CN113999171B - Synthesis method of high-content bipyridine thione - Google Patents
Synthesis method of high-content bipyridine thione Download PDFInfo
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/89—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members with hetero atoms directly attached to the ring nitrogen atom
Abstract
The invention relates to the field of preparation of bipyridine thione, and discloses a synthesis method of high-content bipyridine thione, wherein an oxidant is dropwise added into a mixed system of 2-mercaptopyridine-N-oxide and anionic surfactant, the temperature is raised, and after heat preservation, the solid bipyridine thione is obtained through suction filtration, washing, refining and drying, wherein the oxidant is hypochlorous acid-urea solution. The content of bipyridine thione prepared by the method is more than 98.0%, the yield is improved to more than 90%, the quality requirements of daily chemical products can be met, the process is simple, and the industrial popularization and application are easy.
Description
Technical Field
The invention relates to the field of preparation of bipyridyl thioketone, in particular to a method for synthesizing high-content bipyridyl thioketone.
Background
The bipyridyl thioketone has high-efficiency broad-spectrum antibacterial and antifungal effects, is an excellent anti-dandruff and antipruritic agent, has broad-spectrum antibacterial performance, and is widely applied to the fields of transparent plastics, medical intermediates and the like. Because of the unique molecular structure, compared with the traditional antidandruff agent Zinc Pyrithione (ZPT), the sensitivity of the bipyridyl thioketone to metal ions is greatly reduced, and the bipyridyl thioketone can be more stably existing in a shampoo system.
The research reports on the synthesis method of the bipyridine thione at home and abroad are few, and the current traditional technology for synthesizing the bipyridine thione takes 2-mercaptopyridine nitrogen oxide as a starting material, and the bipyridine thione is prepared by oxidizing a hydrogen peroxide urea system under the weak acidic condition. However, practice proves that when the hydrogen peroxide urea system is used as an oxidant to synthesize the dipyridyl thioketone, more byproducts are generated, so that the yield and the product content of the product are low, the yield is only about 78%, and the dipyridyl thioketone content is about 96%. The daily chemical product requires that the content of the bipyridyl thioketone is more than 98%, and the quality of the bipyridyl thioketone prepared by the traditional method cannot meet the requirement.
Disclosure of Invention
The invention aims to provide a synthesis method of high-content dipyridyl thioketone, which aims to solve the problems that the product yield and content of the traditional method for synthesizing dipyridyl thioketone are low and the requirements of daily chemicals cannot be met.
In order to achieve the above purpose, the invention adopts the following technical scheme: a process for synthesizing high-content bipyridine thioketone includes such steps as dropping oxidant in the mixture of 2-mercaptopyridine-N-oxide and anionic surfactant, heating, vacuum filtering, washing, refining and baking.
The principle and the advantages of the scheme are as follows: in practical application, in the technical scheme, the anionic surfactant and the oxidant are added into the 2-mercaptopyridine-N-oxide solution, and the oxidant is optimized, so that the problem that the raw material residue is high and the reaction time is long due to incomplete reaction is solved because the conventional hydrogen peroxide urea strong oxidant system is used as the oxidant and more byproducts are generated in the process of optimizing the oxidant. During the research, the unexpected discovery that when hypochlorous acid-urea solution is used as the bipyridyl thioketone synthetic oxidant, not only can enough oxidability be ensured to ensure complete reaction, but also the problem that more byproducts are generated when the traditional hydrogen peroxide urea solution is used as the oxidant can be avoided, and the yield and purity of the finished product can be improved; meanwhile, the scheme uses the anionic surfactant which can promote the reaction and cooperate with the urea hypochlorous acid system to ensure high enough oxidability and avoid raw material residue; and can avoid generating too many byproducts. Through practical verification, the content of the bipyridyl thioketone prepared by the technical scheme is more than 98.0%, the yield is improved to more than 90%, the quality requirement of daily chemical products can be met, the process is simple, and the industrial popularization and application are easy.
Preferably, as a modification, the anionic surfactant is sodium dodecylbenzenesulfonate.
In the technical scheme, the sodium dodecyl benzene sulfonate is a common anionic surfactant, is a commercial finished product, has wide sources, is easy to obtain and mature in application technology, and has better effect compared with other anionic surfactants such as stearic acid when being used as the anionic surfactant through experimental verification.
