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Preparation method of mannitol salicylate as cosmetic preservative

A technology of salicylate and mannitol, which is applied in the field of organic synthesis to achieve the effects of excellent anti-corrosion performance and emulsifying performance, preventing ultraviolet radiation and high maintenance costs

Pending Publication Date: 2022-03-18
FUSHUN DONGKE FINE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is a cosmetic additive product with potential market influence, and there are few reports of such products in China at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] ① Preparation of anhydrous mannitol: Add 500 g of solid mannitol and 8 g of sodium hypophosphite monohydrate into a 2L glass reactor, seal the reactor and turn on high-purity nitrogen to replace the oxygen in the reactor three times. Then raise the temperature to 175°C, add 2.6g of phosphoric acid after the mannitol is melted, turn on the vacuum pump to keep the vacuum in the reactor at -0.04~-0.06MPa, and stir for 0.5h. After that, raise the temperature to 190-210°C, dehydrate mannitol under reduced pressure at this temperature, keep the vacuum degree at -0.095--0.1MPa, and the reaction time is 4h, so that the hydroxyl value inner ethers of the 1 and 4 positions of mannitol The amount of dehydration is 54.4g, and the dehydrated mannitol is obtained.

[0026] ②Purification of dehydrated mannitol: reduce the temperature in the kettle to 180°C, add 3g of ZnO to purify the dehydrated mannitol, raise the reaction temperature to 185-195°C, keep stirring at this temperature f...

Embodiment 2

[0031] ① Preparation of anhydrous mannitol: Add 350 g of solid mannitol and 6.8 g of sodium hypophosphite monohydrate into a 2L glass reactor, seal the reactor and turn on high-purity nitrogen to replace the oxygen in the reactor three times. Then raise the temperature to 170°C, add 2g of phosphoric acid after the mannitol is melted, turn on the vacuum pump to keep the vacuum in the reactor, the vacuum degree is kept at -0.04~-0.06MPa, and stir for 0.5h. After that, raise the temperature to 190-210°C, dehydrate mannitol under reduced pressure at this temperature, keep the vacuum degree at -0.095--0.1MPa, and the reaction time is 3h, so that the hydroxyl value inner ethers of the 1 and 4 positions of mannitol The amount of dehydration is 37g, and the dehydrated mannitol is obtained.

[0032] ②Purification of anhydrous mannitol: lower the temperature in the kettle to 180°C, add 5.3g Al 2 o 3 Purify the anhydrous mannitol, raise the reaction temperature to 185-195°C, keep the t...

Embodiment 3

[0037] ① Preparation of anhydrous mannitol: Add 760 g of solid mannitol and 12.2 g of sodium hypophosphite monohydrate into a 2L glass reactor, seal the reactor and turn on high-purity nitrogen to replace the oxygen in the reactor three times. Then the temperature was raised to 170°C, after the mannitol was melted, 3 g of phosphoric acid was added, the vacuum pump was turned on to keep the reactor in a vacuum state, the vacuum degree was kept at -0.04-0.06 MPa, and the reaction was stirred for 1 h. Afterwards, raise the temperature to 190-210°C, dehydrate mannitol under reduced pressure at this temperature, keep the vacuum degree at -0.095--0.1MPa, and the reaction time is 2.5h, so that the hydroxyl values ​​of the 1 and 4 positions of mannitol are within Etherification, the amount of dehydration is 82g, and anhydrous mannitol is obtained.

[0038] ②Purification of dehydrated mannitol: reduce the temperature in the kettle to 180°C, add 10g of ZnO to purify the dehydrated manni...

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Abstract

The invention discloses a preparation method of mannitol salicylate as a cosmetic preservative. The preparation method comprises the following steps: (1) preparing mannitol; (2) purifying the dehydrated mannitol; (3) preparing a crude sample of the dehydrated mannitol salicylate; (4) preparing the dehydrated mannitol salicylate; and (5) recrystallization deacidification treatment. Compared with the prior art, the preparation method has the following advantages: 1, the dehydrated mannitol salicylate prepared by the method has aromatic smell, and has excellent corrosion resistance and emulsifying property when being used in cosmetics; and 2, a plurality of technological processes such as internal etherification, purification, esterification, refining and recrystallization are adopted in the preparation process of the method, so that the product quality and the application in cosmetics are ensured. 3, mannitol and salicylic acid are mainly used as raw materials in the method. Mannitol can be independently used in medicines and is edible; salicylic acid has the effects of preventing corrosion, sterilizing, relieving itching and diminishing inflammation, so that a small amount of residual raw materials in the final product cannot irritate the skin.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to a preparation method of anhydromannitol salicylate, a cosmetic preservative. Background technique [0002] Nowadays, the rapid development of the cosmetics industry has made consumers' requirements for green products continue to rise, and higher requirements have been put forward for the application of cosmetic additives (preservatives, emulsifiers, etc.), so that many traditional preservatives are listed. banned list. At present, the preservative market has formed a more natural, greener, and milder development trend. In order to meet the needs of the market, more and more preservative products that meet regulatory requirements, have no irritation to consumers’ skin, and do not contain harmful ingredients have been developed. Come out, and have been well promoted and applied in the market. [0003] As a product obtained from kelp concentration, crystallization or isome...

Claims

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Application Information

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IPC IPC(8): C07D307/20
CPCC07D307/20
Inventor 徐仕睿张迅刘勇刘威左小青
Owner FUSHUN DONGKE FINE CHEM
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