Method for preparing antioxidant

A technology of hydroxybenzone and s-triazine, which is applied in the field of preparation of antioxidants, can solve problems such as pollution and endanger the health of workers, and achieve the effects of reducing pollution, rationalizing the production process and reducing harm.

Inactive Publication Date: 2010-06-23
天津市北方金恒新材料有限责任公司
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  • Abstract
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Problems solved by technology

Due to the toxicity of hexahydropyridine and acetonitrile, the production process wi...

Method used

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  • Method for preparing antioxidant

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Embodiment Construction

[0009] Add 200 grams of isopropanol and 30 grams of distilled water into a 500ml four-necked bottle, add 24.9 grams of cyanuric acid and 18.5 grams of paraformaldehyde under stirring, and add 3.7 grams of catalyst triethylamine and 1.85 grams of dibutylamine after the dispersion is uniform. After stirring evenly, under the protection of nitrogen, when the temperature was raised to 65°C, 120 grams of 2.6-di-tert-butylphenol was added, and then the temperature was raised to reflux state. After reacting for 10 hours, the temperature was naturally lowered, cooled to 10°C, suction filtered, and dried to obtain The crude product was 148 grams, and 133 grams of the product were refined through recrystallization, with a yield of 88%. The mother liquor was recovered to obtain 3.2 grams of the product, with a yield of 2%, and the total yield was over 90%.

[0010] Reaction equation of the present invention is:

[0011]

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Abstract

A method for preparing 1.3.5-tri(3.5-di tert butyl-4-hydroxybenzaldehyde)1.3.5-s-triazine.2.4.6-(1H, 2H, 3H) triketone is characterized by adding isopropanol and distilled water into a reactor, adding cyanuric acid and paraformaldehyde under stirring, adding catalysts including triethylamine and dibutylamine after uniform dispersion, after uniform stirring, raising the temperature to 60-80 DEG C under the protection of nitrogen, after adding 2.6-di tert butyl phenol, continuing raising the temperature until the reflux state, naturally cooling after reacting for 10-12h, carrying out pumping filtration after cooling to 10 DEG C, drying to obtain the crude product and obtaining the product through recrystallization and refining. The method has the following advantages and benefits: 1. the production technology process is more reasonable and convenient and the production efficiency is improved; 2. the pollution to the environment is lightened and the harm to the production workers is reduced; and 3. the yield of the product is improved and the total yield is over 90%.

Description

Technical field: [0001] The present invention relates to a production method of chemical products, in particular to an antioxidant-1.3.5-tris(3.5-di-tert-butyl-4-hydroxybenzene)1.3.5-s-triazine.2.4.6- Preparation method of (1H, 2H, 3H) triketone. Background technique: [0002] 1.3.5-tris(3.5-di-tert-butyl-4-hydroxybenzene) 1.3.5-s-triazine.2.4.6-(1H, 2H, 3H) triketone, the commercial name is antioxidant 3114, its The traditional preparation and synthesis method is: put cyanuric acid, paraformaldehyde, hexahydropyridine, triethylamine, acetonitrile and distilled water into the reactor in order to stir, heat, reflux for 30 minutes and heat filter, under nitrogen protection, After adding 2.6-di-tert-butylphenol at 50°C, continue to stir, heat, and reflux for 7 hours to complete the reaction, cool down, filter with suction, and dry to obtain the crude product, which is refined by solvent to obtain the final product with a yield of 88%. The final product is recovered from the mo...

Claims

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Application Information

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IPC IPC(8): C07D251/30
Inventor 索士满
Owner 天津市北方金恒新材料有限责任公司
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