Preferably, as an improvement, the hypochlorous acid-urea solution is prepared by introducing carbon dioxide gas into 10-15% sodium hypochlorite solution to saturate, adding 99% urea, and stirring uniformly.
According to the technical scheme, after the hypochlorous acid-urea oxidation system is developed, the preparation method of the oxidant is developed in a targeted design, and the oxidant system prepared by the preparation method is stable in property and can meet the reaction requirement.
Preferably, as a modification, the molar ratio of hypochlorous acid to urea in the hypochlorous acid-urea solution is 1.2-1.4:1.0.
In the technical scheme, the hypochlorous acid-urea oxidant system has important influence on the reaction, byproducts are generated when the addition amount of the oxidant is too high, the purity and the yield of the product are influenced, incomplete reaction is caused when the addition amount of the oxidant is too low, raw material residues are caused, the yield and the purity of the product are also reduced, and the addition ratio is a better addition ratio.
Preferably, as an improvement, the preparation method of the 2-mercaptopyridine-N-oxide comprises the steps of adjusting the pH value of SPT to 1-3 by using concentrated hydrochloric acid, and obtaining a filter cake after suction filtration, wherein the filter cake is the 2-mercaptopyridine-N-oxide and is directly used for synthesizing bipyridyl thione.
According to the technical scheme, the pH value of the SPT (2-pyrithione sodium salt) solution can be adjusted to 1-3 by using concentrated hydrochloric acid through the method, a filter cake obtained after suction filtration is the 2-pyrithione-N-oxide, the method can be directly used for synthesizing bipyridyl thioketone, the subsequent reaction requirement is met, and the preparation process is simple and is suitable for industrial popularization and application.
Preferably, as a modification, the mixed system of the 2-mercaptopyridine-N-oxide solution and the anionic surfactant is heated to 45 ℃ before the oxidant is added dropwise.
In the technical scheme, before the oxidant is dripped, the 2-mercaptopyridine-N-oxide solution and the anionic surfactant are heated, and at the temperature, the oxidant can react with substances after being dripped, so that the reaction speed is increased.
Preferably, as an improvement, the temperature of the mixture is raised to 55-60 ℃ after the oxidant is added dropwise, and the heat preservation time is 1-3h.
In the technical scheme, the temperature of heating is optimized, the oxidant is decomposed due to the fact that the temperature of heating is too high, the reaction is not facilitated due to the fact that the temperature is too low, and the temperature range and the heat preservation time are suitable interval ranges.
Preferably, as an improvement, the drying mode is reduced pressure drying, the drying temperature is 55 ℃, and the water content of the dried solid bipyridyl thioketone is less than 0.5%.
In the technical scheme, ethanol refining is adopted, so that the later-stage lower temperature can meet the drying requirement, and the operation is simple and has no residue.
Detailed Description
The following is a detailed description of embodiments, but embodiments of the invention are not limited thereto. The technical means used in the following embodiments are conventional means well known to those skilled in the art unless otherwise specified; the experimental methods used are all conventional methods; the materials, reagents, and the like used are all commercially available.
The scheme is as follows: a synthesis method of high-content bipyridyl thioketone comprises the following steps:
step I: adding a solvent, a catalyst and 2-chloropyridine into a reactor for uniform stirring, wherein the molar ratio of the 2-chloropyridine to the catalyst is 1:1-2, and the mass ratio of the 2-chloropyridine to the solvent is 1:0.5-1; the solvent in the embodiment is distilled water, and the catalyst is titanium silicalite molecular sieve catalyst (IEZ-Ti-MWW catalyst); then dropwise adding hydrogen peroxide at 40-100 ℃, after the dropwise adding is finished, carrying out heat preservation reaction for 2-5h, cooling and suction filtering after the reaction is finished to obtain filtrate, and thus obtaining the 2-chloropyridine nitrogen oxide solution.
Step II: adding a sodium hydrosulfide solution and a sodium hydroxide solution into a reaction kettle, wherein the concentration of sodium hydrosulfide is 35-45%, the concentration of sodium hydroxide is 27-32%, dropwise adding a 2-chloropyridine nitrogen oxide solution at 40-100 ℃, preserving heat for 1-3h at the temperature, cooling to 40 ℃ after the reaction is finished, adjusting the pH to 5-6, adding active carbon, decoloring and filtering for 1h to obtain a 2-mercaptopyridine oxide sodium salt Solution (SPT). The SPT is adjusted to pH=1-3 by concentrated hydrochloric acid, and then suction filtration is carried out to obtain a filter cake, wherein the filter cake is 2-mercaptopyridine-N-oxide and is directly used for synthesizing bipyridyl thioketone.
