Production device of isothiazolinone

Abstract

The utility model discloses a production device of isothiazolinone, and relates to the technical field of isothiazolinone production, an inlet of a synthesis kettle is respectively communicated with a 2-methyl-2, 4-pentanediol tank, a carbon disulfide tank and a sodium hydroxide solution tank, an outlet of the synthesis kettle is communicated with a hydrolysis kettle, an inlet of the hydrolysis kettle is communicated with a hydrochloric acid solution tank, and an outlet of the hydrolysis kettle is communicated with a sodium hydroxide solution tank. An outlet of the hydrolysis kettle is communicated with a cyclization kettle, and an inlet of the cyclization kettle is communicated with a liquid chlorine tank; an outlet of the cyclization kettle is communicated with a distillation kettle, and a bottom outlet of the distillation kettle is communicated with a finished product tank. The method comprises the following steps: reacting 2-methyl-2, 4-pentanediol with carbon disulfide under an alkaline condition to generate dithiocarbonate, hydrolyzing with an acid to obtain an intermediate 2-methyl-2, 4-pentanedithiol, oxidizing and cyclizing with liquid chlorine at a low temperature, introducing chlorine atoms, and distilling and purifying the obtained reaction mixture to obtain an isothiazolinone product. The safety and the product yield are high, and the production cost is reduced.

Description

TECHNICAL FIELD

[0001] The utility model relates to isothiazolinone production technical field, concretely relates to a kind of isothiazolinone's production device. BACKGROUND

[0002] Isothiazolinone is a kind of compound with high efficiency, broad-spectrum bactericidal performance, is widely used in industrial circulating water, papermaking, paint and multiple fields.Several drawbacks exist in traditional isothiazolinone production device, for example, a large number of toxic and harmful organic solvents are used in the reaction process, these solvents not only pollute the environment, but also have the hidden danger of flammable and explosive;Part of production process reaction condition is harsh, resulting in low product yield, increase production cost. SUMMARY

[0003] The technical problem to be solved by the utility model is: in view of the deficiencies existing in prior art, provide a kind of isothiazolinone's production device, environment-friendly, safety and product yield are high, reduce production cost.

[0004] To solve the above technical problem, the technical scheme of the utility model is:

[0005] A kind of isothiazolinone's production device, including synthesis kettle, the inlet of the synthesis kettle is connected with 2-methyl-2,4-pentanediol tank, carbon disulfide tank and sodium hydroxide solution tank respectively by pipeline communication, the outlet of the synthesis kettle is connected with hydrolysis kettle by pipeline communication, the inlet of the hydrolysis kettle is connected with hydrochloric acid solution tank by pipeline communication, the outlet of the hydrolysis kettle is connected with cyclization kettle by pipeline communication, the inlet of the cyclization kettle is connected with liquid chlorine tank by pipeline communication;

[0006] The outlet of the cyclization kettle is connected with distillation kettle by pipeline communication, the bottom outlet of the distillation kettle is connected with finished product tank by pipeline communication.

[0007] As an improved technical scheme, the top gas phase outlet of the distillation kettle is connected with recovery tank by pipeline communication, the outlet of the recovery tank is connected to the synthesis kettle by pipeline communication.

[0008] As an improved technical scheme, the bottom outlet of the distillation kettle is connected with extraction tank by pipeline communication, the inlet of the extraction tank is connected with ethyl acetate tank by pipeline communication, the outlet of the extraction tank is connected with crystallization tank by pipeline communication, the inlet of the crystallization tank is connected with n-hexane tank by pipeline communication, the outlet of the crystallization tank is connected with suction filter tank by pipeline communication, the solid phase outlet of the suction filter tank is connected to the finished product tank.

[0009] As an improved technical scheme, the solid phase outlet of the suction filter tank is connected with dryer, and the outlet of the dryer is connected to the finished product tank.

[0010] As an improved technical solution, the inlet of the filtration tank is connected to the n-hexane tank via a pipeline.

