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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

Active Publication Date: 2021-08-20
JIANGSU FEIYA CHEM IND
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  • Application Information

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Problems solved by technology

[0008] Technical problem: The purpose of this invention is to provide a more reasonable and efficient preparation method for the preparation of amine oxidation coupled high-temperature antioxidants, which overcomes the existing complex reaction conditions, long reaction time, low product yield, low degree of polymerization, and stable products Defects such as poor performance and difficult post-processing

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  • A solvent-free preparation method of oxidation-coupled high-temperature antioxidant
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  • A solvent-free preparation method of oxidation-coupled high-temperature antioxidant

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preparation example Construction

[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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Abstract

The invention provides a solvent-free preparation method of oxidation coupling high-temperature antioxidant, the specific preparation steps are as follows: add N-phenyl-α-methylnaphthylamine or alkylated N-phenyl-α-methylnaphthylamine into the reaction vessel Naphthylamine and alkylated diphenylamine compounds, the molar ratio is 1:0.2~4.0; build a vacuum, heat up to 80~160°C to melt the material, start stirring; the reaction temperature is 80~160°C, add oxidation coupling catalyst, React for 3-10 hours; after the reaction, 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. The preparation method of the invention adopts direct melting reaction of raw materials, and the oxidation coupling catalyst itself plays dual functions of reaction solvent and catalysis, no additional organic solvent is needed, materials are uniformly mixed, reaction conditions are mild, and reaction effect is good.

Description

technical field [0001] The invention belongs to the technical field of organic polymer compounds, and relates to a preparation method of an oxidation-coupled high-temperature antioxidant. Background technique [0002] At present, amine antioxidants are the earliest and most widely used antioxidants in the field of lubricating oil, including p-phenylenediamine antioxidants, diphenylamine antioxidants, aniline antioxidants, and naphthalene antioxidants. Amine antioxidants, etc. Except for a few polymeric phenolic antioxidants, amine antioxidants have stronger stability in oil products and can be used at higher temperatures, especially alkylated diphenylamine antioxidants, which can be applied to minerals In oil base oil, it can be used as a general-purpose internal combustion engine oil, and it can also be used in lipid synthetic oil as aero-engine lubricating oil. In recent years, with the deepening of people's research on the anti-oxidation mechanism of oil products, vario...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/68C07C211/55C10M133/12C08G73/02C10N30/08C10N30/10
CPCC07C209/68C07C211/55C08G73/02C10M133/12
Inventor 张健雄王忠冬熊畅
Owner JIANGSU FEIYA CHEM IND
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