Study On The Optimization Of Synthesis Process And Performance Of Antioxidant 1076

In this paper,2,6-ditert-butyl phenol and methyl acrylate,18 carbon alcohol as raw materials,synthetic ?-(3,5-ditert-butyl-4-hydroxyphenyl)18 carbon alcohol propionate(antioxidant1076),this reaction can be divided into two steps,Michael addition and ester exchange reaction,respectively by alkaline catalyst LDA and organic metal catalys Zinc isooctanoatet,the synthesis process were studied.The synthetic products were tested for thermal stability and oxidation induction period to evaluate their antioxidant properties.Firstly,the synthesis of ?-(3,5-ditert butyl-4-hydroxyphenyl)methyl propionate(MPC)was studied to investigate the effect of reaction temperature(reaction of 2,6-di-tert-butylphenol on the catalyst),reaction time,catalyst type and material ratio on the reaction yield.Optimum technological conditions were determined as follows:using new alkaline catalystlithium diisopropylamide(LDA),selecting DMF as a solvent,in the material than n(methyl acrylate):n(2,6-phenol)=1.1:1(Moore ratio,the same below),push reacting reaction temperature 110 ? for 2 hours,at 140 ? under the condition of reaction with methyl acrylate 2.5 hours,the yield over 99%,the purity as high as 98.8%.Anti-oxidant 1076 are studied,and then,against the effects of the variety of types of solvent,catalyst,material ratio,reaction temperature and reaction time influencing on the yield of reaction,the optimum technological conditions were determined as follows:Using a zinc isooctanoate catalyst,choose the methyl cyclohexane as solvent,reaction temperature is 130?,reaction time is 3.5 h,the suitable ratio of 1.05:1(3,5-methyl excess),the yield increased to 97%,product purity up to 97.75%.Finally,the product was characterized by infrared,nuclear magnetic resonance.HPLC and determination melting point,and the thermal stability and antioxidant performance of the product were measured by TG,DSC,Through the test of oxidation induction period.The results show that the product structure is consistent with the theoretical structure and has good thermal stability and antioxidant activity.