Study On The Synthesis Of Antioxidants Of 168 And 330

One research and development focuse of antioxidant is the high polymer quantification. This kind of product has low volatilityly,high precipitation resistance characteristics.And it has high durability.The research and development of antioxidant with high molecular weight are widely concerned.In this thesis,tris(2,4-ditertbutylphenyl)phosphate(antioxidant 168) and 1,3,5-trimethyl-2, 4,6-tris(3,5-ditert-butyl-4-hydroxy benzyl)benzene(antioxidant 330) as high molecular weight antioxidants were synthesized.The factors influencing on the synthetic process were investigated.This provides important reference data for future industrial production.The synthesis of antioxidant 168 has been studied by esterification of 2,4-ditertbutylphenol and phosphorus trichloride.The effects of the variety and content of catalyst,reaction temperature,reaction pressure,the molar ratio of reagents on the reaction were studied,and the reaction conditions were optimized.The results showed the optimum conditions were as follows:the molar ratio of 2,4-ditertbutylphenol to phosphorus trichloride was 3.5:1.0,reaction temperature was 120℃,reaction time was 5 h,the dosage of catalyst was 0.5%accounting for the total molar of the raw materials,the yield of 168 was higher than 97%, the purity reached 96.26%.The 3,5-ditert-butyl-4-hydroxy benzyl methyl ether,intermediate of antioxidant 330,was synthesized by catalytic oxidation 2,6-ditert-butyl-4-methyl phenol.Then the ether react with 1,3,5-trimethylbenzene to prepare 1,3,5-trimethyl-2,4,6-tris(3,5-ditert-butyl-4-hydroxy benzyl)benzene(antioxidant 330),which has high molecular weight.The optimized reaction conditions were as follows:(1) Synthesis intermediate 3,5-ditert-butyl-4-hydroxy benzyl methyl ether.Reaction temperature was 75℃,reaction time was 9 h,the yield was 86.2%,the purity reached 99.36%.(2) Synthesis antioxidant 330.The molar ratio of 3,5-ditert-butyl-4-hydroxy benzyl methyl ether to 1,3,5-trimethylbenzene was 3.5:1.0,reaction temperature was 0℃,reaction time was 5 h,catalyst was 98%H₂SO₄,the yield of 330 was 91.2%,the purity reached 99.46%.In this thesis,the structure of the intermediate products,and the target products were characterized by IR and NMR.