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Novel synthetic method of sodium pyrithione

A technology of sodium pyridinethione and a synthesis method, applied in the field of synthesis of sodium pyridinethione, can solve the problems of low 2-chloropyridine reaction yield, low atom economy, large energy consumption for solvent recovery, and the like, and achieves economical efficiency. The effect of removing decolorization work, reducing synthesis cost, and high industrialization value

Inactive Publication Date: 2019-04-19
CHONGQING ZHONGBANG TECH CO LTD
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Problems solved by technology

The raw material 2-chloropyridine of this process is obtained by chlorination of pyridine. U.S. Patent US3297556 and US5536376 disclose the method for preparing 2-chloropyridine by chlorination of pyridine, and the reaction generates by-product 2,6-dichloropyridine, resulting in the reaction of The yield is not high, and strong corrosive hydrogen chloride gas is generated at the same time, and the synthesis cost is high
Acetic acid is used as a solvent in the synthesis of 2-chloropyridine nitrogen oxide, which will seriously corrode the equipment
Chinese patent application CN201710007160.2 discloses that 2-chloropyridine is used as a raw material, water is used as a solvent, and a catalyst is used to catalyze to obtain a 2-chloropyridine nitrogen oxide solution, which is then reacted with sodium sulfide or sodium hydroxide and sodium hydrosulfide to obtain pyridine Sodium thioketone will not only produce sodium chloride as a by-product, but the atom economy of the reaction is not high, and after the reaction, the color of the reaction solution is dark, and tedious decolorization work is required
[0004] At present, there are few reports on the synthesis of sodium pyrithione using pyridine nitrogen oxides as raw materials. The representative one is the use of pyridine nitrogen oxides, vulcanizing agents and alkali reagents in organic solvents by Aoqi Chemical Co., Ltd. (US2013261309 A1) Sodium pyrithione is synthesized by medium and high temperature reaction, but the organic solvents 1,3-diisopropylbenzene (130,000 / ton) and diethylbenzene (23,000 / ton) are expensive and have high boiling point, which makes the synthesis cost high and the solvent Recycling consumes a lot of energy, which limits its industrialization

Method used

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  • Novel synthetic method of sodium pyrithione

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Experimental program
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Effect test

Embodiment 1

[0039] Add 23.85g of pyridine (0.30mol) and 1.43g of phosphomolybdic acid into a 250ml four-necked flask, add 20.00ml of water, install a spherical condenser and mechanical stirring, insert an internal temperature thermometer, then slowly raise the temperature to 80°C, dropwise Add 68.00g (0.60mol) of 30% hydrogen peroxide, and control the temperature at 80°C during the dropping process. After the dropwise addition, continue the reaction at 80°C, monitor the reaction by HPLC, stop the reaction when the raw material pyridine no longer decreases; the reaction solution Cool to room temperature, filter under reduced pressure, recover the catalyst, and distill the filtrate to remove water under reduced pressure to obtain 25.53 g of pyridine nitrogen oxide with a content of 95% (water content is 5%) and a yield of 85%.

[0040]Add 10.01g of pyridine nitrogen oxide (0.10mol), 110.57g of toluene (1.20mol) into a 250ml autoclave, then add 1.50g of sodium dodecylsulfonate, 37.74g (62%, 0...

Embodiment 2

[0042] Add 23.85g of pyridine (0.30mol) and 1.43g of phosphotungstic acid into a 250ml four-neck flask, add 20.00ml of water, install a spherical condenser and mechanical stirring, insert an internal temperature thermometer, then slowly raise the temperature to 80°C, dropwise Add 68.00g (0.60mol) of 30% hydrogen peroxide, and control the reaction temperature at 80°C during the dropwise addition process. After the dropwise addition, continue the reaction at 80°C, monitor the reaction by HPLC, and stop the reaction when the raw material pyridine no longer decreases. The solution was cooled to room temperature, filtered under reduced pressure, and the catalyst was recovered, and the filtrate was distilled off under reduced pressure to obtain 26.75 g of pyridine nitrogen oxide with a content of 96% (water content was 4%) and a yield of 90%.

[0043] Add 9.91g of pyridine nitrogen oxide (0.10mol), 110.57g of toluene (1.20mol) into a 250ml autoclave, then add 1.50g of sodium dodecyls...

Embodiment 3

[0045] Add 23.85g of pyridine (0.30mol) and 1.43g of phosphotungstic acid into a 250ml four-neck flask, add 20.00ml of water, install a spherical condenser and mechanical stirring, insert an internal temperature thermometer, then slowly raise the temperature to 80°C, dropwise Add 61.20g (0.54mol) of 30% hydrogen peroxide, and control the reaction temperature at 80°C during the dropwise addition process. After the dropwise addition, continue the reaction at 80°C, monitor the reaction by HPLC, and stop the reaction when the raw material pyridine no longer decreases. The solution was cooled to room temperature, filtered under reduced pressure, the catalyst was recovered, and the filtrate was distilled off under reduced pressure to obtain 27.34 g of pyridine nitrogen oxide with a content of 96% (water content was 4%) and a yield of 92%.

[0046] 9.91g pyridine nitrogen oxide (0.10mol), 106.18g p-xylene (1.00mol) are added in the 250ml autoclave, then add 1.50g sodium dodecyl diphen...

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Abstract

The invention discloses a novel synthetic method of sodium pyrithione. The method includes the following steps: synthesizing a pyridine n-oxide by using pyridine as a raw material, water as a solventand hydrogen peroxide as an oxidant in the presence of catalysts; and mixing the pyridine n-oxide with organic solvents, adding surfactants, vulcanizing agents and alkali reagents, refluxing water, and raising the temperature and pressurizing for reaction after water in the reaction system is separated to synthesize the sodium pyrithione. The novel synthetic method of sodium pyrithione uses the cheap pyridine as the raw material, has the advantages of easily available raw material, simply synthesis route, high total reaction yield, less ''three wastes'' generated by the reaction and low synthesis cost, and has extremely high industrial value.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a new method for synthesizing sodium pyrithione. Background technique [0002] The chemical name of sodium pyrithione (SPT) is 2-mercaptopyridine-1-oxide sodium salt, and its pure product is white or off-white powder. Zinc pyrithione has a wide range of applications. Sodium pyrithione aqueous solution can be used as an antiseptic and antifungal agent for daily chemical products, which can prevent product spoilage and mildew, and can relieve itching and dandruff; it can be used in architectural coatings, adhesives, sealants, pesticides, textiles, leather Products, pulp, ink, metal processing fluid, water treatment, oil field water injection system and other fields have anti-mildew and anti-bacterial effects. Sodium pyrithione can also be used as a prepared disinfectant and dermatological medical antifungal, and can also be used as a fungicide for fruit trees, peanuts, w...

Claims

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Application Information

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IPC IPC(8): C07D213/89
CPCC07D213/89
Inventor 袁意钱勇王平韩小军王金山
Owner CHONGQING ZHONGBANG TECH CO LTD
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