Process for producing benzophenone ultraviolet ray absorbent

A technology of benzophenones and production process, which is applied in the field of production process of benzophenone ultraviolet absorbers, can solve the problems of potential safety hazards, long reaction time, cumbersome post-processing, etc., and achieve energy saving and Labor costs, reduced consumption of organic solvents, and short time-consuming effects

Active Publication Date: 2017-04-26
江苏富比亚化学品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the process route of benzophenone ultraviolet absorbers is mostly prepared by the reaction of benzophenone compounds and alkyl halides in alkaline aqueous solution using phase transfer catalysts, such as adding water in the reactor in Chinese patent CN100591650C, Using a quaternary ammonium salt or a tertiary amine as a catalyst, the alkyl bromide and 2,4-dihydroxybenzophenone are refluxed in an alkali solution to prepare 2-hydroxyl-4-n-octyloxybenzophenone, and after the reaction Ethanol recrystallization purification and various post-treatments are required, the reaction takes a long time and post-processing is cumbersome
In the Chinese patent CN102503795A, 2,4-dihydroxybenzophenone is reacted with dioctyl carbonate, and after the reaction is completed, ethanol recrystallization is used to purify the product 2-hydroxyl-4-n-octyloxybenzophenone. In this invention It takes a long time for the reaction conditions to be used in industrial production, and there are still potential safety hazards when using organic solvents such as ethanol for recrystallization and centrifugation

Method used

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  • Process for producing benzophenone ultraviolet ray absorbent
  • Process for producing benzophenone ultraviolet ray absorbent
  • Process for producing benzophenone ultraviolet ray absorbent

Examples

Experimental program
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Effect test

Embodiment 1

[0069] 10kg 2,4-dihydroxybenzophenone (UV-0), 10.5kg chlorooctane, 6kg soda ash (99%), 50g polyethylene glycol-400 (99%), 30g potassium bromide (99%) %) into the reaction kettle, start stirring, heat up to 180°C for reflux reaction, heat preservation reaction for 2 hours, add water to stir and wash with water for 30 minutes, let stand for 30 minutes, separate the lower layer of waste water, and transfer the upper layer of product to a high temperature still to be distilled;

[0070]Put the UV-531 crude product obtained by the above alkylation reaction into a stainless steel still, add 1% 2,6-di-tert-butyl-4-methylphenol (BHT) and 2% tris(2,4-di tert-butylphenyl) phosphite (antioxidant 168), warming up to 65°C, stirring for 1h, and then in 1x10 -2 Heating distillation under pa vacuum condition, before 130℃, the distillate is chlorinated n-octane, which is recovered by secondary condensation (stainless steel condenser, condensation area 20m 2 , primary water cooling +5°C and pr...

Embodiment 2

[0073] Put 10kg of n-octanol (99%) and 40g of N,N-dimethylacetamide into the enamel reaction kettle, the pressure inside the kettle is -0.04MPa, heat up to 60°C and keep it warm, slowly drop 11kg of chlorinated chlorinated under the liquid surface After the addition of sulfone and thionyl chloride, keep warm for 3 hours. After the sampling and analysis are qualified, the material is discharged. After washing with water for 3 times, add solid soda ash and water to adjust the pH value to 8. The lower layer of waste water is separated, and the upper layer of chlorooctane is stored. spare tank;

[0074] Put 10kg UV-0, 11kg chlorooctane, 7kg soda ash (99%), 60g alkyltrimethylammonium chloride (99%), and 40g potassium bromide (99%) into the reactor, start stirring, and heat up Reflux reaction at 170°C, keep warm for 2 hours, add water to stir and wash with water for 40 minutes, let stand for 30 minutes, separate the lower layer of wastewater, and transfer the upper layer product to ...

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Abstract

The invention discloses a process for producing a benzophenone ultraviolet ray absorbent, and the process includes mixing of a benzophenone compound A and an alkyl halide for alkylation to obtain a benzophenone compound B. The alkyl halide can be prepared by the reaction of a primary alcohol and thionyl chloride under catalysis of a tertiary amine. Further, hydration and distillation of the system after the completion of the alkylation are carried out in order to eliminate crystallization and purification steps. The process is simplified, a high purity product is obtained, solvent consumption is reduced, and the cost is reduced.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a production process of a benzophenone ultraviolet absorber. Background technique [0002] UV absorber is a kind of light stabilizer, which can absorb the ultraviolet part of sunlight and fluorescent light source without changing itself. Benzophenone ultraviolet absorbers can strongly absorb ultraviolet rays with a wavelength of 270-330nm, and can be used in various plastics, such as polyethylene, polypropylene, polystyrene, ABS resin, polycarbonate, polyvinyl chloride, polyester It has good compatibility with resin and low volatility, and it can also be used as a light stabilizer for various coatings. [0003] At present, the process route of benzophenone ultraviolet absorbers is mostly prepared by the reaction of benzophenone compounds and alkyl halides in alkaline aqueous solution by using phase transfer catalysts, such as adding water in the reactor in Chinese patent CN10059165...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/64C07C49/84
CPCC07C45/64C07C49/84
Inventor 李焕成吴邦元施波孙剑锋张文忠陆伟
Owner 江苏富比亚化学品有限公司
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