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Method for preparing hindered phenol antioxygen 1010

A technology for hindered phenol antioxidant and organic solvent is applied in the field of preparing hindered phenol antioxidant 1010, which can solve the problems of low reaction rate, high metal content in the product, and difficulty in removing organic metals, and achieves high catalytic activity and no heavy metals. , the effect of not easy to color

Active Publication Date: 2017-05-31
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The former strong alkali can easily lead to darker color of the product, greater equipment corrosion, and complicated post-treatment; while the reaction rate of organotin catalysts is low, organic metals are difficult to remove, the product has high metal content, and the range of product use is limited; in addition, the introduction of reaction solvents increases. The difficulty of post-reaction treatment (solvent removal, post-treatment of waste liquid) and production cost

Method used

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  • Method for preparing hindered phenol antioxygen 1010
  • Method for preparing hindered phenol antioxygen 1010

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Take 4.63 g of n-chlorobutane and 6.85 g of N-methylimidazole in a four-necked flask, and react at 50°C for 12 hours under the protection of nitrogen. The mixed solvent of acetonitrile and ethyl acetate was recrystallized to obtain the ionic liquid [Bmim]Cl.

[0021] Dissolve 8.75 g of the above ionic liquid in 50 ml of dichloromethane, add 2.0 g of solid sodium hydroxide particles, stir at room temperature for 10 h, remove the precipitate by suction filtration, and remove the solvent by rotary evaporation to obtain the crude ionic liquid [Bmim]OH. The crude product was washed 3 times with anhydrous ether, evaporated under reduced pressure to remove the ether, and dried in vacuum at 80°C to constant weight to obtain the basic ionic liquid [Bmim]OH. .

Embodiment 2

[0023] Take 0.05 mol of the ionic liquid intermediate [Bmim]Cl and dissolve it in 50 ml of isopropanol, add 2.5 times the amount of KOAc, stir at 25° C. for 10 h, and filter out the insoluble matter. The filtrate was evaporated to remove the solvent to obtain a light yellow oil. Dissolve the crude product in dichloromethane, add activated carbon powder to it and stir for 10 h, filter, remove the solvent by rotary evaporation of the filtrate, and dry in vacuo to obtain a colorless oil, which is the target product [Bmim]OAc.

Embodiment 3

[0025] Dissolve 0.05 mol of [Bmim]Cl in 50 ml of isopropanol, add 2 times the amount of sodium carbonate, stir and react at 60°C for 8 hours, filter, filter and rotary evaporate to obtain an oily liquid, and dry in vacuo to obtain the final product [Bmim] 2 CO 3 .

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Abstract

The invention belongs to the technical field of fine chemistry, and in particular relates to a method for preparing a hindered phenol antioxygen 1010. According to the method provided by the invention, beta-(3,5-ditert-butyl-4-hydroxyphenyl)methyl propionate and pentaerythrotol are used as raw materials and are subjected to ester exchange reaction to obtain the hindered phenol antioxygen 1010; the ester exchange reaction is carried out in an alkaline ion liquid catalysis system. According to the method provided by the invention, alkali ion liquid is used as a catalyst and the catalytic activity is high; the content of a product reaches 97.5 percent or more, and the yield reaches 95 percent or more. The performance of the alkaline liquid catalyst in 1010 esterification reaction is better that that of catalysts including lithium acetate, sodium methoxide, potassium tert-butoxide, organic tin and the like. An ion liquid catalytic reaction system is used and is environmentally friendly; the catalyst can be cyclically utilized; a product is not easily colored, has high yield and does not contain heavy metal.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and specifically relates to a method for preparing hindered phenol antioxidant 1010. [0002] technical background [0003] Antioxidants have good oxidation resistance, stable oxidation stability and thermal stability, good compatibility with polymers, extremely low volatility, and are not easily lost due to volatilization at high temperatures. It can effectively prevent the damage of light, heat and oxygen to the polymer, significantly improve the performance of the polymer, effectively prolong the life of the polymer, no pollution, no coloring. It can be widely used in general plastics, engineering plastics, synthetic rubber, fiber, resin, ink, paint and other industries. [0004] Antioxidant 1010 (tetra[β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] pentaerythritol ester) is a high molecular weight hindered phenolic antioxidant with low volatility and resistance to extraction Good r...

Claims

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Application Information

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IPC IPC(8): C07C69/732C07C67/03B01J31/02
CPCB01J31/0279B01J31/0284C07C67/03C07C69/732Y02P20/54
Inventor 裴立军张新飞董景辉樊其艳赵新华
Owner CHAMBROAD CHEM IND RES INST CO LTD
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