[0011] As an improved technical solution, the liquid phase outlet of the filtration tank is connected to a distillation tank via a pipeline, and the top gas phase outlet of the distillation tank is connected to an ethyl acetate recovery tank and a n-hexane recovery tank via pipelines.

[0012] As a preferred technical solution, the outlet of the ethyl acetate recovery tank is connected to a first adsorption tank via a pipeline, and the outlet of the first adsorption tank is connected to the ethyl acetate tank via a pipeline.

[0013] As a preferred technical solution, the outlet of the n-hexane recovery tank is connected to a second adsorption tank via a pipeline, and the outlet of the second adsorption tank is connected to the n-hexane tank via a pipeline.

[0014] Due to the adoption of the above technical solution, the beneficial effects of this utility model are:

[0015] This invention discloses a production apparatus for isothiazolinone, comprising a synthesis vessel. The inlet of the synthesis vessel is connected via pipes to a 2-methyl-2,4-pentanediol tank, a carbon disulfide tank, and a sodium hydroxide solution tank. The outlet of the synthesis vessel is connected via pipes to a hydrolysis vessel. The inlet of the hydrolysis vessel is connected via pipes to a hydrochloric acid solution tank, and the outlet of the hydrolysis vessel is connected via pipes to a cyclization vessel. The inlet of the cyclization vessel is connected via pipes to a liquid chlorine tank. The outlet of the cyclization vessel is connected via pipes to a distillation vessel, and the bottom outlet of the distillation vessel is connected via pipes to a finished product tank. 2-Methyl-2,4-pentanediol reacts with carbon disulfide under alkaline conditions to generate dithiocarbonate, which is then acid-hydrolyzed to obtain the intermediate 2-methyl-2,4-pentanedithiol. This intermediate is then oxidatively cyclized with liquid chlorine at low temperature, introducing chlorine atoms. The resulting reaction mixture is purified by distillation to obtain the isothiazolinone product. This method is environmentally friendly, safe, and has a high product yield, reducing production costs.

[0016] The top gaseous outlet of the distillation vessel of this invention is connected to a recovery tank via a pipeline, and the outlet of the recovery tank is connected to the synthesis vessel via a pipeline. The gaseous substances generated during distillation mainly contain unreacted raw materials and some recoverable components such as solvents. By connecting the gaseous outlet to the recovery tank, these recoverable substances can be effectively collected. The recovery tank then returns these substances to the synthesis vessel, realizing the recycling of raw materials, reducing production costs, and minimizing resource waste. Simultaneously, this recycling method also helps to improve the utilization rate of raw materials.

[0017] The bottom outlet of the distillation vessel is connected to an extraction tank via a pipe. The inlet of the extraction tank is connected to an ethyl acetate tank via a pipe. The outlet of the extraction tank is connected to a crystallization tank via a pipe. The inlet of the crystallization tank is connected to a hexane tank via a pipe. The outlet of the crystallization tank is connected to a filtration tank via a pipe. The solid phase outlet of the filtration tank is connected to the finished product tank. The distilled product is further extracted in the extraction tank. Utilizing the selective solubility of isothiazolinones in ethyl acetate, impurities in the product can be separated more effectively, improving product purity. The extracted solution enters the crystallization tank, where hexane is added to adjust the solubility of the solution, promoting the crystallization of isothiazolinones. This process further purifies the product. The outlet of the crystallization tank is connected to the filtration tank. Through filtration, the crystals are separated from the mother liquor, and the solid phase is directly connected to the finished product tank. This completes the entire process from reaction to final purification, greatly improving the purity and quality of the product and meeting the market demand for high-quality isothiazolinone products.

[0018] The solid phase outlet of the filtration tank is connected to a dryer, and the outlet of the dryer is connected to the finished product tank. The solid product obtained after filtration still contains a small amount of solvent and other moisture. By connecting to the dryer, the product can be dried to remove residual moisture and solvent, further improving the purity and stability of the product. The dried product directly enters the finished product tank, ensuring that the quality of the final product meets the standards, extending the product's shelf life, and enhancing its competitiveness in the market.

