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Synthesis method of thioether phenolic antioxidant

A technology of phenolic antioxidants and synthetic methods, which is applied in the direction of sulfide preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of poor catalytic effect of catalysts, cumbersome catalyst treatment, and inability to recycle, etc., to achieve Good chromaticity difference at high temperature, no pollution, and the effect of improving product quality

Pending Publication Date: 2021-01-29
利安隆(天津)新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of poor catalyst catalytic effect, large dosage, cumbersome catalyst treatment and inability to recycle the above antioxidant 1035 in the synthesis process, the purpose of the present invention is to provide a high-efficiency, green and recyclable supported transesterification catalyst to prepare anti-oxidant 1035. Oxygen 1035 method

Method used

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  • Synthesis method of thioether phenolic antioxidant
  • Synthesis method of thioether phenolic antioxidant
  • Synthesis method of thioether phenolic antioxidant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment A

[0054] Clean the silica carrier with deionized water, activate at 105°C, and purging with nitrogen for 2 hours, take 20g of silica and put it in 100ml of methanol solution with a concentration of 35% lithium acetate, at 20-25°C Immerse for 12 hours, filter, and dry at 100°C for 2 hours to obtain a supported transesterification catalyst silica / lithium acetate.

Embodiment B

[0056] Clean the hydrotalcite carrier with deionized water, activate it at 140°C, and purging with nitrogen for 3 hours, take 15g of hydrotalcite and put it into 150ml of methanol solution with a lithium methylate concentration of 20%, and immerse it at 32-40°C for 9h. Filter and dry at 120°C for 2 hours to obtain a supported transesterification catalyst hydrotalcite / lithium methoxide.

Embodiment C

[0058] Clean the HY molecular sieve carrier with deionized water, activate at 90°C, and purging with nitrogen for 3h, take 20g of HY molecular sieve and put it into 100ml of methanol solution with a concentration of 40% dioctyltin oxide, and immerse it at 40-50°C for 8h , filtered, and dried at 70°C for 4h to obtain a supported transesterification catalyst HY molecular sieve / dioctyltin oxide.

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Abstract

The invention relates to a synthesis method of a thioether phenolic antioxidant, which comprises the steps of synthesizing 2,2'-thiodiethyl bis[3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] by taking 3-(3,5-di-tert-butyl-4-hydroxyphenyl) methyl propionate and thiodiglycol as raw materials and using a supported ester exchange catalyst. The supported transesterification catalyst provided by theinvention is low in dosage, cheap, easy to obtain, efficient and easy to separate, and can be recycled for multiple times, and meanwhile, the problem that the product quality is influenced by catalystresidues in the reaction is solved.

Description

technical field [0001] The invention relates to the technical field of antioxidant synthesis, specifically sulfide-type phenolic antioxidant 2,2'-thiodiethylbis[3-(3,5-di-tert-butyl-4-hydroxyphenyl) Propionate] preparation. Background technique [0002] Antioxidant 1035, the chemical name is 2,2'-thiodiethylbis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate], is a thioether-type hindered Phenolic antioxidants contain not only the hindered phenolic group of the main antioxidant, but also the low valence sulfur atom of the auxiliary antioxidant. They are widely used in butadiene rubber, styrene butadiene rubber, natural rubber, resin, polypropylene and other high Among molecular materials, it has a good anti-thermal and oxidative aging effect. [0003] The synthesis of antioxidant 1035 usually uses thiodiethylene glycol and 3-(3,5-di-tert-butyl-4-hydroxyphenyl) methyl propionate (referred to as 35 methyl ester) for transesterification, and the commonly used transesterificat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/20C07C323/12B01J31/02B01J31/04B01J31/12B01J31/26
CPCB01J31/04B01J31/0212B01J31/122B01J31/26C07C319/20B01J2231/49Y02P20/584
Inventor 杨智琳王梓鲁惠玲范小鹏孙春光李海平
Owner 利安隆(天津)新材料科技有限公司
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