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Preparation method of high-quality octocrilene sun-screening agent

A technology of octocrylene and sunscreen, which is applied to the preparation of organic compounds, carboxylic acid nitrile preparation, chemical instruments and methods, etc., can solve the problems that affect the use of octocrylene, the product has deep color and low quality, and achieves Easy to control and industrialized production, convenient for industrialization, and the effect of improving yield and quality

Inactive Publication Date: 2019-02-05
ANHUI SHENGNUOBEI CHEM TECH
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0005] However, the octocrylene products prepared in the prior art are usually of low quality, and harmful impurities such as benzophenone, 3,3-diphenylacrylonitrile, 2-cyano-3,3-diphenyl Acrylamide and 2-imino-3,3-diphenylisooctyl acrylate, etc., have relatively high residues in the product, causing the product to fail to meet the quality requirements of cosmetics, which seriously affects the use of octocrylene in cosmetics. used in
[0006] In addition, the octocrylene prepared in the prior art also contains other colored impurities, resulting in a darker color of the product; and the impurity 2-cyano-3,3-diphenylacrylamide will also promote the darker color of the product, Reduce the aesthetics of octocrylene products, thereby affecting its use in cosmetics
[0007] These shortcomings make it difficult for the prepared octocrylene to meet the requirements of cosmetic grade, which limits its wide application in sunscreen cosmetics

Method used

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  • Preparation method of high-quality octocrilene sun-screening agent
  • Preparation method of high-quality octocrilene sun-screening agent
  • Preparation method of high-quality octocrilene sun-screening agent

Examples

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preparation example Construction

[0047] A kind of preparation method of high-quality sunscreen agent octocrylene provided according to the present invention, wherein, described preparation method comprises the following steps:

[0048]Step 1): Recrystallize the raw material Etoridine, so that the content of harmful impurities benzophenone (BP) <500ppm, the content of 3,3-diphenylacrylonitrile (PCN) <50ppm, 2-cyano-3 , 3-diphenylacrylamide (Amide) content <50ppm, and etoridine (ETO) content ≥99.8%;

[0049] Wherein, the raw material Etocurene (ETO) crude product is obtained by the factory, and the impurity content is analyzed by gas chromatography (GC), which contains 1-3% of benzophenone, 0.1-0.3% of 3,3-diphenylacrylonitrile %, containing 95-97% of etoridine and 0.3-1% of 3,3-diphenylacrylamide.

[0050] It is preferable to use alcohol solvents, such as methanol, ethanol, isopropanol and sec-butanol, etc. when recrystallizing etoridine, preferably to use ethanol as the crystallization solvent.

[0051] Whe...

Embodiment 1

[0104] Relying on LEELEN recrystallization treatment:

[0105] Add 1470kg of Etocrine (ETO) crude product and 5880kg of 95% ethanol in the crystallization kettle, wherein, GC analysis contains BP2.48%, PCN 0.17%, ETO 96.47%, Amide 0.81% in the Etocrine crude product.

[0106] Start stirring, raise the temperature to 65°C, and cool down to 43°C for 2 hours after the materials are completely dissolved. After the heat preservation is over, continue to cool down to 8°C for 1 hour. Filtration obtained 1285kg of off-white ETO crystals, which contained BP 308ppm, PCN 46ppm, Amide<10ppm, ETO content was 99.9160%, and the yield was 87.41% according to GC analysis.

[0107] transesterification reaction:

[0108] In the transesterification kettle, add above-mentioned etoridine 1000kg and 3000kg isooctyl alcohol (EH) after the recrystallization. Start stirring, control the vacuum degree of the reaction system at 15-20mmHg, and slowly heat the material in the kettle to 82-85°C, and cont...

Embodiment 2

[0119] Compared with Example 1, the difference is that catalyst sodium carbonate is added at one time in the transesterification reaction.

[0120] After the transesterification reaction, 1197.8 kg of OCT crude product was obtained with a yield of 91.89%. GC analysis content obtained, EH7793.8ppm, BP 728.9ppm, PCN 969.5ppm, ETO 60.3ppm, Amide<10ppm, 2-imino-3,3-ethyl diphenylacrylate (ECDP) 1945.2ppm, and OCT content ( GC) 98.82%.

[0121] Thin film distillation treatment:

[0122] one stage thin film distillation

[0123] Distillation treatment parameter settings are the same as in Example 1. After one-stage distillation treatment, the OCT reboiler was obtained, and the content was analyzed by GC. The harmful impurities EH 20ppm, BP 18ppm, PCN<10ppm, ETO 50ppm, Amide<10ppm, ECDP 1950ppm, and the OCT content was 99.43%;

[0124] two-stage thin film distillation

[0125] The above-mentioned first-stage distillation product was distilled again, and the parameters were set t...

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Abstract

The invention discloses a preparation method of an octocrilene sun-screening agent. The preparation method is characterized by comprising the following steps: step (1) raw material etocrilene is recrystallized; step (2) the recrystallized etocrilene is dissolved in isooctyl alcohol, a catalyst is added, an ester exchange reaction is conducted in segments, and coarse octocrilene is obtained; and step (3), the coarse octocrilene is subjected to fractional distillation and purification, and the octocrilene sun-screening agent is obtained. The prepared octocrilene has less impurities, the color islight, the quality is high, the cosmetic-grade requirement is met, and market competitiveness is high; and meanwhile, the preparation method provided by the invention is simple, convenient, easy to control and capable of meeting industrial production.

Description

technical field [0001] The invention relates to a method for preparing an organic intermediate, in particular to a method for preparing a high-quality sunscreen agent octocrylene, which belongs to the technical field of daily chemicals. Background technique [0002] Octocrylene (OCT), the chemical name is 2-cyano-3,3-diphenylacrylate-2-ethylhexyl ester, the trade name is UV-3039 or N-539, and the CAS number is 6197-30- 4. The English name of Octocrilene is Octocrilene, and its structural formula is as follows: [0003] [0004] Octocrylene is a broad-spectrum ultraviolet absorber in the form of a light yellow liquid with a maximum absorption wavelength of 308nm for ultraviolet rays. It has good compatibility with resins and is not colored. It is widely used as a light stabilizer in plastics such as soft or rigid polyvinyl chloride, nitrocellulose, acrylic resins, and polyurethanes; it has little irritation to the skin. , can be added to cosmetics as a sunscreen (sunscr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C253/34
CPCC07C253/30C07C253/34C07C255/41
Inventor 刘启发王荣杨健王中孝吴军李娟
Owner ANHUI SHENGNUOBEI CHEM TECH
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