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Method for producing 2-hydroxyl-4-methoxybenzophenone-5-sulfonic acid

A technology of methoxybenzophenone and sulfonic acid benzophenone, which is applied in the field of water-soluble ultraviolet absorbers, can solve the problems of hidden safety hazards in product quality, high solvent residues, and high environmental protection pressure, and achieve economic benefits Significant environmental benefits, reduced production costs, and improved safety performance

Active Publication Date: 2013-01-09
宜都市华阳化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Dichloroethane in the above process is a highly toxic, highly residual organic solvent and carcinogenic substance that is internationally restricted, with serious safety hazards and great pressure on environmental protection
At the same time, the product has high solvent residue, hidden safety hazards in product quality, low yield and high production cost

Method used

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  • Method for producing 2-hydroxyl-4-methoxybenzophenone-5-sulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Crude:

[0025] Put 100 kg of qualified 2-hydroxy-4-methoxybenzophenone, 50 kg of chlorosulfonic acid, 100 kg of dimethyl carbonate, and 10 kg of water into the crude product reaction kettle for reaction, and the temperature is controlled at 23-25°C , Insulated for 18 hours to obtain crude BP-4.

[0026] refined:

[0027] Dissolve 100 kg of crude BP-4 in a mixed solvent of 200 kg of dimethyl carbonate, 50 kg of higher aliphatic alcohol and 10 kg of water, recrystallize, and separate the solid-liquid phase to obtain solid phase BP-4. The product yield is 92.1%, and the product purity is 99.5%.

Embodiment 2

[0029] Crude:

[0030] Put 200 kg of qualified 2-hydroxy-4-methoxybenzophenone boutique, 250 kg of chlorosulfonic acid, 1000 kg of dimethyl carbonate, and 100 kg of water into the crude product reaction kettle for reaction, and the temperature is controlled at 30-32 °C, heat preservation reaction for 15 hours to obtain the crude product of BP-4.

[0031] refined:

[0032] Dissolve 200 kg of crude BP-4 in a mixed solvent of 1,000 kg of dimethyl carbonate, 200 kg of higher alcohol, and 30 kg of water, recrystallize, separate the solid-liquid phase, and obtain solid phase BP-4. The product yield is 92.3%, and the product purity is 99.7%.

Embodiment 3

[0034] Crude:

[0035] Put 100 kg of qualified 2-hydroxy-4-methoxybenzophenone boutique, 200 kg of chlorosulfonic acid, 200 kg of dimethyl carbonate, and 50 kg of water into the crude product reaction kettle for reaction, and the temperature is controlled at 36-38 °C, heat preservation reaction for 20 hours to obtain the crude product of BP-4.

[0036] refined:

[0037] Dissolve 100 kg of crude BP-4 in a mixed solvent of 250 kg of dimethyl carbonate, 150 kg of higher alcohol, and 50 kg of water, recrystallize, and separate the solid-liquid phase to obtain solid phase BP-4. The product yield is 92%, and the product purity is 99.6%.

[0038] The crude product of BP-4 obtained in the present invention refers to: the purity of BP-4 is 90-95%; the refined product refers to the purity of BP-4 above 99%.

[0039] The BP-4 fine product obtained by the present invention has the following technical indicators:

[0040] technical indicators

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Abstract

The invention provides a method for producing benzophenone ultraviolet absorbent 2-hydroxyl-4-methoxybenzophenone-5-sulfonic acid (BP-4). The invention uses a BP-3 refined product and chlorsulfonic acid to synthesize and prepare the BP-4 in methyl carbonate, and is characterized in that the method comprises the following steps: adding BP-3 refined product, chlorsulfonic acid, methyl carbonate andwater according to a production ratio into a crude product reaction kettle, controlling the temperature to be 23-38 DEG C, keeping temperature and reacting for 18-20 hours to obtain a BP-4 crude product; dissolving the BP-4 crude product in the mixed solvent of the methyl carbonate and a latent solvent, recrystallizing, separating solid phase from liquid phase to obtain the solid phase BP-4 refined product; refining and drying the BP-4 refined product to obtain a finished product. The invention reduces the harmful solvent residue of the product, decreases production cost, and has notable economic benefit and environmental benefit. The product yield reaches 92% and the product purity is increased to 99.5% from 99%.

Description

technical field [0001] The present invention relates to a kind of production method of water-soluble ultraviolet absorber, specifically benzophenone ultraviolet absorber 2-hydroxyl-4-methoxy-5-sulfonic acid benzophenone (hereinafter referred to as BP-4) production method. Background technique [0002] In recent years, as the earth's ozone layer has been destroyed more and more seriously, the sun's ultraviolet radiation on the earth has become more and more intense. Developed countries such as Europe and the United States have made mandatory regulations on the proportion of ultraviolet absorbers in daily cosmetics in the last period. In recent years, my country has also begun to pay attention to the content of ultraviolet absorbers in various products. 2-Hydroxy-4-methoxybenzophenone-5 sulfonic acid, also known as Sunscreen No. 3 (BP-4), is an excellent water-soluble broad-spectrum ultraviolet absorber with high absorption efficiency, non-toxic, No teratogenic side effects,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/44C07C303/08C07C303/44A61K8/46
Inventor 赵定春袁明翔孙大明
Owner 宜都市华阳化工有限责任公司
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