[0019] The inlet of the filtration tank is connected to the n-hexane tank via a pipeline. During filtration, n-hexane can be used to wash the filter cake. By connecting the n-hexane tank to the inlet of the filtration tank, the amount of n-hexane added and the washing operation can be easily controlled. Hexane washing can effectively remove residual impurities and mother liquor from the surface of the filter cake, further improving the purity of the product. This design makes the washing operation more convenient and efficient, helping to improve product quality and yield.

[0020] The liquid phase outlet of the filtration tank is connected to a distillation tank via a pipeline. The top gas phase outlet of the distillation tank is connected to an ethyl acetate recovery tank and a hexane recovery tank via pipelines. The liquid phase after filtration mainly contains solvents such as ethyl acetate and hexane, as well as a small amount of incompletely separated impurities. By connecting the liquid phase outlet to the distillation tank, the solvents such as ethyl acetate and hexane can be separated by distillation. The separately connected ethyl acetate recovery tank and hexane recovery tank enable the recycling of these two solvents. The recovered solvents can be recycled for extraction and crystallization steps, reducing production costs, minimizing resource waste, and reducing environmental pollution, which aligns with the production principles of green chemistry.

[0021] The outlet of the ethyl acetate recovery tank is connected to a first adsorption tank via a pipeline, and the outlet of the first adsorption tank is connected to the ethyl acetate tank via a pipeline. The recovered ethyl acetate may still contain trace impurities, which may affect its effectiveness in subsequent extraction processes. By using the first adsorption tank, the impurities are adsorbed by the adsorbent, further purifying the recovered ethyl acetate. The purified ethyl acetate is then returned to the ethyl acetate tank for a new round of extraction, ensuring the purity of ethyl acetate during extraction, thereby improving extraction efficiency and product quality, extending solvent lifespan, and reducing production costs.

[0022] The outlet of the hexane recovery tank is connected to a second adsorption tank via a pipeline, and the outlet of the second adsorption tank is connected to the hexane tank via a pipeline. Adsorption purification is performed in the second adsorption tank. During crystallization and other processes, hexane may be contaminated with impurities; the second adsorption tank effectively removes these impurities, improving the purity of the hexane. The purified hexane is returned to the hexane tank and can be used for further crystallization and washing operations, ensuring the quality stability of hexane during production, helping to improve the crystallization effect and purity of the product, reducing production costs, and increasing production efficiency. Attached Figure Description

[0023] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0024] Figure 1 This is a structural schematic diagram of an embodiment of the present utility model;

[0025] The tanks are as follows: 1. Synthesis vessel; 2. 2-Methyl-2,4-pentanediol tank; 3. Carbon disulfide tank; 4. Sodium hydroxide solution tank; 5. Hydrolysis vessel; 6. Hydrochloric acid solution tank; 7. Cycling vessel; 8. Liquid chlorine tank; 9. Distillation vessel; 10. Finished product tank; 11. Recovery tank; 12. Extraction tank; 13. Ethyl acetate tank; 14. Crystallization tank; 15. n-Hexane tank; 16. Filter tank; 17. Dryer; 18. Distillation tank; 19. Ethyl acetate recovery tank; 20. n-Hexane recovery tank; 21. First adsorption tank; 22. Second adsorption tank. Detailed Implementation

[0026] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0027] like Figure 1As shown, an isothiazolinone production apparatus includes a synthesis vessel 1. The inlet of the synthesis vessel 1 is connected via pipes to a 2-methyl-2,4-pentanediol tank 2, a carbon disulfide tank 3, and a sodium hydroxide solution tank 4. The outlet of the synthesis vessel 1 is connected via pipes to a hydrolysis vessel 5. The inlet of the hydrolysis vessel 5 is connected via pipes to a hydrochloric acid solution tank 6. The outlet of the hydrolysis vessel 5 is connected via pipes to a cyclization vessel 7. The inlet of the cyclization vessel 7 is connected via pipes to a liquid chlorine tank 8. The outlet of the cyclization vessel 7 is connected via pipes to a distillation vessel 9. The bottom outlet of the distillation vessel 9 is connected via pipes to a finished product tank 10. 2-methyl-2,4-pentanediol reacts with carbon disulfide under alkaline conditions to generate dithiocarbonate, which is then hydrolyzed with acid to obtain the intermediate 2-methyl-2,4-pentanedithiol. This intermediate is then oxidized and cyclized with liquid chlorine at low temperature, introducing chlorine atoms. The resulting reaction mixture is purified by distillation to obtain the isothiazolinone product. This method is environmentally friendly, safe, and has a high product yield, reducing production costs.