Step III: synthesis of bipyridylthioketone
(1) 25% -35% of hydrogen peroxide, 99% of urea is added, and the mixture is stirred uniformly to obtain a hydrogen peroxide-urea solution (oxidant) for standby.
(2) And (3) introducing carbon dioxide gas into a 10% -15% sodium hypochlorite solution to saturate, adding 99% urea, and uniformly stirring to obtain hypochlorous acid-urea solution for standby (oxidant).
(3) 2-mercaptopyridine-N-oxide, pure water and an anionic surfactant are added into a reactor, wherein the anionic surfactant in the embodiment is sodium dodecyl benzene sulfonate, and the addition amount of the anionic surfactant is 0.5-1% of the molar amount of the 2-chloropyridine-N-oxide. Stirring and dissolving, heating to 45 ℃, dropwise adding an oxidant (hydrogen peroxide-urea solution or hypochlorous acid-urea solution), heating to 55-60 ℃ after the dropwise adding is finished, preserving heat for 1-3 hours, carrying out suction filtration, washing, refining with ethanol, and drying under reduced pressure at 55 ℃ to obtain an off-white solid, namely bipyridyl thioketone.
Example 1
A synthesis method of high-content bipyridyl thioketone comprises the following steps:
step I: and (3) performing an oxidation reaction, namely respectively adding 100g of 2-chloropyridine, 75g of distilled water and 2g of IEZ-Ti-MWW catalyst into a 500L four-neck flask, stirring and heating to 40 ℃, and then dropwise adding 97g of 35% hydrogen peroxide by mass fraction, wherein the temperature is controlled between 60 ℃ and 80 ℃. Preserving heat for 4 hours after the dripping is finished, cooling to 40 ℃ after the heat preservation is finished, filtering to obtain 2-chloropyridine nitrogen oxide, and recovering a filter cake as a catalyst for later use;
step II: adding 117g of 45% sodium hydrosulfide solution and 107g of 32% sodium hydroxide solution into a 1000L four-neck flask, stirring and heating to 60 ℃, beginning to dropwise add the obtained filtrate of 2-chloropyridine nitrogen oxide, controlling the reaction temperature to 60-70 ℃, preserving heat for 3 hours after the dropwise addition, cooling to 40 ℃ after the heat preservation is finished, dropwise adding 30% hydrochloric acid to adjust the pH value to 5-6, adding 1g of active carbon and stirring for 1 hour, filtering to obtain filtrate of 2-mercaptopyridine oxide sodium salt Solution (SPT), adjusting the pH value of the filtrate to 1-3 by using 30% hydrochloric acid, and carrying out suction filtration to obtain 104g of filter cake, wherein the content of the filter cake is 98.0%.
Step III: synthesis of bipyridylthioketone
(1) The oxidant in this example is hypochlorous acid-urea solution, the mole ratio of hypochlorous acid to urea is 1.2:1.0, and the preparation process is as follows: 300g of 13% sodium hypochlorite solution is weighed, and carbon dioxide gas is introduced until saturation for later use. 26.5g of 99% urea is added into the solution and stirred uniformly, thus obtaining hypochlorous acid-urea solution.
(2) Weighing 100g of 2-mercaptopyridine-N-oxide and 300g of pure water, dispersing in a 1000ml four-necked flask, adding 1.4g of sodium dodecyl benzene sulfonate, stirring for dissolution, heating to 45 ℃, and dripping the prepared hypochlorous acid-urea solution; after the dripping is finished, the temperature is raised to 55-60 ℃ and kept for 1 hour, the solution is filtered, washed, refined by ethanol and dried under reduced pressure at 55 ℃ to obtain 90.8g of off-white solid bipyridyl thioketone with the content of 99.0 percent and the yield of 92.3 percent.
