Preparation method for polymerization-type asymmetric hindered phenol anti-oxidant resins

Abstract

Provided is a preparation method for polymerization-type asymmetric hindered phenol anti-oxidant resins. The preparation method comprises steps: with strong acid resins as catalysts, and benzene or cyclohexane as a solvent, 2-tert-Butyl-p-cresol and dicyclopentadiene are subjected to a polymerization reaction to form phenol-type petroleum resins; the phenol-type petroleum resins and saturated alcohols with one to three carbons are subjected to an alkylation reaction to form polymerization-type asymmetric hindered phenol anti-oxidant resins in presence of phosphoric acid and nickel-containing catalysts; the alkylation reaction products are subjected to reduced pressure distillation to remove the unreacted raw materials and solvent to obtain polymerization-type asymmetric hindered phenol antioxidant resin products. The preparation method has obvious positive effects, the polymerization reaction and the alkylation reaction have high selectivity and conversion rate, and the yield is about 80%. What is more important is that compared to traditional hindered phenol antioxidants, the synthesized polymerization-type asymmetric hindered phenol antioxidant resins are advantaged by high antioxidant activity, high heat stability, extracting resistance, compatibility, non-toxic and environmentally friendly characteristics.

Description

technical field [0001] The present invention relates to a method for preparing a polymeric asymmetric hindered phenolic antioxidant resin, in particular to preparing a polymeric asymmetric hindered phenolic antioxidant resin from dicyclopentadiene, o-tert-butyl p-cresol and C1-C3 saturated alcohol through polymerization and alkylation. Asymmetric hindered phenolic antioxidant resin approach. Background technique [0002] Antioxidants are a class of polymer additives that can effectively reduce the rate of autoxidation of plastic or rubber products and delay aging degradation, and their applications involve almost all polymer products. Since most polymers need to be heated at 220-350°C to be processed into products, traditional antioxidants are easy to volatilize at high temperatures, thus affecting the performance of products and causing environmental degradation. At present, the typical antioxidants are amines and phenols. Among them, amine antioxidants are mainly used in...

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Problems solved by technology

Currently disclosed phenolic antioxidant literature, such as: CN 100424122C discloses a p-cresol-dicyclopentadiene styrenated antioxidant, which polymerizes with styrene at the ortho position of the phenolic hydroxyl group, and only one A larger ortho group, low antioxidant efficiency

CN101402721A discloses a synthesis method of p-cresol-dicyclopentadiene isobutynylated antioxidant resin. Concentrated sulfuric acid catalyst is used in the production of this process, which is highly corrosive, and a large amount of solid waste will be generated by using activated clay to remove the catalyst and decolorize , increasing the pollution of the environment

CN101967223A discloses a synthesis method of methylphenol-dicyclopentadiene isobutyl resin antioxidant. The process uses composite sulfonic acid as a butylation catalyst, and p-cresol, dicyclopentadiene and isobutylene are synthesized as raw materials Methylphenol-dicyclopentadiene isobutyl resin antioxidant, because the ortho position of the antioxidant space structure has only tert-butyl group, the antioxidant effect is low; the raw material is isobutylene, which is not suitable for storage and has potential safety hazards

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