent and synthesizes two [propyltriethoxysilane] disulfides under aqueous phase conditions, comprising the following steps: A, making sodium polysulfide aqueous solution, chloropropane Base triethoxysilane reacts under the aqueous phase condition of phase-transfer catalyst and water-insoluble organic solvent, produces reaction mixture; B, separates two [propyl triethoxysilane] disulfides from above-mentioned reaction mixture . The method for separating the product bis[propyltriethoxysilane] disulfide from the reaction mixture in the step B comprises the following steps: a, organic phase separation: the upper layer of the reaction mixture obtained in step A is an organic phase, and the lower layer is water phase, separate the organic phase; b, purify the organic phase: distill and purify the above organic phase to obtain the product bis[propyltriethoxysilane] disulfide. Using the method of the invention improves the yield, reduces the generation of three wastes, and eases the pressure on environmental protection.

Description

technical field [0001] The invention relates to a production method of bis[propyltriethoxysilane] disulfide, which belongs to the synthesis of organic chemicals. More specifically, a method for producing bis[propyltriethoxysilane] disulfide under aqueous phase conditions without the use of a buffer. Background technique [0002] Bis[propyltriethoxysilane] disulfide is an important auxiliary agent for the production of green tires. It is widely used in the products of sulfur vulcanized rubber system. Through the coupling of inorganic filler or fiber and rubber matrix, it can achieve Improvement of product performance. Used in tires, especially to improve the friction resistance, rolling resistance and wet skid resistance of tires. [0003] At present, there are generally two large-scale industrial production methods of bis[propyltriethoxysilane] disulfide. The first one is the synthesis method of organic solvent technology such as using alcohol solvent, hydrogen sulfide, al...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
Inventor 陶再山李春华王金勇刘兰香
Owner 南京曙光新材料有限公司
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