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Intramolecular compound antioxidant and preparation method thereof

A compound type, antioxidant technology, applied in the field of antioxidants, can solve the problems that the anti-oxidation performance of ABS resin and polyolefin cannot be realized, and the synthesis and processing process of ABS resin and polyolefin are not suitable, so as to improve the antioxidant efficiency , good extraction performance, and the effect of reducing side reactions

Inactive Publication Date: 2019-08-02
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned intramolecular composite stabilizers are not suitable for the synthesis and processing of ABS resins and polyolefins, and cannot achieve the effect of improving the oxidation resistance of ABS resins and polyolefins.

Method used

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  • Intramolecular compound antioxidant and preparation method thereof
  • Intramolecular compound antioxidant and preparation method thereof
  • Intramolecular compound antioxidant and preparation method thereof

Examples

Experimental program
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preparation example Construction

[0048] The embodiment of the present invention also provides a preparation method of the above-mentioned intramolecular composite antioxidant, which specifically includes the following steps:

[0049] (1) According to the molar ratio of diphenylphosphorous chloride: 2,2'-methylenebis-(4-methyl-6-tert-butylphenol):acid-binding agent=1:1.0~1.2:1 weighed respectively Amount of diphenylphosphorous chloride, 2,2'-methylenebis-(4-methyl-6-tert-butylphenol) and acid binding agent, standby; 2,2'-methylenebis-( 4-methyl-6-tert-butylphenol) and acid-binding agent are dissolved in a solvent to obtain a mixed solution; diphenylphosphorous chloride is dissolved in a solvent to obtain a diphenylphosphorous chloride solution; wherein the acid-binding agent includes Combination of one or more compounds in pyridine, triethylamine, N,N-dimethylaniline or 4-dimethylaminopyridine, the solvent includes one of toluene, cyclohexane, dimethyl sulfoxide or tetrahydrofuran Combination of one or more com...

Embodiment 1

[0062] Weigh 9.39g N,N-dimethylaniline (0.05mol) and 17.025g 2,2'-methylenebis-(4-methyl-6-tert-butylphenol) (0.05mol), Dissolve it in hexane, add it to a three-necked flask with magnetic stirring, under the condition of ice bath, the temperature is 0°C, and stir for 30min under the protection of nitrogen; use the dropping funnel to slowly add 50mL of cyclohexane-dissolved diphenyl Phosphorous chloride (11.0g, 0.05mol) solution, after the dropwise addition was completed, the temperature was raised to 50°C, a white precipitate appeared in the solution, and the reaction was kept for 2 hours; Most of the solvent was distilled off by the evaporator under reduced pressure to obtain a light yellow oily liquid; the solution was dropped into ether (50ml) solution and crystallized at -10°C for 24h; the white crystals obtained were suction filtered and washed with ether for 50 ℃ vacuum drying to obtain intramolecular composite antioxidant, characterized by high performance liquid chroma...

Embodiment 2

[0064] Weigh 9.39g of N,N-dimethylaniline (0.05mol) and 18.7275g of 2,2'-methylenebis-(4-methyl-6-tert-butylphenol) (0.055mol), and use 50mL of toluene Dissolve it and add it to a three-necked flask with magnetic stirring. Under the condition of ice bath, the temperature is 0° C. and stirred for 30 min under the protection of nitrogen; slowly add 50 mL of diphenylphosphorous chloride dissolved in toluene dropwise with a dropping funnel ( 11.0g, 0.05mol) solution, after the dropwise addition was completed, the temperature was raised to 80°C, a white precipitate appeared in the solution, and the reaction was kept for 4h; Most of the solvent was distilled off to obtain a light yellow oily liquid; the solution was dropped into ether (50ml) solution, and crystallized at -10°C for 24h; the obtained white crystals were suction filtered, washed with ether, and dried in vacuo at 50°C. The intramolecular composite antioxidant was obtained, and the purity of the product was 99% as charac...

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Abstract

The invention discloses an intramolecular compound antioxidant and a preparation method thereof. The obtained intramolecular compound antioxidant has good hydrolysis resistance, high oxidation resistance efficiency and dual effects of hindered phenol and phosphite antioxidants, can replace an existing compound system of hindered phenol and phosphite antioxidants and can meet the function requirement for antioxidants during synthesis and processing of ABS resin and polyolefin.

Description

technical field [0001] The invention relates to the technical field of antioxidants, in particular to an intramolecular composite antioxidant and a preparation method thereof. Background technique [0002] ABS resin is mainly used as exterior materials for TVs, air conditioners, refrigerators, washing machines and other home appliances. Its aging resistance during storage, molding and use is poor, and its structure changes with time, and it appears yellowing, brittle, Cracks, surface loss of luster, greatly reduced mechanical properties, etc., will eventually lose its use value. The poor aging resistance of ABS resin is due to the fact that the double bonds contained in butadiene are easy to react with light and oxygen, and its aging rate is proportional to the content of butadiene components. In order to improve its aging resistance, it is necessary to add additives to delay degradation. [0003] At present, the common additives are antioxidants compounded by hindered phe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/46C08K5/5377
CPCC07F9/46C08K5/5377
Inventor 计海峰王卫东郑娣莲石洪飞刘保雷
Owner JILIN INST OF CHEM TECH
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