Preparation method of bis [propyl triethoxysilane] disulfide

A technology of propyl triethoxy silane and disulfide, which is applied in the production field of bis[propyl triethoxy silane] disulfide, can solve the problem of increasing the output of three wastes of raw materials, difficult to handle by-products, toxic and harmful Substances and other issues can reduce the risk of polymerization, reduce the input of raw materials, and reduce the generation of three wastes.

Active Publication Date: 2014-05-07
南京曙光精细化工有限公司
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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 used

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Embodiment 2

[0050] Into a 1000mL three-neck flask equipped with a stirring and heating device, put 60g of sodium hydrosulfide aqueous solution with a mass fraction of 46%, 38g of a sodium hydroxide aqueous 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. Separate the water phase of the lower floor, transfer the upper organic phase to the short-range molecular distillation device, collect the cuts in sections, reclaim the solvent n-heptane, and obtain the product 193g of the light yellow transparent liquid as the substrate. After infrared spec...

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Abstract

The invention aims at providing a method for synthesizing bis [propyl triethoxysilane] disulfide under an aqueous phase condition free from a buffer. The method comprises the steps of A. carrying out reaction on a sodium polysulfide aqueous solution and chloropropyl triethoxysilane under an aqueous phase condition in presence of a phase transfer catalyst and a water-insoluble organic solvent to generate a reaction mixture; and B. separating bis [propyl triethoxysilane] disulfide from the reaction mixture, wherein the way of separating the product bis [propyl triethoxysilane] disulfide from the reaction mixture in the step B comprises the steps of a. separating an organic phase: separating an organic phase from the upper layer of the reaction mixture obtained from the step A, wherein the lower layer of the reaction mixture is an aqueous phase; and b. purifying the organic phase: distilling and purifying the organic phase to obtain the product bis [propyl triethoxysilane] disulfide. The method disclosed by the invention can improve yield, reduce generation of three wastes and relieve environmental protection pressure.

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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IPC IPC(8): C07F7/18
Inventor 陶再山李春华王金勇刘兰香
Owner 南京曙光精细化工有限公司
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