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Synthetic technology of anti-oxidant 3114

A synthesis process and antioxidant technology, applied in the field of synthesis process of antioxidant 3114, can solve the problems of unrecyclable recycling, adverse effects on the environment, multiple by-products, etc., and achieve high reusability and good chemical stability and thermal stability, the effect of short reaction time

Inactive Publication Date: 2019-08-23
JIANGSU JIYI NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this paper, the catalyst used in the one-step reaction is HMTA, which cannot be recycled and reused. Improper disposal will also cause adverse effects on the environment, and the temperature of the one-step reaction is fixed, which easily generates more by-products

Method used

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  • Synthetic technology of anti-oxidant 3114
  • Synthetic technology of anti-oxidant 3114

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) 2,6-di-tert-butylphenol and paraformaldehyde are added to the reactor containing 10-15% dimethylformamide solution according to the ratio of 1:1.1-1.2 substance amount, and The amount of the amine substance is 0.45-0.55% of the amount of the 2,6-di-tert-butylphenol substance, adding triethylamine-butanesulfonic acid cationic ionic liquid, nitrogen protection, and reacting at 90-100°C for 3 ~4h;

[0031] (2) Control the temperature in the reactor to rise to 120-125°C, add cyanuric acid accounting for 25-28% of the amount of 2,6-di-tert-butylphenol, and continue the reaction for 2-3 hours under nitrogen protection;

[0032] (3) After the reaction, the by-product methanol was continuously removed at -0.05 to 0.07 MPa, cooled and crystallized, centrifuged to obtain the crystallized product, washed with deionized water, and then vacuum-dried at 60°C to obtain the target product;

[0033] (4) Distill the centrifugate at 10-100MPa and 30-50°C to remove the dimethylformami...

Embodiment 2

[0038] (1) 2,6-di-tert-butylphenol and paraformaldehyde are added to the reactor containing 10-15% dimethylformamide solution according to the ratio of 1:1.1-1.2 substance amount, and The amount of the amine substance is 0.45-0.55% of the amount of the 2,6-di-tert-butylphenol substance, adding triethylamine-butanesulfonic acid cationic ionic liquid, nitrogen protection, and reacting at 90-100°C for 3 ~4h;

[0039] (2) Control the temperature in the reactor to rise to 120-125°C, add cyanuric acid accounting for 25-28% of the amount of 2,6-di-tert-butylphenol, and continue the reaction for 2-3 hours under nitrogen protection;

[0040] (3) After the reaction, the by-product methanol was continuously removed at -0.05 to 0.07 MPa, cooled and crystallized, centrifuged to obtain the crystallized product, washed with deionized water, and then vacuum-dried at 60°C to obtain the target product;

[0041] (4) Distill the centrifugate at 10-100MPa and 30-50°C to remove the dimethylformami...

Embodiment 3

[0046] (1) 2,6-di-tert-butylphenol and paraformaldehyde are added to the reactor containing 10-15% dimethylformamide solution according to the ratio of 1:1.1-1.2 substance amount, and The amount of the amine substance is 0.45-0.55% of the amount of the 2,6-di-tert-butylphenol substance, adding triethylamine-butanesulfonic acid cationic ionic liquid, nitrogen protection, and reacting at 90-100°C for 3 ~4h;

[0047] (2) Control the temperature in the reactor to rise to 120-125°C, add cyanuric acid accounting for 25-28% of the amount of 2,6-di-tert-butylphenol, and continue the reaction for 2-3 hours under nitrogen protection;

[0048] (3) After the reaction, the by-product methanol was continuously removed at -0.05 to 0.07 MPa, cooled and crystallized, centrifuged to obtain the crystallized product, washed with deionized water, and then vacuum-dried at 60°C to obtain the target product;

[0049] (4) Distill the centrifugate at 10-100MPa and 30-50°C to remove the dimethylformami...

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Abstract

The invention discloses synthetic technology of anti-oxidant 3114. The anti-oxidant 3114 is prepared through step-by-step reaction at a controlled reaction temperature. The synthetic technology comprises following steps: 1, at 90 to 100 DEG C, raw materials 2, 6-di-tert-butyl phenol and paraformaldehyde are reacted for 3 to 4h; and 2, at 120 to 125 DEG C, a product of the first step is reacted with raw material cyanuric acid for 2 to 3h; wherein in the two steps of reaction, an ionic liquid is taken as a catalyst, and a dimethyl formamide solution is taken as a solvent. According to the synthetic technology, the ionic liquid can be recycled conveniently is taken as a catalyst, the synthetic technology is green, is friendly to the environment, and is high in reaction efficiency.

Description

technical field [0001] The invention relates to a synthesis process of antioxidant 3114, which belongs to the technical field of antioxidant synthesis. Background technique [0002] Antioxidants can delay or prevent the oxidation process of organic materials such as plastics, rubber, fibers, adhesives, food and feed, etc., and prolong the service life of materials. The performance impact is minor. [0003] The chemical name of antioxidant 3114 is 1,3,5-tri-(3,5-di-tert-butyl-4-hydroxybenzyl) isocyanurate, which is a multi-component hindered phenolic antioxidant, slightly soluble Soluble in water, soluble in acetone, benzene, chloroform, N,N-dimethylformamide, ethanol, methanol, non-polluting, non-coloring, due to its large relative molecular mass and high melting point, its volatility is extremely small and its mobility is small. Good water extraction resistance, can endow plastics with excellent thermal oxidation resistance and light oxidation resistance, suitable for pol...

Claims

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Application Information

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IPC IPC(8): C07D251/30
CPCC07D251/30Y02P20/584
Inventor 郭骄阳赵崇鑫
Owner JIANGSU JIYI NEW MATERIAL CO LTD