Example 2
This example differs from example 1 in that the molar ratio of hypochlorous acid to urea is 1.4:1.0: in this embodiment, step III: the oxidant is hypochlorous acid-urea solution, and the preparation process is as follows: 350g of 13% sodium hypochlorite solution is weighed and carbon dioxide gas is introduced until saturation for later use. 26.5g of 99% urea is added into the solution and stirred uniformly, thus obtaining hypochlorous acid-urea solution.
In the bipyridyl thioketone synthesis step, 100g of 2-mercaptopyridine-N-oxide and 300g of pure water are weighed and dispersed in a 1000ml four-necked flask, 1.4g of sodium dodecyl benzene sulfonate is added, stirring and dissolving are carried out, the temperature is raised to 45 ℃, hypochlorous acid-urea solution is dropwise added, the temperature is raised to 55-60 ℃ after the dropwise addition is completed, the temperature is kept for 1 hour, the temperature is kept at 55-60 ℃, the filtration, the washing and the ethanol refining are carried out, and the pressure is reduced and the drying is carried out at 55 ℃, thus obtaining 90.3g of white-like solid bipyridyl thioketone with the content of 98.9% and the yield of 91.8%.
Example 3
This embodiment differs from embodiment 1 in that: in this embodiment, in step III: in the bipyridyl thioketone synthesis step, the addition amount of sodium dodecyl sulfate is 2.7g, and 91.2g of white solid bipyridyl thioketone is obtained, the content is 99.3%, and the conversion rate is 93.1%.
Example 4
This embodiment differs from embodiment 2 in that: in this embodiment, in step III: in the bipyridyl thioketone synthesis step, the addition amount of sodium dodecyl sulfate is 2.7g, and 90.5g of white solid bipyridyl thioketone is obtained, the content is 99.1%, and the yield is 92.0%.
Comparative example 1
This comparative example differs from example 1 in that: in the comparative example, a hydrogen peroxide-urea solution was used as the oxidizing agent. The preparation process of the hydrogen peroxide-urea solution comprises the following steps: weighing 25g of pure water and 26.5g of urea, stirring and dissolving, weighing 50g of 30% hydrogen peroxide, adding into urea solution, and uniformly mixing to obtain the aqueous urea solution.
Preparation of bipyridyl thioketone: 100g of 2-mercaptopyridine-N-oxide and 300g of pure water are weighed and dispersed in a 1000ml four-necked flask, 1.4g of sodium dodecyl benzene sulfonate is added, stirring and dissolving are carried out, the temperature is raised to 45 ℃, hydrogen peroxide-urea solution is dropwise added, after the dropwise addition is completed, the temperature is raised to 55-60 ℃ and the temperature is kept for 1 hour, suction filtration, washing, ethanol refining and decompression drying at 55 ℃ are carried out, and 86.5g of off-white solid bipyridine thione with the content of 97.2% and the yield of 86.5% is obtained.
Comparative example 2
This comparative example differs from example 1 in that: no anionic surfactant was added in this comparative example.
100g of 2-mercaptopyridine-N-oxide and 300g of pure water are weighed and dispersed in a 1000ml four-necked flask, stirred and heated to 45 ℃, hypochlorous acid-urea solution is added dropwise, the temperature is raised to 55-60 ℃ after the completion of the dropwise addition, the temperature is kept for 1 hour, the mixture is filtered, washed, refined by ethanol, dried at 55 ℃ under reduced pressure, 86.8g of off-white solid bipyridyl thioketone is obtained, the content of which is 97.1 percent, and the yield is 87.5 percent.
Comparative example 3
This comparative example differs from example 1 in that: the oxidant in this comparative example is a hydrogen peroxide-urea solution, and no anionic surfactant is added. The preparation process of the hydrogen peroxide-urea solution comprises the following steps: weighing 25g of pure water and 26.5g of urea, stirring and dissolving, weighing 50g of 30% hydrogen peroxide, adding into urea solution, and uniformly mixing to obtain the aqueous urea solution.
Preparation of bipyridyl thioketone: 100g of 2-mercaptopyridine-N-oxide and 300g of pure water are weighed, dispersed, stirred and heated to 45 ℃ in a four-necked flask, hydrogen peroxide-urea solution is dripped, the temperature is raised to 55-60 ℃ after the dripping is finished, the temperature is kept for 1 hour, suction filtration, washing, ethanol refining and drying are carried out at 55 ℃ under reduced pressure, and 84.4g of white-like solid dipyridylthioketone with 96.5 percent of content and 83.7 percent of yield is obtained.
