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Preparation method of novel polyphenols antioxidant

A technology of polyphenols and antioxidants, applied in the field of antioxidant preparation, can solve the problems of poor polymer compatibility and dispersibility, and achieve good compatibility, simple process, good thermal stability and antioxidant performance. Effect

Inactive Publication Date: 2018-03-23
SHAANXI QIYUAN TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these antioxidants have good thermal stability, they have poor compatibility and dispersion with polymers.

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] The preparation method of novel polyphenolic antioxidant of the present invention comprises the following steps:

[0012] The first step, the preparation of intermediate 3,5-di-tert-butyl-4-hydroxybenzyl alcohol, 7.27g paraformaldehyde, 1.08g potassium tert-butoxide and 100mL tert-butanol were added in a 500mL round-bottomed flask. Heat at 70°C until paraformaldehyde is depolymerized; add 20g of 2,6-di-tert-butylphenol to the above reaction solution, react for 3 hours at room temperature, add 200mL deionized water to the reaction solution, and then add 100mL Extract the organic phase with ethyl acetate, and dry it with a desiccant for 2 h, and remove the desiccant by suction filtration to obtain a yellow clear liquid, which is separated and purified by column chromatography to obtain a white solid powder 3,5-di-tert-butyl-4-hydroxy Benzyl alcohol;

[0013] The second step, the preparation of polyphenol antioxidants: Weigh 1.90g of 4-tert-butylphenol and 6g of intermedi...

Embodiment 2

[0015] The preparation method of novel polyphenolic antioxidant of the present invention comprises the following steps:

[0016] The first step, the preparation of intermediate 3,5-di-tert-butyl-4-hydroxybenzyl alcohol, 7.27g paraformaldehyde, 1.08g potassium tert-butoxide and 100mL tert-butanol were added in a 500mL round-bottomed flask. Heat at 70°C until paraformaldehyde is depolymerized; add 20g of 2,6-di-tert-butylphenol to the above reaction solution, react for 3 hours at room temperature, add 200mL deionized water to the reaction solution, and then add 100mL Extract the organic phase with ethyl acetate, and dry it with a desiccant for 2 h, and remove the desiccant by suction filtration to obtain a yellow clear liquid, which is separated and purified by column chromatography to obtain a white solid powder 3,5-di-tert-butyl-4-hydroxy Benzyl alcohol;

[0017] The second step, the preparation of polyphenol antioxidants: Weigh 1.90g of 4-tert-butylphenol and 6g of intermedi...

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PUM

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Abstract

The invention relates to the field of preparation of antioxidants, in particular to a preparation method of a novel polyphenols antioxidant. The preparation method comprises the following steps: preparing an intermediate which adopts 3,5-di-tert-butyl-4-hydroxy-benzyl alcohol: adding 7.27 g of paraformaldehyde, 1.08 g of potassium tert-butoxide and 100 mL of tertiary butanol into a round-bottom flask with the volume of 500 mL, heating the flask under a condition of 70 DEG C till the paraformaldehyde is depolymerized; adding 20 g of 2,6-di-tert-butylphenol into the reaction liquid for reactionunder a normal temperature condition for 3 h, then adding 200 mL of deionized water into the reaction liquid, adding 100 mL of an ethyl acetate extraction organic phase, drying the mixture with a drying agent for 2 h, and carrying out suction filtering to remove the drying agent. The preparation method is simple in process and convenient to operate; a product is relatively high in heat stability and oxidization resistance, is high in compatibility with a polymer, can inhibit oxidative degradation of polypropylene, polyethylene, acrylonitrile-butadiene-styrene resin and polystyrene, and also can be used for synthesizing natural rubber, plastic and lubricating oil.

Description

technical field [0001] The invention relates to the field of antioxidant preparation, in particular to a preparation method of a novel polyphenol antioxidant. Background technique [0002] Adding antioxidants to polymers can significantly improve their oxidation stability and service life, and are widely used in the fields of plastics, fibers, rubber, lubricating oils, inks and coatings. Antioxidants can be divided into amines, phenols, thioesters and phosphites according to different chemical structures. Hindered phenolic antioxidants have the advantages of good anti-oxidation effect, low toxicity and low color pollution, and are widely used in the fields of plastics, synthetic fibers, rubber, fuel, lubricating oil and food. [0003] At present, domestic hindered phenolic antioxidants are mostly monophenolic [such as 2,6-di-tert-butyl-4-methylphenol] or bisphenolic antioxidants [such as 2,2-methylene - bis(4-methyl-6-tert-butylphenol)], these products are not resistant to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/20C07C39/11C07C37/11C07C39/16C07C39/15C08K5/13C08L23/12C08L23/06C08L55/02C08L25/06
CPCC07C37/11C07C37/20C08K5/13C08L23/12C08L23/06C08L55/02C08L25/06C07C39/11C07C39/16C07C39/15
Inventor 张淑芬
Owner SHAANXI QIYUAN TECH DEV
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