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Preparation method of modified and micronized 2-mercaptopyridine oxide zinc salt

A technology of pyrithione and zinc oxide, which is applied in the field of preparation of modified micro-sized 2-pyridine oxide zinc salt, can solve problems such as difficulties in the preparation method, achieve rich performance, overcome difficulties in post-processing, and have low cost Effect

Inactive Publication Date: 2010-10-20
深圳市矽尔德新材料有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing a modified micronized 2-pyrithione zinc salt, to solve the technical problem of difficult post-processing of the preparation method of 2-pyrithione zinc salt in the prior art

Method used

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  • Preparation method of modified and micronized 2-mercaptopyridine oxide zinc salt
  • Preparation method of modified and micronized 2-mercaptopyridine oxide zinc salt
  • Preparation method of modified and micronized 2-mercaptopyridine oxide zinc salt

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preparation example Construction

[0030] see figure 1 , a kind of preparation method of micronized 2-mercapto pyrithione zinc salt, comprises the following steps:

[0031] S11: Co-precipitate an aqueous solution of a water-soluble 2-mercapto pyrithione salt and an aqueous solution of a water-soluble metal salt containing at least zinc ions at a temperature of 0-99°C and a pH of 4-9 to obtain 2-mercaptopyridine Mixed precipitation of zinc salt precipitation and other insoluble precipitation;

[0032] In this step, the co-precipitation reaction is preferably carried out between pH5-8, most preferably between pH7-8. Other insoluble precipitates refer to inorganic or organic precipitates containing polyvalent metal ions whose dissolved mass in 100 g of water is less than 1 gram, more preferably less than 0.1 gram, and most preferably less than 0.01 gram. After the co-precipitation reaction, the content of the mixed precipitate in the mother liquor after the reaction is 0.01%-30%, most preferably 0.5%-10%. And t...

Embodiment 1

[0051] At room temperature of 25°C, add 10 ml of sodium bicarbonate solution containing 0.1 mol / L of 2-mercaptopyridine oxide and 0.05 mol / L of sodium bicarbonate to a 50-ml beaker, put it into a magnetic rotor coated with PTFE, and put the SH05-3 constant temperature magnetic stirrer (Shanghai Minhang Hongpu Instrument Factory) adjust the speed to the maximum. Then, 10 ml of an aqueous solution of zinc sulfate containing 0.11 mol / L (adjusted to pH 4-4.5 with sulfuric acid) was added dropwise from the top of the center of the vortex formed by the magnetic rotor within 1 minute. After the dropwise addition, the stirring was continued for 30 minutes and then stopped.

[0052] The suspension containing zinc pyrithione and insoluble inorganic zinc precipitate was filtered through filter paper. Under the intense stirring of vacuuming, the obtained filter cake was added to 150 milliliters containing 20% ​​(weight ratio) ammonium lauryl alcohol ether sulfate and ammonium lauryl alco...

Embodiment 2

[0055] At room temperature of 25°C, add 10 ml of sodium bicarbonate solution containing 0.1 mol / L of 2-mercaptopyridine oxide and 0.05 mol / L of sodium bicarbonate to a 50-ml beaker, put it into a magnetic rotor coated with PTFE, and put the SH05-3 constant temperature magnetic stirrer (Shanghai Minhang Hongpu Instrument Factory) adjust the speed to the maximum. Then, 10 ml of an aqueous solution of zinc sulfate containing 0.11 mol / L (adjusted to pH 4-4.5 with sulfuric acid) was added dropwise from the top of the center of the vortex formed by the magnetic rotor within 1 minute. After the dropwise addition, the stirring was continued for 30 minutes and then stopped.

[0056] Slowly drop 4.8 ml of 0.2mol / L dilute hydrochloric acid solution into the reaction mother liquor, and control the pH value of the solution not to be lower than 4.5 during the dropwise addition, after the dropwise addition is completed. The obtained suspension was filtered with filter paper and washed and t...

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Abstract

The invention relates to a preparation method of a modified and micronized 2-mercaptopyridine oxide zinc salt. The preparation method comprises the following steps of: firstly, carrying out a coprecipitation reaction on a water-soluble aqueous solution of 2-mercaptopyridine oxide salt and an aqueous solution at least containing zinc ion water-soluble metal salt at 0-99 DEG C in a pH range of 4-9 to obtain a mixed precipitation containing a 2-mercaptopyridine oxide zinc salt precipitation and other insoluble precipitations; and then, mixing and reacting the mixed precipitation with a surface modifier in the pH range of 4-9 to obtain modified micronized 2-mercaptopyridine oxide zinc salt, wherein the mixed precipitation can be purified as required. The invention effectively overcomes the defects of later-period treatment difficulty of a traditional preparation method of the modified and realizes the industrial production of micronized 2-mercaptopyridine oxide zinc salt. The invention also has the advantages of flexible application, enriched 2-mercaptopyridine oxide zinc salt performance, time and labor saving and low cost.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of modified micronized 2-mercaptopyridine zinc salt. Background technique [0002] Polyvalent metal salts of pyrithione are known to be effective biocides and are widely used as antifungal and antibacterial agents in paints and personal care products such as anti-dandruff shampoos. Polyvalent metal salts of pyrithione are only slightly soluble in water, and these salts include magnesium pyrithione, barium pyrithione, strontium pyrithione, 2- Copper pyrithione, zinc pyrithione, chromium pyrithione, and zirconium pyrithione. The most widely used divalent pyrithione salt is the zinc pyrithione salt. [0003] Zinc salt of pyrithione can be used as an antimicrobial agent active against Gram-positive and negative bacteria, fungi and yeasts, and is widely used in products such as coatings, plastics, rubber, fibers, shampoos or hair conditioners Preserva...

Claims

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Application Information

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IPC IPC(8): A61K8/49A61Q17/00A61Q5/02A61Q5/12
Inventor 刘刚张颖
Owner 深圳市矽尔德新材料有限责任公司
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