Preparation method of thiophenol compound antioxidant product

Abstract

The invention relates to a preparation method of a thiophenol compound antioxidant product, relating to the technical field of preparation of antioxidant products. A process technical method of the thiophenol compound antioxidant product comprises the following steps of: taking 3, 5-methyl ester and thiodiglycol as raw materials, performing ester exchange reaction under the actions of a catalyst and a color blocking agent, and generating a reaction product mixed solution containing 2, 2'-thiodiethyl bis(3-(3, 5-di-tert-butyl-4-hydroxyphenyl) propionate by continuously removing a byproduct, namely methanol during the reaction process; adding an appropriate amount of phosphite ester-like compound into the reaction product mixed solution, and generating a new phosphite ester-like compound by secondary ester exchange reaction; and selecting a recrystallization solvent, performing recrystallization and refining on the reaction product mixed solution, and performing solid-liquid separation to obtain a while granular crystal product.

Description

technical field [0001] The invention relates to a preparation method of a thiophenol compound antioxidant product, which relates to the technical field of antioxidant product preparation, and the thiophenol compound antioxidant product specifically refers to the following formula (I): [0002] [0003] Formula (I) chemical name: 2,2'-thiodiethylbis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]. Background technique [0004] 2,2'-thiodiethylbis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate] (abbreviated as Antioxidant 1035), is a thiophenol compound belonging to Intramolecular composite antioxidant, which is widely used in polymer materials such as polyethylene, polypropylene, polystyrene, ABS resin, and various synthetic rubbers. Antioxidant 1035 is used in combination with hindered phenolic main antioxidants, which has a good synergistic effect and can effectively improve the processing stability, heat resistance stability, color improvement and weather resistance ...

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Problems solved by technology

[0014] US4085132 discloses a technical method for preparing antioxidant 1035, which uses 2,6-di-tert-butylphenol, thiodiglycol, and methyl acrylate as raw materials to prepare 2,2'-sulfur Substitute diethyl bis[3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate], its shortcoming is that the difficulty of refining and purifying the product is relatively large, and the product yield is low

[0015] US4228297 and US4694099 respectively disclose a technical method for preparing antioxidant 1035, which uses 2,6-di-tert-butylphenol and methyl acrylate as raw materials, and carries out transesterification under the action of a catalyst to prepare 2,2'-sulfur Diethyl bis[3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate], its disadvantage is that the product is more difficult to refine and purify, and finally the product reaches the expected purity result low yield

[0016] CN102050768A discloses a separation method and preparation method of antioxidant 1035, which uses 3,5-methyl ester and thiodiglycol as raw materials, and selects dibutyltin oxide, dioctyltin oxide, monobutyl oxide Tin is a catalyst, and the reaction product mixture of 2,2'-thiodiethylbis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate] is prepared by transesterification, and the crystallization Solvent contact is carried out crystallization, to isolate antioxidant 1035 product, wherein, described recrystallization solvent is the mixture of methanol and ethanol, or the mixture of at least one in methanol and ethanol and water, and its disadvantage is that it cannot make people Satisfactorily solve the general problems in the process of transesterification reaction in the synthesis process and product recrystallization, purification and separation

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