Comparative example 4
This comparative example differs from example 1 in that: the oxidizing agent in this comparative example was hypochlorous acid.
Preparation of bipyridyl thioketone: 100g of 2-mercaptopyridine-N-oxide and 300g of pure water are weighed, dispersed and stirred in a 1000ml four-necked flask, 28g of hypochlorous acid is added dropwise at normal temperature, the temperature is raised to 55-60 ℃ after the completion of the dropwise addition, the temperature is kept for 1 hour, the mixture is filtered, washed, refined by ethanol, and dried under reduced pressure at 55 ℃ to obtain 76.8g of white-like solid bipyridyl thioketone with the content of 95.4 percent and the yield of 75.3 percent.
Comparative example 5
This embodiment differs from embodiment 1 in that: in this embodiment, in step III: in the bipyridyl thioketone synthesis step, the addition amount of sodium dodecyl sulfate is 0.8g, and 87.3g of white solid bipyridyl thioketone is obtained, the content is 98.4%, and the yield is 88.3%.
Comparative example 6
This embodiment differs from embodiment 1 in that: in this embodiment, in step III: in the bipyridyl thioketone synthesis step, the addition amount of sodium dodecyl sulfate is 3.2g, and 90.7g of white solid bipyridyl thioketone is obtained, the content is 99.1%, and the conversion rate is 92.4%.
Comparative example 7
This example differs from example 1 in that the molar ratio of hypochlorous acid to urea is 1.0:1.0: in this embodiment, step III: the preparation process is as follows: 250g of 13% sodium hypochlorite solution is weighed and carbon dioxide gas is introduced until saturation for later use. 26.5g of 99% urea is added into the solution and stirred uniformly, thus obtaining hypochlorous acid-urea solution.
In the bipyridyl thioketone synthesis step, 100g of 2-mercaptopyridine-N-oxide and 300g of pure water are weighed and dispersed in a 1000ml four-necked flask, 1.4g of sodium dodecyl benzene sulfonate is added, stirring and dissolving are carried out, the temperature is raised to 45 ℃, hypochlorous acid-urea solution is dropwise added, the temperature is raised to 55-60 ℃ after the dropwise addition is completed, the temperature is kept for 1 hour, the temperature is kept at 55-60 ℃, the filtration, the washing and the ethanol refining are carried out, and the pressure is reduced and the drying is carried out at 55 ℃, thus obtaining 85.7g of white-like solid bipyridyl thioketone with the content of 98.3 percent and the yield of 86.6 percent.
Comparative example 8
This example differs from example 1 in that the molar ratio of hypochlorous acid to urea is 1.6:1.0. In this embodiment, step III: the preparation process is as follows: 400g of 13% sodium hypochlorite solution is weighed and carbon dioxide gas is introduced until saturation for later use. 26.5g of 99% urea is added into the solution and stirred uniformly, thus obtaining hypochlorous acid-urea solution.
In the bipyridyl thioketone synthesis step, 100g of 2-mercaptopyridine-N-oxide and 300g of pure water are weighed and dispersed in a 1000ml four-necked flask, 1.4g of sodium dodecyl benzene sulfonate is added, stirring and dissolving are carried out, the temperature is raised to 45 ℃, hypochlorous acid-urea solution is dropwise added, the temperature is raised to 55-60 ℃ after the dropwise addition is completed, the temperature is kept for 1 hour, the temperature is kept at 55-60 ℃, the filtration, the washing and the ethanol refining are carried out, and the pressure is reduced and the drying is carried out at 55 ℃, so that the white-like solid bipyridyl thioketone is obtained, wherein the content is 97.4%, and the yield is 87.7%.
The preparation methods of example 1-example 4 and comparative example 1-comparative example 8 are mainly different in the kinds and the addition amounts of the oxidizing agent and the anionic surfactant, and for comparison, the addition amounts shown in Table 1 below are summarized as the addition amounts corresponding to 100g of 2-mercaptopyridine-N-oxide.