[0028] The top gas phase outlet of the distillation vessel 9 is connected to a recovery tank 11 via a pipeline, and the outlet of the recovery tank 11 is connected to the synthesis vessel 1 via a pipeline. The gaseous substances generated during the distillation process mainly contain unreacted raw materials and some recoverable components such as solvents. By connecting the gas phase outlet to the recovery tank 11, these recoverable substances can be effectively collected. The recovery tank 11 then returns these substances to the synthesis vessel 1, realizing the recycling of raw materials, reducing production costs, and minimizing resource waste. Simultaneously, this recycling method also helps improve the utilization rate of raw materials.

[0029] The bottom outlet of the distillation vessel 9 is connected to an extraction tank 12 via a pipe. The inlet of the extraction tank 12 is connected to an ethyl acetate tank 13 via a pipe. The outlet of the extraction tank 12 is connected to a crystallization tank 14 via a pipe. The inlet of the crystallization tank 14 is connected to a hexane tank 15 via a pipe. The outlet of the crystallization tank 14 is connected to a filtration tank 16 via a pipe. The solid phase outlet of the filtration tank 16 is connected to the finished product tank 10. The distilled product is further extracted in the extraction tank 12. Utilizing the selective solubility of isothiazolinones in ethyl acetate, impurities in the product can be separated more effectively, improving product purity. The extracted solution enters the crystallization tank 14, where hexane is added to adjust the solubility of the solution, promoting the crystallization of isothiazolinones. This process further purifies the product. The outlet of the crystallization tank 14 is connected to the filtration tank 16. Through filtration, the crystals are separated from the mother liquor, and the solid phase is directly connected to the finished product tank 10. This completes the entire process from reaction to final purification, greatly improving the purity and quality of the product and meeting the market demand for high-quality isothiazolinone products.

[0030] The solid phase outlet of the filtration tank 16 is connected to a dryer 17, and the outlet of the dryer 17 is connected to the finished product tank 10. The solid phase product obtained after filtration still contains a small amount of solvent and other moisture. By connecting to the dryer 17, the product can be dried to remove residual moisture and solvent, further improving the purity and stability of the product. The dried product directly enters the finished product tank 10, ensuring that the quality of the final product meets the standards, extending the product's shelf life, and improving the product's competitiveness in the market.

[0031] The inlet of the filtration tank 16 is connected to the n-hexane tank 15 via a pipe. During filtration, n-hexane can be used to wash the filter cake. By connecting the n-hexane tank 15 to the inlet of the filtration tank 16, the amount of n-hexane added and the washing operation can be easily controlled. Hexane washing can effectively remove residual impurities and mother liquor from the surface of the filter cake, further improving the purity of the product. This design makes the washing operation more convenient and efficient, helping to improve product quality and yield.

[0032] The liquid phase outlet of the filtration tank 16 is connected to a distillation tank 18 via a pipeline. The top gas phase outlet of the distillation tank 18 is connected to an ethyl acetate recovery tank 19 and a hexane recovery tank 20 via pipelines. The liquid phase after filtration mainly contains solvents such as ethyl acetate and hexane, as well as a small amount of incompletely separated impurities. By connecting the liquid phase outlet to the distillation tank 18, the solvents such as ethyl acetate and hexane can be separated by distillation. The ethyl acetate recovery tank 19 and the hexane recovery tank 20, which are connected respectively, realize the recycling of these two solvents. The recovered solvents can be recycled for extraction and crystallization steps, reducing production costs, reducing resource waste, and also reducing environmental pollution, which is in line with the production concept of green chemistry.

