Preparation method of antioxidant product with stable performance

Abstract

The invention provides a preparation method of antioxidant product with stable performance. 2, 4-di-tert-butylphenol and phosphorus trichloride are taken as raw materials, organic amino compound is taken as catalyst, organic solvent is taken as reaction solvent, esterification is carried out to prepare tri(2,4-ditertrabutyl phenyl) phosphite ester crystal product, namely antioxidant crude product; after reaction is completed, the organic solvent is added into a kettle, so that the antioxidant crystal product is completely dissolved into the organic solvent, an amount of triethylamine is added to react with HCl remained in product mixture, so as to generate triethylamine hydrochloride crystal, filter aid is added to remove solids triethylamine hydrochloride and organic amine catalyst hydrochloride by heat filtering, reduced pressure distillation is carried out to remove the organic solvent, and crystal is washed by low carbon fatty alcohol, thus obtaining the antioxidant product with stable performance. The invention has the advantages of simple production technology, high product yield and good quality; and the obtained product has long time hydrolytic resistance, pyrolysis resistance and good oxidation resistance.

Description

technical field [0001] The invention relates to a process for preparing an antioxidant product with stable performance, in particular to a process for preparing tris(2,4-di-tert-butylphenyl)phosphite. Background technique [0002] Antioxidant 168 product belongs to phosphorous acid antioxidant, chemical name: tris(2,4-di-tert-butylphenyl) phosphite, specifically refers to the following formula (I): [0003] [0004] Antioxidant 168 is an excellent phosphite antioxidant product, which is widely used in polymer materials such as synthetic rubber, polyolefin plastics, and engineering plastics. When it is used in conjunction with hindered phenolic primary antioxidants, it has a good synergistic effect and can effectively improve the processing stability, heat resistance stability, color improvement and weather resistance of polymer materials. It is a phosphite secondary antioxidant Mainstream varieties of agents. [0005] The preparation process of antioxidant 168, in the p...

AI Technical Summary

Problems solved by technology

The chlorine atoms in phosphorus trichloride are all replaced by hydroxyl groups, and will be converted into phosphorous acid, which cannot continue to undergo esterification reaction with 2,4 phenol; if part of the chlorine atoms are replaced by hydroxyl groups, the intermediate product will continue to undergo esterification with 2,4 phenol reaction, the result will undoubtedly generate irreversible by-products of phosphite monoester dihydroxylate and phosphite diester monohydroxylate, which will be mixed into the product, making it impossible to obtain high-purity antioxidant 168 products

[0014] One of the disadvantages of the above method is that in the process of preparing the antioxidant 168 product, substances such as 2,4-di-tert-butylphenol and organic solvents are added or other natural conditions bring a small amount of water into the reactor, which is not removed in the process. Trace Water Measures

[0015] The second disadvantage of the above method is that in the process of preparing the antioxidant 168 product, there is no measure to remove a certain amount of impurities such as HCl and organic amine catalyst hydrochloride wrapped in the crystallized product, which leads to the hydrolysis reaction of the 168 product

The fatal weakness of antioxidant 168 is the hydrolysis reaction. Once hydrolyzed, it will not only cause unnecessary loss of antioxidants, but also make the polymer aging without effective protection, and its hydrolyzed acid substances will corrode during the polymer processing process. equipment

[0016] Two reasons cause the quality and stability of the obtained antioxidant 168 product to be defective

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