Preparation method of phenyl silicone oil

Abstract

The invention discloses a preparation method of phenyl silicone oil, the preparation method comprises the following steps: (1) adding a hydrolysis mixed solution and dimethyl alkoxy silane into diphenyl alkoxy silane to have a hydrolysis reaction to obtain a hydrolysate, wherein the speed ratio of the dimethyl alkoxy silane to the hydrolysis mixed solution is (3-10):1, the hydrolysis mixed solution comprises a hydrolysis catalyst, a hydrolysis accelerator and water; (2) adding an end capping agent and a polymerization catalyst into the hydrolysate to have a polymerization reaction, adding a hydroxyl remover in the process of the polymerization reaction, and finishing the reaction to obtain a finished product. The dimethyl alkoxy silane and the hydrolysis mixed solution are added into the diphenyl alkoxy silane at certain speed ratio, the hydrolysis speed is effectively controlled, the phenyl in the hydrolysate is more evenly distributed, the prepared hydrolysate is clear and transparent, the hydrolysate with the evenly distributed phenyl is obtained without rearranging at the high temperature, and the quality of a final product, the phenyl silicone oil, is improved.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of phenyl silicone oil. Background technique [0002] Phenyl silicone oil is a product in which some of the methyl groups on methyl silicone oil are replaced by phenyl groups. Because of its excellent high and low temperature resistance, good lubricating performance, radiation resistance and better compatibility with plastic rubber and other materials , Phenyl silicone oil is widely used in lubrication, insulation, mold release, damping, shockproof and dustproof and other fields. According to the different phenyl structural units, phenyl silicone oil is divided into two types: methylphenyl-dimethylsiloxane copolymer and diphenyl-dimethylsiloxane copolymer. Among them, diphenyl raw material Compared with methyl phenyl raw materials, the synthesis is simple and the price is cheap and easy to obtain. Therefore, the research on polydiphenyl-dimethylsil...

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Problems solved by technology

For example: Patent CN106977720A discloses a preparation method of phenylmethyl silicone oil, which uses octamethylcyclotetrasiloxane, methylphenylcyclotrisiloxane, dimethyltetraphenyldisiloxane, Methylammonium hydroxide, polyethylene oxide, hexamethyldisiloxane, and o-benzoylsulfonimide are used as raw materials to prepare phenylmethyl silicone oil; patent CN107759790A discloses a preparation method of phenylmethyl silicone oil, which The phenylmethyl silicone oil is prepared from dimethyldiphenyl mixed cyclosiloxane, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide silicon alkoxide and hexamethyldisiloxane; the above two This method not only has high cost of raw materials, but also the catalyst used is unsatisfactory for the rearrangement effect of phenyl groups, and only phenyl silicone oil with lower phenyl content can be prepared, and the boiling point of the end-capping agent used is lower than the reaction temperature, so that the viscosity of the product is not good. Stable; while the silicone oil prepared by tetramethylammonium hydroxide or its silicon alkoxide needs high-temperature rearrangement to make the phenyl group evenly distributed, but the phenyl silicone oil after high-temperature treatment is prone to yellowing, and it is difficult to meet high-end requirements such as high light transmittance. field requirements

Patent CN104892943A discloses a preparation method of phenyl vinyl silicone oil, which adds methylphenylcyclosiloxane, dimethylcyclosiloxane and end-capping agent to a basic catalyst for equilibrium polymerization reaction, and the polymerization reaction ends After adding an acid neutralizer, washing and drying to obtain phenylvinyl silicone oil, this method not only has high cost, but also produces a large amount of waste acid water

[0004] The hydrolytic condensation method mainly uses phenylalkoxysilane or phenylchlorosilane and methylalkoxysilane or methylchlorosilane as raw materials, and then adds water through hydrolytic condensation; the preparation cost of this method is relatively low, but the hydrolysis process Alkoxy groups and hydroxyl groups will remain, and the performance of the obtained phenyl silicone oil is poor, and due to the large difference in the hydrolysis rate of the phenyl raw material and the methyl raw material, the phenyl group is unevenly distributed, and the phenyl group is unevenly distributed. It will lead to a decrease in product performance and transparency, so most of the synthesis process requires solvent assistance, making it difficult for the light transmittance of the final product to meet the requirements of the high-end field

For example: Patent CN103408759A discloses a preparation method of methylphenyl silicone oil, which uses dimethyldichlorosilane and methylphenyldichlorosilane as raw materials and xylene as a solvent to synthesize phenyl silicone oil; the synthesis process of the method The medium solvent and water are immiscible, while the hydrolysis rate of dimethyldichlorosilane is faster, the hydrolysis rate of methylphenyldichlorosilane is slower, and the distribution of phenyl groups is uneven, making it difficult to make transparent and high refractive index Phenyl silicone oil

Patent CN103304818A discloses a preparation method of methylphenyl silicone oil, after mixing dimethyldichlorosilane, diphenyldichlorosilane, xylene and acetone, adding ketone and water, washing and drying, adding end-capping agent and catalyst to obtain phenyl silicone oil; in this method, acetone that can be miscible with water is used, but acetone is difficult to recycle, and the acetone remaining in phenyl silicone oil will affect its product performance and transparency

Patent CN106008980A discloses a preparation method of phenylmethyl silicone oil, hydrolyzing diphenyldimethoxysilane and dimethyldiethoxysilane with dilute hydrochloric acid solution, washing and drying the product with tetramethylhydroxide Ammonium catalyzes phenyl silicone oil; the phenyl group in the phenyl silicone oil prepared by this method tends to be unevenly distributed, resulting in turbidity of the product and seriously affecting its performance

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