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Method for recovering antioxidant 1098 by-product

A recovery method and technology for by-products, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylic acid esters, etc., can solve problems such as few recovery studies, achieve simple and controllable operation, and improve utilization rate , Recycling operation is simplified and controllable

Active Publication Date: 2019-07-26
JIANGSU JIYI NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, in the prior art, the residual antioxidant 1098 by-product (such as figure 1 Shown) There are very few recycling studies

Method used

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  • Method for recovering antioxidant 1098 by-product
  • Method for recovering antioxidant 1098 by-product
  • Method for recovering antioxidant 1098 by-product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A recovery method of antioxidant 1098 by-product, the steps are as follows:

[0030] (1) Obtaining of antioxidant 1098 mother liquor: add 5.84g (0.02mol) 3,5-di-tert-butyl-4-hydroxyphenylpropionate methyl ester in the reaction flask equipped with mechanical stirrer, thermometer and reflux condenser , 1.174g (0.0101mol) 1,6-hexamethylenediamine as raw material and 40ml xylene, first pass into 5min of N 2 , then add 0.0033g of basic catalyst sodium methoxide, in N 2 Under protection, the pressure is -0.075MPa, heating reaction, the temperature is controlled at 167 ~ 170 ° C, after 6 ~ 8 hours of reaction, add 20ml of 100% ethanol to dissolve, recrystallize, age for 1 ~ 2 hours, centrifugal filtration, carry out 2 ~ 3 Once, the white crystal obtained by drying is antioxidant 1098, which weighs 5.739g, and the remaining solution is antioxidant 1098 mother liquor;

[0031] (2) Mother liquor pretreatment: remove the solvent from the mother liquor under reduced pressure, the...

Embodiment 2

[0039] A recovery method of antioxidant 1098 by-product, the steps are as follows:

[0040] (1) Obtaining of antioxidant 1098 mother liquor: add 5.84g (0.02mol) 3,5-di-tert-butyl-4-hydroxyphenylpropionate methyl ester in the reaction flask equipped with mechanical stirrer, thermometer and reflux condenser , 1.195g (0.0103mol) 1,6-hexamethylenediamine as raw material and 40ml xylene, first pass into 5min of N 2 , then add 0.0033g of basic catalyst sodium methoxide, in N 2 Under protection, the pressure is -0.075MPa, heating reaction, the temperature is controlled at 167 ~ 170 ° C, after 6 ~ 8 hours of reaction, add 20ml of 100% ethanol to dissolve, recrystallize, age for 1 ~ 2 hours, centrifugal filtration, carry out 2 ~ 3 Once, the white crystal obtained by drying is antioxidant 1098, which weighs 5.782g, and the remaining solution is antioxidant 1098 mother liquor;

[0041] (2) Mother liquor pretreatment: remove the solvent from the mother liquor under reduced pressure, the...

Embodiment 3

[0049] A recovery method of antioxidant 1098 by-product, the steps are as follows:

[0050] (1) Obtaining of antioxidant 1098 mother liquor: add 5.84g (0.02mol) 3,5-di-tert-butyl-4-hydroxyphenylpropionate methyl ester in the reaction flask equipped with mechanical stirrer, thermometer and reflux condenser , 1.195g (0.0103mol) 1,6-hexamethylenediamine as raw material and 40ml xylene, first pass into 5min of N 2 , then add 0.0033g of basic catalyst sodium methoxide, in N 2 Under protection, the pressure is -0.075MPa, heating reaction, the temperature is controlled at 167 ~ 170 ° C, after 6 ~ 8 hours of reaction, add 20ml of 100% ethanol to dissolve, recrystallize, age for 1 ~ 2 hours, centrifugal filtration, carry out 2 ~ 3 Time, the white crystal that drying obtains is antioxidant 1098, weighs it to be 5.781g, and the remaining solution is antioxidant 1098 mother liquor;

[0051] (2) Mother liquor pretreatment: Ethanol is evaporated off mother liquor under reduced pressure, t...

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Abstract

The invention discloses a method for recovering an antioxidant 1098 by-product. The method includes carrying out reduced pressure distillation treatment on a specific antioxidant 1098 mother liquor; and separating and recovering the antioxidant 1098 by-product and 3,5-methyl ester in the mother liquor by adopting a thermal filtration method to obtain the antioxidant 1098 by-product with higher purity. The recovery method has the advantages of tight connection, reasonable collocation, synergy, simplified and controllable recovery operation, high safety, high recovery rate of the antioxidant 1098 byproduct and 3,5-di-tert-butyl-4-hydroxyphenylpropionate, and realization of environmental benefits and economic benefits.

Description

technical field [0001] The invention relates to a method for recovering by-products of antioxidant 1098, which belongs to the technology for recovering by-products. Background technique [0002] Antioxidant 1098 (N,N'-bis-(3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl)hexamethylenediamine) is an intramolecular complex antioxidant with The dual effects of hindered phenol and hindered amine antioxidants, good thermal stability, anti-separation, anti-radiation tin radiation and compatibility with resins, is an excellent antioxidant for polymer materials. Agent and heat stabilizer, mainly used for polyamide and polyacetal, also can be used for polyolefin, polyester, natural or synthetic rubber, and other polymer compounds sensitive to thermal oxidation, the general dosage is 0.3-1.0%, When it is used in polyamide fiber, the advantage of antioxidant 1098 is particularly obvious. With the maturity of localization technology, the application and production of antioxidant 1098 con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C235/34C07C67/48C07C69/732C07C67/56
CPCC07C67/48C07C67/56C07C231/24C07C235/34C07C69/732
Inventor 郭骄阳赵崇鑫
Owner JIANGSU JIYI NEW MATERIAL CO LTD
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