A Kathon production apparatus

Abstract

This utility model discloses a Kathon production apparatus, relating to the field of Kathon production technology. A 2-methyl-4-isothiazolin-3-one tank is connected to a dissolving tank, which in turn is connected to a phosphate buffer solution tank and a primary microchannel reactor. The primary microchannel reactor is connected to an activating chlorinating agent tank and a secondary microchannel reactor. The secondary microchannel reactor is connected to the activating chlorinating agent tank and a tertiary stabilizer. The inlet of the tertiary stabilizer is connected to a sodium thiosulfate solution tank, and the outlet of the tertiary stabilizer is connected to a Kathon product tank. This significantly improves product yield, shortens the reaction cycle, enhances safety, and is environmentally friendly. The microchannel reactor ensures efficient mass and heat transfer, reduces side reactions, and improves product purity. The tertiary stabilizer ensures complete removal of residual chlorine, improving product stability.

Description

Technical Field

[0001] This utility model relates to the field of Kathon production technology, specifically to a Kathon production apparatus. Background Technology

[0002] Kathon (an isothiazolinone compound) is a highly efficient and broad-spectrum preservative widely used in numerous fields such as industrial circulating water, papermaking, coatings, and daily chemicals. Traditional Kathon production methods suffer from several problems, including: the production process is mostly batch-based, with long reaction times and low production efficiency; the product purity is not high, and the presence of impurities affects its application in high-end fields; the reaction process uses large amounts of organic solvents, resulting in high processing costs, serious environmental threats, and safety hazards. Summary of the Invention

[0003] The technical problem to be solved by this utility model is to provide a Kathon production device that addresses the shortcomings of the existing technology, has a short reaction time, improves production efficiency, is environmentally friendly, and is highly safe.

[0004] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:

[0005] A Kathon production apparatus includes a 2-methyl-4-isothiazolin-3-one tank, the outlet of which is connected via a pipeline to a dissolving tank, the inlet of which is connected via a pipeline to a phosphate buffer solution tank, the outlet of which is connected via a pipeline to a primary microchannel reactor, the inlet of which is connected via a pipeline to an activating chlorinating agent tank, the outlet of which is connected via a pipeline to a secondary microchannel reactor, the inlet of which is connected via a pipeline to the activating chlorinating agent tank, the outlet of which is connected via a pipeline to a tertiary stabilizer, the inlet of which is connected via a pipeline to a sodium thiosulfate solution tank, and the outlet of which is connected via a pipeline to a Kathon product tank.

[0006] As an improved technical solution, the outlet of the 2-methyl-4-isothiazolin-3-one tank is connected to a distillation tank via a pipeline, the gas phase outlet of the distillation tank is connected to a purification tank via a pipeline, and the outlet of the purification tank is connected to the dissolving tank via a pipeline.

[0007] As an improved technical solution, the inlet of the activating chlorinating agent tank is connected to a plasma activation tank via a pipeline, and the inlet of the plasma activation tank is connected to a sodium hypochlorite solution tank via a pipeline.

[0008] As an improved technical solution, a flow sensor and a switching valve are installed on the pipeline between the activating chlorinator tank and the primary microchannel reactor, and the flow sensor and the switching valve are interlocked to the control system.

[0009] As an improved technical solution, a shut-off valve is provided on the pipeline between the primary microchannel reactor and the secondary microchannel reactor, and a UV sensor is provided inside the secondary microchannel reactor. The shut-off valve and the UV sensor are interlocked to the control system.

[0010] As an improved technical solution, the inlet of the three-stage stabilizer is connected to a nitrogen tank, and the outlet of the three-stage stabilizer is connected to a chlorine recovery tank via a pipeline.

[0011] As a preferred technical solution, the outlet of the Kathon product tank is connected to a thin-film evaporator via a pipe, and the outlet of the thin-film evaporator is connected to a Kathon pure product tank via a pipe.

[0012] As a preferred technical solution, the outlet of the Kathon product tank is connected to a molecular sieve adsorber via a pipeline, and the outlet of the molecular sieve adsorber is connected to the thin film evaporator via a pipeline.

[0013] Due to the adoption of the above technical solution, the beneficial effects of this utility model are:

[0014] This utility model discloses a Kathon production apparatus, comprising a 2-methyl-4-isothiazolin-3-one tank, the outlet of which is connected to a dissolving tank via a pipeline, the inlet of which is connected to a phosphate buffer solution tank via a pipeline, the outlet of which is connected to a primary microchannel reactor via a pipeline, the inlet of which is connected to an activating chlorinating agent tank via a pipeline, the outlet of which is connected to a secondary microchannel reactor via a pipeline, the inlet of which is connected to the activating chlorinating agent tank via a pipeline, the outlet of which is connected to a tertiary stabilizer via a pipeline, the inlet of which is connected to a sodium thiosulfate solution tank via a pipeline, and the outlet of which is connected to a Kathon product tank via a pipeline. A 2-methyl-4-isothiazolin-3-one solution reacts with an activated sodium hypochlorite solution in a primary microchannel reactor for less than 30 seconds to generate a 5-chloro-2-methyl-4-isothiazolin-3-one intermediate. Then, activated sodium hypochlorite solution is added to a secondary microchannel reactor, and the reaction continues for approximately 2 minutes. Finally, the reaction is terminated by adding sodium thiosulfate solution to a tertiary stabilizer, ultimately yielding the Kathon product. This process significantly improves product yield and shortens the reaction cycle. The low liquid holdup in the microchannel reactor greatly reduces the possibility of boiling over, ensuring higher safety. Furthermore, the use of a phosphate buffer solution instead of an organic solvent is environmentally friendly. The microchannel reactor ensures efficient mass and heat transfer, reduces side reactions, and improves product purity. The tertiary stabilizer ensures complete removal of residual chlorine, enhancing product stability.

