Water-phase preparation method of low-impurity light-smell polysulfide silane coupling agent

Abstract

The invention aims at provide a water-phase preparation method of a low-impurity light-smell polysulfide silane coupling agent. The water-phase preparation method comprises the following specific steps: a, synthesis of a sodium polysulfide aqueous solution, namely adding sodium bisulfide or sodium sulfide, sodium hydroxide, sodium chloride, sulfur and water to a reaction device capable of stirring and heating, stirring and heating to the range from 70 to 80 DEG C, and preserving heat; b, addition of catalyst, namely feeding a catalyst aqueous solution into the sodium polysulfide aqueous solution; c, synthesis of coarse product, namely dropwise adding chloropropyltriethoxysilane to the sodium polysulfide aqueous solution, controlling the temperature of the reaction system within the range from 75 to 95 DEG C, and preserving heat after finishing dropwise adding; d, phase separation, namely separating the organic phase of the upper layer and the water phase of the lower layer and filtering the organic phase of the upper layer; e, purification of the organic phase, namely purifying the filtered organic phase by means of filtering or distillation, and then obtaining the product, namely, the polysulfide silane coupling agent.

Description

technical field [0001] The invention relates to a preparation method of a polysulfide silane coupling agent, which belongs to the synthesis of organic chemicals. More specifically, it is an aqueous phase production method of a polysulfide silane coupling agent with low impurity and light odor. Background technique [0002] Polysulfide silane coupling agent is an important auxiliary agent for the production of green tires. It is widely used in the products of sulfur vulcanized rubber system. It can improve the performance of products by coupling inorganic fillers or fibers with rubber matrix. Used in tires, especially to improve the friction resistance, rolling resistance and wet skid resistance of tires. At present, the polysulfide silane coupling agent products on the domestic market generally have a smell similar to the smell of hydrogen sulfide rotten eggs, which is caused by the smelly sulfur-containing impurities in the product, such as impurities hydrogen sulfide, mer...

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Problems solved by technology

[0003] The current large-scale industrial production method of polysulfide silane coupling agent generally has two kinds, the first kind is the synthetic method that uses alcohol solvent, hydrogen sulfide, alkali metal alcoholate etc. as raw material for organic solvent process, and this method exists raw material as Inflammable, explosive, toxic and harmful substances, unsafe production, high cost of raw materials, and unavoidable residual unreacted hydrogen sulfide raw materials and by-product mercaptosilane and other odorous impurities in the product will affect the quality and quality of the product. Odor; the second is the aqueous phase method, such as the production method using alkali metal sulfide or hydrogen sulfide, water, buffering agent, etc. as raw materials, the raw material alkali metal sulfide or hydrogen sulfide of the method, in the production process, In the presence of water and heating, side reactions inevitably occur to generate hydrogen sulfide and other odorous sulfur-containing substances such as mercaptosilane. There is also the problem of complex impurities and odor after the synthesis is completed.