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Novel synthesis method for hindered phenol anti-oxidants

A technology for antioxidants and hindered phenols, which is applied in the synthesis of hindered phenolic antioxidants to achieve the effects of high product conversion rate, reduced waste discharge, and efficient catalytic reaction.

Active Publication Date: 2009-08-19
北京极易控股集团有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In recent years, organic oxides of metal tin, such as dibutyltin oxide, and fatty acid salts of metal zinc, such as stannous octoate, have been used as catalysts for transesterification. Although the appearance of the reaction solution has improved, solvent crystallization is still required. In order to meet the quality requirements of the product

Method used

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  • Novel synthesis method for hindered phenol anti-oxidants
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  • Novel synthesis method for hindered phenol anti-oxidants

Examples

Experimental program
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Embodiment 1

[0034] Example 1: Taking the typical product of antioxidant: tetra-[β-(3,5-di-tert-butyl, 4-hydroxyphenyl)propionic acid]pentaerythritol ester (antioxidant 1010) as an example to describe the implementation of the present invention .

[0035] In a four-necked flask equipped with a stirrer, a condenser and a heater, add 136 grams (1 mole) of pentaerythritol, 1460 grams (5 moles) of 3,5 methyl esters, and then add 7 grams of pre-configured composite catalysts (main The catalyst is diisooctyl dimaleate di-n-butyltin, the co-catalyst is tris-(2,4-di-tert-butylphenol) phosphite, the compound ratio is 6:1), and it is replaced with pure nitrogen. The air in the system depressurizes the system and heats it up. The first stage of low heat preservation reaction, the temperature is 140-165 ℃, the pressure is 5000-20000pa, the reaction time is 3 hours, and the by-product methanol is extracted. The reaction temperature of the second stage is 165-190°C, the pressure is 5000-100pa, and the...

Embodiment 2

[0038] Embodiment 2: (main catalyst and 3,5 methyl ester recycling experiment of recovery for the first time)

[0039] Stirrer is equipped with condenser, in the four-necked flask of heater, add 136 grams (1 mole) pentaerythritol, add the reclaimed 3,5 methyl esters (wherein contain main catalyst), 292 grams, add 1168 grams (4 moles again) ) of fresh 3,5 methyl ester, add 1 gram of cocatalyst tris-(2,4-di-tert-butylphenol) phosphite, replace the air in the clean system with pure nitrogen, decompress the system, and heat up. In the first stage of low heat preservation reaction, the temperature is 140-165 ° C, the pressure is 5000-20000 Pa, the reaction time is 3 hours, and the by-product methanol is extracted. In the second stage, the reaction temperature is 165-190°C, the pressure is 5000-100pa, the reaction time is 4 hours, and the by-product methanol is continuously extracted. The third stage: the temperature is 170-190°C, the pressure is 500-20pa. The 3,5 methyl esters are d...

Embodiment 3

[0042] Embodiment 3. (main catalyst and 3,5 methyl ester experiments after circulation many times)

[0043] The amount of the main catalyst contained in the 3,5 methyl ester after many cycles has been determined in advance, and the lost amount of the main catalyst is made up in the test. Stirrer is equipped with, condenser, in the four-necked flask of heater, add 68 grams (0.5 mole) pentaerythritol, add the 3,5 methyl ester 146 grams (0.5 mole) that contains procatalyst repeatedly, add 584 grams (2 mol) of fresh 3,5 methyl esters, add the amount of the main catalyst that is determined to be lost through testing, and this experiment determines to add 1 gram of the main catalyst dibutyltin dilaurate, and the cocatalyst di(octadecyl)dipropionate Esters 0.5 g. Replace the air in the clean system with pure nitrogen, depressurize the system, and raise the temperature. Continue the previous three-stage reaction operation, steam the 3,5 methyl ester and the main catalyst, break the ...

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Abstract

The invention provides a new method for the synthesis of hindered phenols antioxidants. Under the action of a composite catalyst, a compound II and a compound III are subjected to transesterification and byproducts-methanol is obtained via heating and decompression; the rate of conversion of the product is more than 98%, and the compound I of hindered phenols antioxidants is directly obtained without crystallizing and purifying reaction liquid by solvent. The composite catalyst is composed of a primary catalyst of carboxylates of organotin and a secondary catalyst of thioester compounds of phosphite ester. The primary catalyst can be recycled.

Description

technical field [0001] The invention provides a new synthesis method of hindered phenolic antioxidants. The product conversion rate is high, and the reaction solution does not need solvent crystallization and purification, and the target product can be directly obtained. Background technique [0002] Hindered phenolic antioxidant is a widely used anti-aging agent for plastics, rubber and polymer materials, which can effectively protect plastics, rubber and polymer materials from the aging damage of oxygen in the environment, thereby prolonging the service life of materials. Representative products of hindered phenolic antioxidants are: tetrakis-[β-(3,5-di-tert-butyl, 4-hydroxyphenyl)propionic acid]pentaerythritol ester (trade name: Antioxidant 1010); 3,5- Di-tert-butyl, octadecyl 4-hydroxyphenylpropionate (trade name: Antioxidant 1076); 3,5-di-tert-butyl, hexylene glycol 4-hydroxyphenylpropionate, (trade name : Antioxidant 259); 2,2 / -Sulfidoethylene glycol bis[beta-(3,5-di...

Claims

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Application Information

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IPC IPC(8): C07C67/03C07C69/732B01J31/12C08K5/134
CPCY02P20/584
Inventor 郭永武
Owner 北京极易控股集团有限公司
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