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Synthesis method of high-content bispyrithione

A bipyridinethione and synthesis method technology, applied in the field of bispyridinethione preparation, can solve the problems of low yield and content, inability to meet the needs of daily chemical products, etc.

Active Publication Date: 2022-02-01
CHONGQING ZHONGBANG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention intends to provide a method for synthesizing high-content bispyridinethione to solve the problem that the traditional method for synthesizing bispyridinethione has low product yield and content and cannot meet the needs of daily chemical products

Method used

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  • Synthesis method of high-content bispyrithione

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preparation example Construction

[0022] Scheme overview: a kind of synthetic method of high-content dipyridinethione, comprises the following steps:

[0023] Step I: Nitrogen oxidation reaction, add solvent, catalyst and 2-chloropyridine to the reactor and stir evenly, the molar ratio of 2-chloropyridine and catalyst is 1:1~2, the mass ratio of 2-chloropyridine to solvent is 1: 0.5-1; the solvent in this embodiment is distilled water, and the catalyst is a titanium-silicon molecular sieve catalyst (IEZ-Ti-MWW catalyst); then hydrogen peroxide is added dropwise at 40-100°C, and after the dropwise addition is completed, the insulation reaction is carried out for 2-5h. After the reaction was completed, the filtrate was obtained by suction filtration under reduced temperature, and the 2-chloropyridine nitrogen oxide solution was obtained.

[0024] Step II: mercaptolation reaction, add sodium hydrosulfide solution and sodium hydroxide solution to the reaction kettle, the concentration of sodium hydrosulfide is 35-...

Embodiment 1

[0030] A kind of synthetic method of high-content dipyridinethione, comprises the steps:

[0031] Step I: Nitrogen oxidation reaction, add 100g of 2-chloropyridine, 75g of distilled water and 2g of IEZ-Ti-MWW catalyst respectively in a 500L four-necked flask, start stirring and raise the temperature to 40°C, then add 97g of hydrogen peroxide with a mass fraction of 35% dropwise, and control the temperature Between 60-80°C. After the dropwise addition, keep warm for 4 hours, cool down to 40°C after the warm keeping, filter to get 2-chloropyridine nitrogen oxide, and the filter cake is used for recovery of the catalyst for later use;

[0032] Step II: mercaptolation reaction, add 117g of 45% sodium hydrosulfide solution and 107g of 32% sodium hydroxide solution in a 1000L four-neck flask, start stirring and heat up to 60°C, start adding the above obtained filtrate 2-chloropyridine nitrogen oxidation Control the reaction temperature at 60-70°C, keep the reaction for 3 hours afte...

Embodiment 2

[0037]The difference between this embodiment and Example 1 is that the molar ratio of hypochlorous acid to urea is 1.4:1.0: in this embodiment, step III: the oxidizing agent is hypochlorous acid-urea solution, and its preparation process is as follows: weigh 350g 13% sodium hypochlorite solution, pass through carbon dioxide gas to saturation, set aside. Add 26.5 g of 99% urea to the above solution and stir evenly to obtain hypochlorous acid-urea solution.

[0038] In the bipyridinethione synthesis step, weigh 100g of 2-mercaptopyridine-N-oxide and 300g of pure water in a 1000ml four-neck flask to disperse them, add 1.4g of sodium dodecylbenzenesulfonate, stir to dissolve, and heat up To 45°C, add hypochlorous acid-urea solution dropwise, after the dropwise addition, raise the temperature to 55-60°C for 1 hour, filter with suction, wash, refine with ethanol, and dry under reduced pressure at 55°C to obtain off-white solid bispyridinethione 90.3g, content 98.9%, yield 91.8%.

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Abstract

The invention relates to the field of preparation of bispyrithione, and discloses a synthesis method of high-content bispyrithione. The synthesis method comprises the following steps: dropwise adding an oxidant into a mixed system of 2-mercaptopyridine-N-oxide and an anionic surfactant, carrying out heating, keeping a temperature and successively carrying out suction filtration, washing, refining and drying to obtain solid bispyrithione, wherein the oxidant is a hypochlorous acid-urea solution. The content of the prepared bispyrithione is 98.0% or above, yield is increased to 90% or above, the quality requirements of daily chemical products can be met, a process is simple, and industrial application and popularization are easy.

Description

technical field [0001] The invention relates to the field of bispyridinethione preparation, in particular to a method for synthesizing high-content bispyridinethione. Background technique [0002] Bipyridinethione has high-efficiency and broad-spectrum antibacterial and antifungal effects. It is an excellent anti-dandruff and antipruritic agent with broad-spectrum antibacterial properties. It is widely used in transparent plastics, pharmaceutical intermediates and other fields. Due to its unique molecular structure, bispyridinethione greatly reduces its sensitivity to metal ions compared to the traditional anti-dandruff agent-zinc pyrithione (ZPT), and can exist more stably in the shampoo system. [0003] There are very few research reports on the synthesis methods of bispyridinethione at home and abroad. At present, the synthesis of bispyridinethione is based on 2-mercaptopyridine nitrogen oxide as the starting material. pyrithione. However, it has been verified by practi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/89
CPCC07D213/89
Inventor 何小强龚传秀向龙周学平邬美彦
Owner CHONGQING ZHONGBANG TECH CO LTD
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