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Microchannel continuous sulfonation synthesis method of ultraviolet light absorber BP-4

The technology of BP-4 and absorbent, which is applied in the field of preparation of ultraviolet absorbent BP-4, can solve the problems of corrosiveness of reaction equipment, cumbersome post-processing and high production cost, and achieves low industrial cost, low raw material cost and easy operation. Effect

Pending Publication Date: 2022-01-07
HUBEI NORMAL UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the present invention is aimed at the synthesis process of the existing ultraviolet absorber BP-4, all of which have high industrial production costs, serious corrosion to the reaction equipment, great potential safety hazards, or long production time and cumbersome post-processing and other issues, we improved the sulfonation process of the ultraviolet absorber BP-4 according to the catalog of 18 key regulated hazardous chemical processes and safety control requirements issued by the State Administration of Work Safety, and provided a safe and effective ultraviolet absorber BP- 4 Microchannel Continuous Sulfonation Synthesis Method

Method used

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  • Microchannel continuous sulfonation synthesis method of ultraviolet light absorber BP-4
  • Microchannel continuous sulfonation synthesis method of ultraviolet light absorber BP-4
  • Microchannel continuous sulfonation synthesis method of ultraviolet light absorber BP-4

Examples

Experimental program
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Effect test

Embodiment 1

[0032] The microchannel continuous sulfonation synthesis of the ultraviolet absorber BP-4 of the present embodiment, including the steps of: 22.8 g of 2-hydroxy-4-methoxy-diphenone ketone (dissolved in 90 ml of dichloroethane) Configure a clear raw material solution, 2-hydroxy-4-methoxy-benzophenone raw material solution and trioxide, respectively, from 25 ml / min, 0.64 l / min, respectively, and flow into the microchannel reactor. The reaction temperature is 100 ° C, the pressure is 1.0 MPa, the residence time is 2.0 min, the reaction liquid flowing out of the reactor is collected, and the ultraviolet absorbent BP-4 product solution, the organic solvent is recovering, and the crystal is cooled to obtain a light yellow ultraviolet absorption. The agent BP-4 was 32 g, and the purity of the BP-4 crude material was 96.13%.

[0033] The above product was crystallized from 160 ml of ethanol, filtered, dried. 99.57% (see attached figure 1 : High performance liquid chromatograph: Agilen...

Embodiment 2

[0040] The microchannel continuous sulfonation synthesis of the ultraviolet absorber BP-4 of the present embodiment includes the steps of: 2-hydroxy-4-methoxy-dibenzophenone 228 g is soluble in 900 ml of trichloroethane configuration Curable raw material solution, 2-hydroxy-4-methoxy-dibenzophenone raw material solution and trioxide, respectively, from 30 ml / min, 0.77 l / min, respectively, feed into the microchannel reactor, reaction The temperature is 90 ° C, the pressure is 1.5 MPa, the residence time is 3.3 min, collecting the reaction liquid flowing out of the reactor to obtain an ultraviolet absorber BP-4 product solution, and the organic solvent is recovered, and the crystal is cooled to obtain a light yellow ultraviolet absorber BP. -4 crude 310g, the BP-4 crude purity was 96.26%.

[0041] The above product was crystallized from 1.7L ethanol, filtered, dried. It is 99.43%.

[0042] In this example, the apparatus for preparing a microchannels of UV absorbent BP-4 is used ...

Embodiment 3

[0044] The microchannel continuous sulfonation synthesis of the ultraviolet absorber BP-4 of the present embodiment includes the steps of: weighing 2-hydroxy-4-methoxy-dibenzophenone 114 g is formed into 450 ml of trichlorethylene. The clear raw material solution, 2-hydroxy-4-methoxy-diphenone ketone raw material solution and sulfur dioxide are respectively 20 ml / min, 0.51L / min, respectively, and flow into the microchannel reactor, reaction temperature. It is 50 ° C, the pressure is 0.5 MPa, the residence time is 4.5min, the reaction mixture flowing out of the reactor is collected, and the ultraviolet absorber BP-4 product solution is obtained, and the organic solvent is recovered at normal pressure, cooling crystals, to obtain a pale yellow ultraviolet absorber BP- 4 crude 155 g, the BP-4 crude purity was 95.36%.

[0045] The above product was crystallized from 1.2 l ethanol, filtered, dried. 99.29%

[0046] In this example, the apparatus for preparing the microfield continuo...

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Abstract

The invention discloses a microchannel continuous sulfonation synthesis method and device for an ultraviolet light absorber BP-4, and the method comprises the following steps: dissolving 2-hydroxy-4-methoxy-benzophenone in a halogenated hydrocarbon solvent to prepare a raw material solution with the concentration of 1.0 mol / L; feeding a 2-hydroxy-4-methoxy-benzophenone solution and sulfur trioxide into a micro-channel reactor in a parallel flow manner at the speeds of 20.0-30.0 ml / min and 0.51-0.77 L / min respectively, conducting reacting at the temperature of 50-150 DEG C under the pressure of 0.5-2.0 MPa for 1.0-5.0 minutes, collecting reaction liquid flowing out of the reactor to obtain an ultraviolet light absorber BP-4 product solution, conducting distilling at normal pressure to recover an organic solvent, conducting cooling and crystallizing, and conducting refining to obtain an ultraviolet light absorber BP-4 product. The total synthesis yield of the BP-4 product is greater than or equal to 95%, and the purity of the BP-4 product is greater than or equal to 99%. The method provided by the invention has the advantages of high synthesis yield, high product purity, no generation of wastewater and waste acid, environmental protection, safe and convenient production, low cost, and suitableness for industrial production.

Description

Technical field [0001] The present invention relates to the preparation method of ultraviolet absorber BP-4, in particular, a microchannel continuous sulfonation synthesis of ultraviolet absorbent BP-4. Background technique [0002] UV absorbent BP-4 (chemical name: 2-hydroxy-4-methoxy-diphenone-5-sulfonic acid) belongs to a diphenyl ketone compound, is a broad-spectrum ultraviolet absorber with absorption efficiency High, non-toxic, non-tertiary side effects, good light, thermal stability, etc. In the United States and Europe, the frequency is high, widely used in sunscreen cosmetics such as sunscreen cream, cream, honey, emulsion, oil, as an anti-ultraviolet finishing agent, a good anti-aging and soft effects of cotton fabric, polyester fiber. It is mainly used in water-soluble cosmetics to sunscreen, and can also be used in other water-soluble inks, coatings, and the like as ultraviolet absorbers. [0003] At present, there are two synthetic methods of synthesis of ultraviolet...

Claims

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Application Information

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IPC IPC(8): C07C303/06C07C309/44
CPCC07C303/06C07C309/44
Inventor 汪敦佳殷国栋胡艳军宋红刚徐文立刘建军
Owner HUBEI NORMAL UNIV
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