A solvent-free preparation method of oxidation-coupled high-temperature antioxidant
A high-temperature antioxidant and oxidation coupling technology, applied in the preparation of amino compounds from amines, additives, organic chemistry, etc., can solve problems such as poor product stability, complex reaction conditions, and difficult post-processing, and achieve short reaction time and high reaction temperature. High, catalyst stable effect
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[0029] A solvent-free preparation method of an oxidation-coupled high-temperature antioxidant of the present invention, the preparation steps of the method are as follows:
[0030] 1) Add N-phenyl-α-methylnaphthylamine or alkylated N-phenyl-α-methylnaphthylamine and alkylated diphenylamine compounds in the reaction vessel, and the molar ratio is 1:0.2~ 4.0;
[0031] 2) Create a vacuum, heat up to 80-160°C to melt the material, and start stirring;
[0032] 3) The reaction temperature is 80-160°C, add an oxidation coupling catalyst, and react for 3-10 hours;
[0033] 4) After the reaction is finished, slowly build up a vacuum to a 2mmHG column, raise the temperature to 160-200°C, remove the catalyst, and obtain a yellow-brown solid product.
Embodiment 1
[0035] Use a 250ml four-necked flask, weigh 0.075mol, 16.425g of N-phenyl-α-methylnaphthylamine, 0.075mol, 29.475g of P, P diisooctyl diphenylamine, connect the four mouths of the flask to thermometers, and condense Reflux tube, constant pressure titrator and stirrer, set up a vacuum 300mmHG column, the reaction temperature is 80 ~ 100 ℃, add 0.15mol, 36.3g benzoyl peroxide, the reaction is refluxed for 10h, after the reaction, wash with hot water until neutral , Distilled under reduced pressure to obtain dark brown viscous liquid.
Embodiment 2
[0037] Use a 250ml four-necked flask, weigh 0.075mol, 16.425g of N-phenyl-α-methylnaphthylamine, 0.075mol, 29.475g of P, P diisooctyl diphenylamine, connect the four mouths of the flask to thermometers, and condense Reflux tube, constant pressure titrator and stirrer, set up a vacuum 300mmHG column, the reaction temperature is 120 ~ 140 ° C, add 0.15mol, 21.9g di-tert-butyl peroxide, the reaction is refluxed for 3.5h, after the reaction, use 20g hot water Wash and distill under reduced pressure to obtain a tan solid product.
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