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Preparation method of anti-aging agent

A catalyst and content technology, applied in the direction of organic chemistry, etc., can solve the problems of no quantitative intermediate control method and high IBA content, and achieve the effect of reducing the generation of carcinogens and the emission of three wastes

Active Publication Date: 2020-04-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no quantitative intermediate control method yet, and there is no solution to the problem of high IBA content in finished products for the time being, and we can only deal with defective products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 620 grams of aniline and 50 grams of 30% hydrochloric acid to the reactor, stir at 100°C for 3 hours to remove the water in the hydrochloric acid, then add 1348 grams of acetone dropwise for about 5 hours while stirring at 120°C, and maintain for 0.5h , 10.3% of acetone content, 9.5% of aniline content, 2.5% of mesityl oxide content and 23.0% of 2,2,4-trimethyl-1,2-dihydroquinoline in the detected reaction solution. The reaction solution was neutralized by adding 53 grams of liquid caustic soda, the water phase was separated, and the organic phase was distilled under vacuum at -0.098MPa to obtain 483 grams of the pot liquid, that is, the finished anti-aging agent TMQ. After testing, 2,2,4-trimethyl-1 , The content of 2-dihydroquinoline di, tri, tetramer is 49.32%, and the content of isopropyl diphenylamine is 8.3ppm.

Embodiment 2

[0022] Other conditions are the same as in Example 1, except that the addition of hydrochloric acid is 60 grams. After testing, the content of acetone in the TMQ reaction solution is 10.9%, the content of aniline is 7.5%, the content of mesityl oxide is 1.5%, and 2,2,4-tri Methyl-1,2-dihydroquinoline 13.4%. The obtained TMQ finished product had a content of 2,2,4-trimethyl-1,2-dihydroquinoline di-, tri-, and tetramers of 40.30%, and a content of isopropyldiphenylamine of 2.3 ppm.

Embodiment 3

[0024] Other conditions are the same as in Example 1, except that the catalyst is benzenesulfonic acid. After testing, the content of acetone in the TMQ reaction liquid is 15.6%, the content of aniline is 8.5%, the content of mesityl oxide is 4.3%, and the content of 2,2,4-trimethyl-1,2-dihydroquinoline is 23.4%. The obtained TMQ finished product contained 43.30% of 2,2,4-trimethyl-1,2-dihydroquinoline di-, tri-, and tetramers, and 7.3 ppm of isopropyldiphenylamine.

[0025] Example 3

[0026] Other conditions are the same as in Example 1, except that the catalyst is sulfuric acid. After testing, the content of acetone in the TMQ reaction solution is 19.6%, the content of aniline is 5.5%, the content of mesityl oxide is 2.3%, and the content of 2,2,4-trimethyl-1,2-dihydroquinoline is 24.8%. In the obtained TMQ product, the content of 2,2,4-trimethyl-1,2-dihydroquinoline di-, tri-, and tetramers was 63.30%, and the content of isopropyldiphenylamine was 3.8ppm.

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PUM

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Abstract

The invention belongs to the technical field of fine chemical engineering, and relates to a preparation method of an anti-aging agent, in particular to preparation of TMQ. Aniline, a catalyst and acetone are subjected to a condensation polymerization reaction to generate a TMQ condensation polymerization reaction solution; the content of key components in the TMQ polycondensation reaction liquid is controlled, neutralization, water separation and oil phase distillation are performed to obtain a TMQ finished product, and the quality of the finished product TMQ is controlled by controlling the content of the key components, so that the generation of carcinogens is reduced, the generation of TMQ inferior-quality products is controlled, the emission of three wastes is reduced, and the environment-friendly production of the TMQ is realized.

Description

technical field [0001] The present invention relates to a preparation method of anti-aging agent, especially the preparation method of the content of impurity isopropyl diphenylamine (IBA for short) in anti-aging agent TMQ, which is a relatively cheap, green and environment-friendly preparation method of anti-aging agent TMQ. It belongs to the technical field of organic synthesis. Background technique [0002] Anti-aging agent TMQ is the two, three and four polymers of 2,2,4-trimethyl-1,2-dihydroquinoline, also known as anti-aging agent RD, mainly used as an antioxidant for rubber and rubber products. It is suitable for natural rubber, synthetic rubber and latex. It has a strong inhibitory effect on the catalytic oxidation of copper, manganese and other harmful metal ions. It has good compatibility with rubber, low volatility, small blooming resistance and high extraction resistance. It is widely used in the rubber processing industry at home and abroad. Whether it is ordin...

Claims

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Application Information

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IPC IPC(8): C07D215/06
CPCC07D215/06
Inventor 刘建韦志强付春赵福宝马敏
Owner CHINA PETROLEUM & CHEM CORP
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