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Synthetic method of water-soluble ultraviolet absorber bp-9

A technology of BP-9, synthesis method, applied in the preparation of sulfonate, organic chemistry and other directions, can solve the problems of complex sulfonation process, acid waste water pollution, poor sulfonation selectivity, etc., and achieve high yield and purity, corrosiveness Small, stable effect

Active Publication Date: 2016-03-09
HUANGGANG MEIFENG CHEM TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, BP-9 is mainly prepared by methylation reaction and sulfonation reaction at home and abroad. The methylating agent used in the methylation reaction is usually methyl halide, dimethyl sulfate, trimethyl phosphate, etc. The catalyst used is Inorganic bases, organic bases, etc.; although inorganic bases and organic bases are widely used as catalysts and are suitable for a variety of methylation reaction processes, there are poor selectivity and low product purity in the polyhydroxy methylation process and other disadvantages; the sulfonation reaction industry mainly includes concentrated sulfuric acid sulfonation, fuming sulfuric acid sulfonation, chlorosulfonic acid sulfonation, sulfur trioxide sulfonation and other processes, although these processes are widely used at home and abroad, and can meet the absolute Most of the sulfonation process production requirements, but there are disadvantages such as complex sulfonation process, serious acid wastewater pollution, poor sulfonation selectivity, etc.

Method used

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  • Synthetic method of water-soluble ultraviolet absorber bp-9
  • Synthetic method of water-soluble ultraviolet absorber bp-9
  • Synthetic method of water-soluble ultraviolet absorber bp-9

Examples

Experimental program
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Effect test

Embodiment 1

[0026] ①Methylation reaction: Put 123kg of 2,2',4,4'-tetrahydroxybenzophenone, 2.95kg of zinc chloride and a mixture of 295L dichloroethane + 295L absolute ethanol into the reactor Solvent 590L, heat and stir to dissolve, heat up to 45~50℃, add 148kg of dimethyl sulfate dropwise, after 2h dripping, keep the reaction for 6h; cool to room temperature, add 148L of water and stir to dissolve, then stand for stratification, separate the organic phase , The water phase is extracted twice with dichloroethane, the amount of each is 50L, the organic phases are combined, the solvent is recovered by distillation, and the cooling and crystallization are performed to obtain 2,2'-dihydroxy-4,4'dimethoxybenzophenone About 130kg, the molar yield is 95% (calculated based on 2,2',4,4'-tetrahydroxybenzophenone);

[0027] ② Sulfonation reaction: Put 130kg of the methylated product 2,2'-dihydroxy-4,4'dimethoxybenzophenone and 610L of dichloroethane into the reaction kettle, heat and stir to dissolve,...

Embodiment 2

[0031] ①Methylation reaction: put 123kg of 2,2',4,4'-tetrahydroxybenzophenone, 2.46kg of copper chloride and a mixture of 276L dichloroethane + 276L absolute ethanol into the reactor Solvent 552L, heat and stir to dissolve, heat up to 45~50℃, add 148kg of dimethyl sulfate dropwise, after 2h dripping, keep the reaction for 6h; cool to room temperature, add 148L of water and stir to dissolve, then stand for stratification and separate the organic phase , The water phase is extracted twice with dichloroethane, 50L each time, the organic phases extracted twice are combined, the solvent is recovered by distillation, and the crystal is cooled to obtain 2,2'-dihydroxy-4,4'dimethoxydi Benzophenone 124kg;

[0032] ②Sulfonation reaction: put the methylated product 2,2'-dihydroxy-4,4'dimethoxybenzophenone and 596L of chloroform into the reaction kettle, heat and stir to dissolve, raise the temperature To 60~65℃, add 99kg of sulfamic acid in 3 times, keep the reaction for 5h, cool to room t...

Embodiment 3

[0035] ①Methylation reaction: put 123kg of 2,2',4,4'-tetrahydroxybenzophenone, 3.1kg of nickel chloride and a mixture of 307L dichloroethane + 307L absolute ethanol into the reactor Solvent 614L, heat and stir to dissolve, warm up to 45~50℃, add 184.5kg of dimethyl sulfate dropwise, after 2h dripping, keep reaction for 6h; cool to room temperature, add 185L water and stir to dissolve, then stand for layering and separate organic The water phase is extracted twice with dichloroethane, 55L each time, the two organic phases are combined, the solvent is recovered by distillation, and the crystal is cooled to obtain 2,2'-dihydroxy-4,4'dimethoxydiphenyl Methyl ketone 127kg;

[0036] ②Sulfonation reaction: Put the methylated product 2,2'-dihydroxy-4,4'dimethoxybenzophenone and 610L of dichloroethylene into the reaction kettle, heat and stir to dissolve, and increase the temperature. To 60~65℃, put in 112kg of sulfamic acid in 3 times, keep the reaction for 5h, cool to room temperature,...

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Abstract

The invention discloses a synthetic method of a water soluble ultraviolet light absorber BP-9. The method mainly comprises the following process steps: (1) carrying out methylation on the main raw materials of 2, 2', 4, 4'-tetrahydroxyl benzophenone, a transition metal salt catalyst and a mixed solvent which is prepared from dichloroethane and anhydrous ethanol in equal parts by weight to obtain 2, 2'-dihydroxyl-4, 4'-dimethoxyl benzophenone; (2) carrying out sulfonation reaction on the main raw materials of methylate, sulfamic acid and C1-C3 halohydrocarbon to obtain 2, 2'-dihydroxyl-4, 4'-dimethoxyl benzophenone-5, 5'-disulfonic acid; and (3) carrying out neutral reaction on the main raw materials of sulfonated product, inorganic base and ethanol water to finally obtain the BP-9 product. The synthetic method disclosed by the invention is few in reaction step, low in cost, high in product purity and stable in quality, and raw materials are easily available.

Description

Technical field [0001] The invention relates to a method for synthesizing an ultraviolet absorber, in particular to a method for synthesizing a water-soluble ultraviolet absorber BP-9. Background technique [0002] BP-9 is a water-soluble ultraviolet absorber with an absorption wavelength of 280~380nm, and its chemical name is 2,2'-dihydroxy-4,4'dimethoxybenzophenone-5,5'-disulfon Sodium is a series of benzophenone ultraviolet absorbers. It absorbs UV-A and UV-B bands at the same time. Compared with ultraviolet absorbers BP-1, BP-2, BP-3, BP-4, etc. , Its anti-ultraviolet function has been greatly improved, and it is an excellent sunscreen agent. Because of its excellent water solubility and extremely low side effects, it is widely used in water-soluble cosmetics, water-soluble inks, paints, and paints. [0003] At present, BP-9 is mainly prepared by methylation reaction and sulfonation reaction at home and abroad. The methylating agent used in the methylation reaction is usually...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/32C07C309/44
Inventor 汪敦佳刘建军李小林殷国栋范玲徐文立魏先红郑静
Owner HUANGGANG MEIFENG CHEM TECH
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