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High-efficiency purifying method for sodium pyrithione

A technology of sodium pyrithione and purification method, applied in the field of fine chemical industry, can solve the problems of material loss, slow oxidation, inclusion of sodium chloride, etc., and achieve the effects of improving quality, simple operation and avoiding oxidation

Inactive Publication Date: 2018-01-19
CHONGQING ZHONGBANG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] But the above-mentioned purification process has the following defects: 1. in the acid analysis process, solids are separated out in the aqueous solution, and the materials are not easy to separate in industrial production, and the solids are mixed with sodium chloride, which requires a large amount of purified water to wash; 2.2-mercapto Pyridine-N-oxide itself is unstable and will be oxidized slowly in the air. When encountering high temperature, oxygen will quickly convert into sulfonic acid groups; 3. During the purification process, the transfer and oxidation of materials will cause material loss of more than 10%

Method used

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  • High-efficiency purifying method for sodium pyrithione

Examples

Experimental program
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Embodiment 1

[0025] In a 500ml four-neck flask, add 100g of crude sodium pyrithione aqueous solution (content 22%, Ghana chroma 10), 100g of ethyl acetate, control the temperature at 5-10°C, add 18g of 30% hydrochloric acid dropwise, and dropwise complete , measured pH=2, continued to stir for 30 minutes, separated liquids, added 100 g of a mass fraction of 6% sodium hydroxide solution to the organic phase, stirred for 30 minutes, measured pH=9.5, separated liquids, collected the water phase, and quantified pyridine in the liquid phase The quality of sodium thioketone is 21.6g, the isolated yield is 98%, and the chromaticity of Ghana is 1.

Embodiment 2

[0027] In a 500ml four-necked flask, add 100g of the crude product of sodium pyrithione aqueous solution (content 22%, Garner chromaticity 10), control the temperature at 5-10°C, add 18g of 30% hydrochloric acid dropwise, after the dropwise addition, the pH= 2. A large amount of white solid precipitated, then add 100g of ethyl acetate and stir for 30min, separate the liquid, add 100g of 6% sodium hydroxide solution to the organic phase, stir for 30min, the measured pH = 10, separate the liquid, collect The quality of the aqueous phase and liquid phase quantitative pyrithione sodium was 21.1 g, the separation yield was 96%, and the chromaticity was 1 in Ghana.

Embodiment 3

[0029] In a 500ml four-neck flask, add 100g of crude sodium pyrithione aqueous solution (content 22%, Garner chromaticity 10), 100g of chloroform, control the temperature at 5-10°C, add 21.6g of 25% hydrochloric acid dropwise, and dropwise, Measured pH = 2, continue to stir for 30 minutes, separate liquids, add 100 g of 6% sodium hydroxide solution to the organic phase, stir for 30 minutes, measure pH = 9.7, separate liquids, collect the water phase, quantify pyridinesulfur in the liquid phase The quality of sodium ketone is 21g, the isolated yield is 95.5%, and the chromaticity of Ghana is 1.

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Abstract

The invention discloses a high-efficiency purifying method for sodium pyrithione. The method comprises the following steps: adjusting the pH value of a raw material which is an aqueous solution of crude sodium pyrithione to 1-4 at a low temperature -5-25 DEG C by adopting a non-oxidizing acid to convert the sodium pyrithione into 2-mercaptopyridine-N-oxide; and completely dissolving the above precipitated solid in an organic solvent, carrying out liquid separation, allowing the obtained organic phase to be in full contact with an alkali liquid at a low temperature of -5-25 DEG C to convert the2-mercaptopyridine-N-oxide into the sodium pyrithione which enter a water phase, carrying out liquid separation, and collecting the water phase to obtain the purified aqueous solution of purified sodium pyrithione. The 2-mercaptopyridine-N-oxide precipitated from the sodium pyrithione through the acid by using the organic acid is rapidly transferred into the organic phase, the liquid separation is carried out, the 2-mercaptopyridine-N-oxide is dissolved by the alkali and enters the water phase, and the liquid separation is carried out to obtain the aqueous solution of purified sodium pyrithione, so the conversion rate approaches 100%, and the separation yield is more than 95%.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, in particular to a high-efficiency purification method of sodium pyrithione. Background technique [0002] Sodium pyrithione is widely used in related fields due to its excellent performance of high efficiency, broad spectrum and low toxicity. It is mainly used in daily chemicals (shampoo and hair care products), architectural coatings, adhesives, sealants, pesticides, textiles, Antifungal and antibacterial for products in the fields of leather products, metal processing fluids, etc. It can also be used to prepare disinfectants, detergents, and medical broad-spectrum antifungal dermatology drugs. It is also an effective fungicide for fruit trees, peanuts, wheat, vegetables and other crops And excellent silkworm disinfectant. [0003] Simultaneously, sodium pyrithione (SPT) is the important raw material of synthetic shampoo anti-dandruff zinc pyrithione (ZPT), and 2-chloropyridine-N-oxide re...

Claims

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Application Information

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IPC IPC(8): C07D213/89
Inventor 丁永山桂清王平钱勇韩小军薛谊
Owner CHONGQING ZHONGBANG TECH CO LTD
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