[0033] The outlet of the ethyl acetate recovery tank 19 is connected to a first adsorption tank 21 via a pipeline, and the outlet of the first adsorption tank 21 is connected to the ethyl acetate tank 13 via a pipeline. The recovered ethyl acetate may still contain trace impurities, which may affect its effectiveness in subsequent extraction processes. Through the first adsorption tank 21, the recovered ethyl acetate can be further purified by the adsorption of impurities by the adsorbent. The purified ethyl acetate is then returned to the ethyl acetate tank 13 for a new round of extraction, ensuring the purity of ethyl acetate during the extraction process, thereby improving the extraction effect and product quality, extending the solvent's lifespan, and reducing production costs.

[0034] The outlet of the hexane recovery tank 20 is connected to a second adsorption tank 22 via a pipeline, and the outlet of the second adsorption tank 22 is connected to the hexane tank 15 via a pipeline. Adsorption purification is performed through the second adsorption tank 22. During crystallization and other processes, hexane may be contaminated with impurities; the second adsorption tank 22 effectively removes these impurities, improving the purity of the hexane. The purified hexane is returned to the hexane tank 15 and can be used for further crystallization and washing operations, ensuring the quality stability of hexane during production, helping to improve the crystallization effect and purity of the product, reducing production costs, and increasing production efficiency.

[0035] It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.

Claims

1. An apparatus for producing isothiazolinone, comprising a synthesis tank, characterized by: The inlet of the synthesis kettle is communicated with 2-methyl-2,4-pentanediol tank, carbon disulfide tank and sodium hydroxide solution tank through pipelines respectively, the outlet of the synthesis kettle is communicated with hydrolysis kettle through pipeline, the inlet of the hydrolysis kettle is communicated with hydrochloric acid solution tank through pipeline, the outlet of the hydrolysis kettle is communicated with cyclization kettle through pipeline, the inlet of the cyclization kettle is communicated with liquid chlorine tank through pipeline; The outlet of the cyclization kettle is communicated with distillation kettle through pipeline, the bottom outlet of the distillation kettle is communicated with product tank through pipeline.

2. The apparatus for producing an isothiazolone according to claim 1, characterized by: The top gas phase outlet of the distillation kettle is communicated with recovery tank through pipeline, the outlet of the recovery tank is communicated with the synthesis kettle through pipeline.

3. The apparatus for producing isothiazolone according to claim 1, wherein: The bottom outlet of the distillation kettle is communicated with extraction tank through pipeline, the inlet of the extraction tank is communicated with ethyl acetate tank through pipeline, the outlet of the extraction tank is communicated with crystallization tank through pipeline, the inlet of the crystallization tank is communicated with n-hexane tank through pipeline, the outlet of the crystallization tank is communicated with suction filter tank, and the solid phase outlet of the suction filter tank is communicated with the product tank.

4. The apparatus for producing isothiazolone according to claim 3, wherein: The solid phase outlet of the suction filter tank is communicated with a dryer, and the outlet of the dryer is communicated with the product tank.

5. The apparatus for producing isothiazolone according to claim 3, wherein: The inlet of the suction filter tank is communicated with the n-hexane tank through pipeline.

6. The apparatus for producing isothiazolone according to claim 3, wherein: The liquid phase outlet of the suction filter tank is communicated with distillation tank, and the top gas phase outlet of the distillation tank is communicated with ethyl acetate recovery tank and n-hexane recovery tank through pipelines respectively.

7. The apparatus for producing an isothiazolone according to claim 6, characterized by: The outlet of the ethyl acetate recovery tank is communicated with first adsorption tank through pipeline, and the outlet of the first adsorption tank is communicated with the ethyl acetate tank through pipeline.

8. The apparatus for producing an isothiazolone according to claim 6, characterized by: The outlet of the n-hexane recovery tank is communicated with second adsorption tank through pipeline, and the outlet of the second adsorption tank is communicated with the n-hexane tank through pipeline.

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