TABLE 1
The content and yield of the white-like solid-bipyridyl thioketone prepared in each of the above examples and comparative examples were measured by quantitative liquid phase measurement, and three parallel experiments were performed for each experimental group, and the results are shown in table 2. As can be seen from the data in Table 2, the invention uses hypochlorous acid-urea solution as oxidant, and the content of bipyridyl thioketone can be improved to about 99% by optimizing the adding ratio of hypochlorous acid and urea and assisting with a proper adding amount of surfactant, the yield of bipyridyl thioketone can be improved to more than 90%, and the quality requirement of daily chemical products can be met. In the comparative example 1, the conventional hydrogen peroxide-urea solution is adopted as an oxidant, so that the content and the yield of the bipyridyl thioketone are obviously reduced; comparative example 2 and comparative example 3, without the addition of anionic surfactant, also resulted in a significant reduction in the content and yield of bipyridyl thione; comparative example 4 only uses hypochlorous acid as the oxidant, the yield of bipyridyl thione is only 75%; in addition, the addition ratio of hypochlorous acid to urea and the addition amount of the anionic surfactant also affect the content and yield of bipyridyl thione.
TABLE 2
| Mass of bipyridyl thioketone (g) | Content of bipyridylthioketone (%) | Yield of bipyridylthioketone (%) | |
| Example 1 | 90.8 | 99.0 | 92.3 |
| Example 2 | 90.3 | 98.9 | 91.8 |
| Example 3 | 91.2 | 99.3 | 93.1 |
| Example 4 | 90.5 | 99.1 | 92.2 |
| Comparative example 1 | 86.5 | 97.2 | 86.5 |
| Comparative example 2 | 86.8 | 97.1 | 87.5 |
| Comparative example 3 | 84.4 | 96.5 | 83.7 |
| Comparative example 4 | 76.8 | 95.4 | 75.3 |
| Comparative example 5 | 87.3 | 98.4 | 88.3 |
| Comparative example 6 | 90.7 | 99.1 | 92.4 |
| Comparative example 7 | 85.7 | 98.3 | 86.6 |
| Comparative example 8 | 87.6 | 97.4 | 87.7 |
The foregoing is merely exemplary of the present invention, and specific technical solutions and/or features that are well known in the art have not been described in detail herein. It should be noted that, for those skilled in the art, several variations and modifications can be made without departing from the technical solution of the present invention, and these should also be regarded as the protection scope of the present invention, which does not affect the effect of the implementation of the present invention and the practical applicability of the patent. The protection scope of the present application shall be subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.
Claims (6)
1. A synthesis method of high-content bipyridine thione is characterized by comprising the following steps: and (3) dropwise adding an oxidant into a mixed system of 2-mercaptopyridine-N-oxide and an anionic surfactant, heating, carrying out suction filtration, washing, refining and drying after heat preservation to obtain solid bipyridine thione, wherein the oxidant is hypochlorous acid-urea solution, and the hypochlorous acid-urea solution is prepared by introducing carbon dioxide gas into 10-15% sodium hypochlorite solution to saturation, adding 99% urea, and uniformly stirring to obtain hypochlorous acid-urea solution, wherein the anionic surfactant is sodium dodecyl benzene sulfonate.
2. The method for synthesizing the high-content bipyridyl thione according to claim 1, which is characterized in that: the mol ratio of hypochlorous acid to urea in the hypochlorous acid-urea solution is 1.2-1.4:1.0.
3. The method for synthesizing the high-content bipyridyl thione according to claim 1, which is characterized in that: the preparation method of the 2-mercaptopyridine-N-oxide comprises the steps of adjusting the pH value of SPT to 1-3 by using concentrated hydrochloric acid, and obtaining a filter cake after suction filtration, wherein the filter cake is the 2-mercaptopyridine-N-oxide and is directly used for synthesizing bipyridyl thione.
4. The method for synthesizing the high-content bipyridyl thione according to claim 1, which is characterized in that: the temperature of the mixed system of the 2-mercaptopyridine-N-oxide aqueous solution and the anionic surfactant is raised to 45 ℃ before the oxidant is added dropwise.
5. The method for synthesizing the high-content bipyridyl thione according to claim 1, which is characterized in that: the temperature of the mixture is raised to 55-60 ℃ after the oxidant is added dropwise, and the heat preservation time is 1-3h.
6. The method for synthesizing high-content bipyridyl thione according to claim 5, wherein the method comprises the steps of: the drying mode is reduced pressure drying, the drying temperature is 55 ℃, and the water content of the dried solid bipyridyl thioketone is less than 0.5%.
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