Preparation method for (para, para)-diisopropylphenyl diphenylamine product

Abstract

The invention belong to the technical field of organic compound synthesis and provides a preparation method for a (para, para)-diisopropylphenyl diphenylamine product. The method includes the steps of: (A) in the presence of a montmorillonite-type supported catalyst and under the protection of nitrogen gas, mixing a polymerization inhibitor with [alpha]-olefin and diphenylamine to perform an alkylation reaction at 75-175 DEG C for 4-16 h; and (B) reducing the temperature to 45-140 DEG C, and adding an organic cosolvent and a stabilizer with stirring, and filtering the reaction liquid while hot, and performing stepwise crystallization and purification, wherein a mother liquid can be recycled. The (para, para)-diisopropylphenyl diphenylamine crystal product has stable performance and high base number, is free of the problems such as yellowing, performance reduction and the like even after long-time storage, has uniform granular size and is less than 0.2% in residual diphenylamine content. In the production process, the olefin and the catalyst can be recycled and no waste water and waste gas emission exists, so that the process is environment-friendly. The product can be widely applied in various elastomers, foam plastics and lubricant oil for achieving the effects of resisting oxidization and aging.

Description

technical field [0001] The invention belongs to the technical field of organic compound synthesis, and relates to a preparation method of p-, p-dicumyl diphenylamine product. Background technique [0002] At present, there are many kinds of antioxidants that can be used in the fields of lubricating oil blending plastic rubber products technology, medicine, dyes, etc. The typical ones are amine-type and phenol-type antioxidants. Among the amine-type antioxidants, alkylated di Aniline and alkylated naphthalene amines have been widely used, but the application of amine antioxidants in the food field is relatively seldom, because aromatic amines used as raw materials for production have strong carcinogenicity, and many widely used None of the amine-type antioxidants can reduce the remaining diphenylamine content in the product to a range that is completely non-toxic to the human body, while p-, p-dicumyl diphenylamine can reduce the content of dicumyl diphenylamine to The raw m...

AI Technical Summary

Problems solved by technology

[0018] The technical solution of the present invention is to overcome the problem of discharge and pollution in the preparation method of p-, p-dicumyl diphenylamine products, and reaction problems existing in the prior art because the catalyst cannot be completely recycled. The activity is poor, the reaction time is long, and after the catalyst is recycled each time, it is necessary to further add some new catalysts to continue to recycle. A kind of p-, p-dicumyl diphenylamine product preparation method is proposed, The invention is montmorillonite loaded silica prepared by means of activation, active Al 2 o 3 etc. There are no free H ions and Cl ions in the catalytic system, so the product is light and bright in color; by adding a stabilizer and using a new process, the product prepared is a white, non-toxic, odorless crystal, which can be stored for a long time without performance and appearance. Changes, the base number is greater than 140, the remaining diphenylamine content is less than 0.2%, olefins and catalysts can be recycled and recycled, and there is no waste water and waste gas discharge in the production process, which is conducive to environmental protection

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