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Method for purifying terephthalylidene dicamphor sulfonic acid

A technology of terephthalimethylene dicamphorsulfonic acid and terephthalene dicamphor sulfonic acid is applied in the field of purification methods related to terephthalimethylene dicamphor sulfonic acid, and can solve the problem of lowering the content, Inability to remove anionic substances such as chlorine

Active Publication Date: 2021-03-26
SHIN SUNG MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0019] However, in the case of acid precipitation, the reason for the low content is that anionic substances such as chlorine cannot be removed, and the content becomes low through salt precipitation like metal components. There are limitations in the complete removal of organic impurities, anionic substances, metals, etc. by the said existing synthesis techniques and purification methods

Method used

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  • Method for purifying terephthalylidene dicamphor sulfonic acid
  • Method for purifying terephthalylidene dicamphor sulfonic acid

Examples

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Effect test

Embodiment 1

[0071] Step 1: Synthesis of Terexylylene Dicamphorsulfonic Acid

[0072] After dispersing 223 g of sodium methoxide and 464.8 g of 10-d,l-camphorsulfonic acid in 4 liters of toluene and 0.2 liter of methanol, 134.2 g of terephthalaldehyde was added and reacted in a nitrogen atmosphere. Hydrochloric acid and water were added and heated, and after refluxing, toluene was removed and cooled. This was filtered and dried to obtain 428.0 g of terexylylenebiscamphorsulfonic acid. This is the substance before purification obtained by acid neutralization after synthesis.

[0073] Step 2: the purification of terexylylene biscamphorsulfonic acid

[0074] After dissolving 100 g of terexylylenebiscamphorsulfonic acid obtained in step 1 in 2,000 ml of purified water, it was slowly passed through activated 1,300 ml of Samyang Corporation UPRC320 cation exchange resin for 1 hour After mixing and filling the column with 200ml of Samyang Corporation UPRA320 anion exchange resin, the aqueous s...

Embodiment 2

[0076] After putting 100 g of terephthalylidene biscamphorsulfonic acid obtained in Step 1 of said Example 1 into 2,000 ml of purified water, it was slowly passed through 1,125 ml of activated Samyang Co. After the column was mixed and filled with UPRC320 cation exchange resin and 375ml Samyang Corporation UPRA320 anion exchange resin, the accumulated aqueous solution of terexylylenebiscamphorsulfonic acid was removed under high vacuum by washing with 1,000ml of purified water. After concentrating with water, 300 ml of acetone was added to precipitate, and after filtration, it was dried to obtain 80 g of the target substance.

Embodiment 3

[0078] After dissolving 100 g of terephthalylidene biscamphorsulfonic acid obtained in Step 1 of said Example 1 in 2,000 ml of purified water, it was slowly passed through 1,425 ml of activated Samyang Co. UPRC320 cation exchange resin and 75ml of Samyang Corporation UPRA320 anion exchange resin were mixed and packed, after that, the accumulated aqueous solution of terephthalylidene dicamphorsulfonic acid was removed under high vacuum by washing with 1,000ml of purified water After concentration with purified water, 300 ml of acetone was added to precipitate, filtered, and then dried to obtain 88.3 g of the target product.

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Abstract

The present invention relates to a method for purifying terephthalylidene dicamphor sulfonic acid. In the purification method of the present invention, an anionic material and a cationic material produced in the synthesis and precipitation of terephthalylidene dicamphor sulfonic acid are purified by separation using an anion exchange resin and a cation exchange resin in mixture while the mixing ratio is optimized, followed by concentration, so that through the enhancement of absorbance at the inherent absorption wavelength of terephthalylidene dicamphor sulfonic acid, terephthalylidene dicamphor sulfonic acid securing irritation of the skin and stability to the skin can be easily purified and obtained.

Description

technical field [0001] The present invention relates to a method for purifying terexylylene biscamphorsulfonic acid, and more particularly to an anionic substance and a cationic substance that will be generated during the synthesis and precipitation of terexylylene biscamphorsulfonic acid By using a mixture of cation exchange resin and anion exchange resin, and optimizing the mixing ratio, separating, purifying, and concentrating, in the absorption wavelength inherent to terexylylenebiscamphorsulfonic acid, the positive effect confirmed by improving the absorbance A method for purifying xylylene dicamphorsulfonic acid. Background technique [0002] Due to the destruction of the ozone layer due to climate change, ultraviolet rays directly contact human skin, which induces skin spots and skin aging. Therefore, sunscreen is indispensable in cosmetics, and sunscreen is widely used in cosmetics. . [0003] In particular, wavelengths of 280 to 320 nm known as UVA B cause erythem...

Claims

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Application Information

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IPC IPC(8): C07C303/44C07C309/24
CPCC07C303/44C07C309/24
Inventor 申相圭金廣植
Owner SHIN SUNG MATERIALS
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