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Method for synthesizing dendritic phenolic antioxidant

A technology of phenolic antioxidant and synthesis method, which is applied in the production of bulk chemicals, etc., can solve the problems of poor antioxidant performance and poor compatibility, and achieve the effect of easy operation and appropriate reaction time

Inactive Publication Date: 2010-05-12
DAQING GASOLINEEUM INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2002, Helena Bergenudda proposed a new type of antioxidant, that is, hyperbranched phenolic antioxidant, which is an antioxidant modification of hyperbranched macromolecules, so that it has multiple antioxidant groups, Improve its anti-oxidation activity, but this type of antioxidant has good anti-oxidation performance in high-grade lubricants with low freezing point, but in polyolefin materials due to poor compatibility, the anti-oxidation performance is inferior to the antioxidant Irganox 1010

Method used

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  • Method for synthesizing dendritic phenolic antioxidant
  • Method for synthesizing dendritic phenolic antioxidant
  • Method for synthesizing dendritic phenolic antioxidant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: Preparation of 3,5-propionyl chloride: Accurately weigh 5.56g of 3,5-propionic acid and put it into a dry 250mL three-neck flask, add 50mL of chloroform to dissolve, and place in a constant temperature magnetic stirring water bath at 50°C In, slowly drop 4mL of thionyl chloride, react for 5h. Distill under reduced pressure at 62°C and 133Pa to remove the solvent chloroform and unreacted thionyl chloride to obtain β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl chloride light yellow The crystal, referred to as 3,5-propionyl chloride, has a yield of 97.8%.

Embodiment 2

[0013] Example 2: Preparation of 1.0G polyamide-amine: Accurately weigh 9g of ethylenediamine and dissolve it in 30g of methanol, slowly add 103.2g of methyl acrylate dropwise while stirring, react at 25°C for 24h, at 50°C, 133.3Pa Distilled under reduced pressure under the conditions to obtain 0.5G polyamidoamine; then accurately weigh 12.0g 0.5G polyamidoamine, dissolve it in 60g methanol, slowly add 108.0g ethylenediamine dropwise while stirring, and react at 25°C After 24 hours, under the conditions of 72°C and 133Pa, vacuum distillation was carried out for 3 hours to obtain 1.0 g of polyamidoamine.

Embodiment 3

[0014] Embodiment 3: Utilize the 3,5-propionyl chloride synthesized in embodiment 1 and embodiment 2 and 1.0G polyamido-amine, 3,5-propionyl chloride is dissolved in chloroform, prepare 3,5-propionyl chloride Chloroform solution: Accurately weigh 2.0g of 1.0-generation polyamide-amine in a dry 250mL three-necked bottle, dissolve it in 50mL of chloroform, add 3mL of acid-binding agent triethylamine, and put it in a constant temperature magnetic stirring water bath at 15°C , use a constant pressure dropping funnel to add dropwise the chloroform solution of 3,5-propionyl chloride, after the addition, raise the reaction temperature to 30°C, react for 12 hours, and investigate the relationship between 3,5-propionyl chloride and 1.0-generation polyamide-amine Effect of molar ratio on the yield of dendritic antioxidants. The result is as figure 1 shown. Result shows, when 3, the mol ratio of 5-propionyl chloride and 1.0 generation polyamide-amine is 8: 1, the yield of dendritic phe...

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Abstract

The invention relates to a method for synthesizing a dendritic phenolic antioxidant, which comprises the following steps: firstly, using ethylenediamine and methyl acrylate as raw materials; secondly, synthesizing frameworks of 0.5 generation polyamide-amine and 1.0 generation polyamide-amine through two steps including Michael addition reaction and amidation condensation reaction; thirdly, using the 1.0 generation polyamide-amine and beta-(3,5-di-tertiary-butyl-4-hydroxyphenyl) propionyl chloride as raw materials, and using triethylamine as an acid-binding agent and trichloromethane as a solvent to perform the amidation condensation reaction; and finally, performing reduced pressure distillation, extraction and filtering to obtain the dendritic phenolic antioxidant. The dendritic phenolic antioxidant has readily available reaction raw materials, mild reaction conditions, easy product purification and high product yield; and the reactions belongs to basic reaction types, so the dendritic phenolic antioxidant can achieve industrialization very easily.

Description

Technical field: [0001] The invention relates to a method for synthesizing dendritic phenolic antioxidants. Specifically, organic substances are used as raw materials to synthesize a new class of polymer material additives through organic synthesis reactions under the condition of no catalyst. Background technique: [0002] Antioxidant is an important additive that can stabilize polymers, and its application involves almost all polymer products. Phenolic antioxidants are the most non-polluting and non-discoloring antioxidants among all antioxidants. At present, phenolic antioxidants account for about 50% of the consumption in my country, and 2,6-di-tert-butylphenol (BHT) still occupies a dominant position as the basic species, but due to the relatively low molecular weight and high volatility of BHT, And there are shortcomings such as yellowing and discoloration, and the consumption is decreasing year by year. The consumption proportion of hindered phenol varieties with rel...

Claims

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Application Information

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IPC IPC(8): C08G69/48C08L77/00C08L23/06C08L23/12
CPCY02P20/52
Inventor 王俊李翠勤杨洪军邸晓贺李杰吕春胜张会平郭艳东
Owner DAQING GASOLINEEUM INST
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