[0015] The outlet of the 2-methyl-4-isothiazolin-3-one vessel of this invention is connected to a distillation tank via a pipeline. The gas phase outlet of the distillation tank is connected to a purification tank via a pipeline, and the outlet of the purification tank is connected to the dissolution tank via a pipeline. This process removes organic impurities (such as esters and solvents) from 2-methyl-4-isothiazolin-3-one, reduces subsequent side reactions, avoids impurities interfering with the chlorination process, and improves the Kathon yield.

[0016] The inlet of the activating chlorinating agent tank is connected to a plasma activation tank via a pipeline, and the inlet of the plasma activation tank is connected to a sodium hypochlorite solution tank via a pipeline. Plasma activation of NaClO generates highly reactive chlorine species (Cl...). + / Cl·), eliminating the need for hazardous gas storage and reducing excessive chlorination byproducts.

[0017] A flow sensor and a switching valve are installed on the pipeline between the activated chlorinating agent tank and the primary microchannel reactor. The flow sensor and the switching valve are interlocked to the control system. The feed of activated sodium hypochlorite is dynamically adjusted according to the added flow rate of 2-methyl-4-isothiazolin-3-one (MIT) to ensure a stable Cl:MIT molar ratio and prevent excessive chlorination from causing a runaway reaction.

[0018] A shut-off valve is installed on the pipeline between the primary microchannel reactor and the secondary microchannel reactor. A UV sensor is installed inside the secondary microchannel reactor. The shut-off valve and the UV sensor are interlocked to the control system. The reaction progress is determined by the absorbance at 285 nm, and the amount of 5-chloro-2-methyl-4-isothiazolin-3-one produced is monitored in real time to ensure the quality of Kathon.

[0019] The inlet of the three-stage stabilizer is connected to a nitrogen tank, and the outlet of the three-stage stabilizer is connected to a chlorine recovery tank via a pipeline. The three-stage stabilizer is bubbled with nitrogen, and the outlet is connected to the chlorine recovery tank. The nitrogen carries away the dissolved Cl2, leaving residual chlorine <1ppm. The recovered Cl2 is converted into NaClO for recycling, reducing waste.

[0020] The outlet of the Kathon product tank is connected to a thin-film evaporator via a pipeline, and the outlet of the thin-film evaporator is connected to a Kathon pure product tank via a pipeline. Through low-temperature, high-efficiency concentration (operating temperature ≤50℃), thermal decomposition of Kathon is avoided, the effective ingredient retention rate is >99%, and energy saving is also achieved.

[0021] The outlet of the Kathon product tank is connected to a molecular sieve adsorber via a pipeline, and the outlet of the molecular sieve adsorber is connected to the thin-film evaporator via a pipeline. Through deep impurity removal, trace colored impurities (such as metal ions) are removed, improving the product's light transmittance and stability. Attached Figure Description

[0022] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0023] Figure 1 This is a structural schematic diagram of an embodiment of the present utility model;

[0024] The components include: 1. 2-methyl-4-isothiazolin-3-one tank; 2. Dissolving tank; 3. Phosphate buffer solution tank; 4. Primary microchannel reactor; 5. Activating chlorinating agent tank; 6. Secondary microchannel reactor; 7. Tertiary stabilizer; 8. Sodium thiosulfate solution tank; 9. Kathon product tank; 10. Distillation tank; 11. Purification tank; 12. Plasma activation tank; 13. Sodium hypochlorite solution tank; 14. Flow sensor; 15. Switch valve; 16. Shut-off valve; 17. UV sensor; 18. Nitrogen tank; 19. Chlorine recovery tank; 20. Thin-film evaporator; 21. Kathon pure product tank; 22. Molecular sieve adsorber. Detailed Implementation

[0025] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0026] like Figure 1 As shown, a Kathon production apparatus includes a 2-methyl-4-isothiazolin-3-one tank 1. The outlet of the 2-methyl-4-isothiazolin-3-one tank 1 is connected to a dissolving tank 2 via a pipeline. The inlet of the dissolving tank 2 is connected to a phosphate buffer solution tank 3 via a pipeline. The outlet of the dissolving tank 2 is connected to a primary microchannel reactor 4 via a pipeline. The inlet of the primary microchannel reactor 4 is connected to an activating chlorinating agent tank 5 via a pipeline. The outlet of the primary microchannel reactor 4 is connected to a secondary microchannel reactor 6 via a pipeline. The inlet of the secondary microchannel reactor 6 is connected to the activating chlorinating agent tank 5 via a pipeline. The outlet of the secondary microchannel reactor 6 is connected to a tertiary stabilizer 7 via a pipeline. The inlet of the tertiary stabilizer 7 is connected to a sodium thiosulfate solution tank 8 via a pipeline. The outlet of the tertiary stabilizer 7 is connected to a Kathon production apparatus. In the Kathon product tank 9, a 2-methyl-4-isothiazolin-3-one solution and an activated sodium hypochlorite solution react in a primary microchannel reactor 4 with a residence time of less than 30 seconds, generating a 5-chloro-2-methyl-4-isothiazolin-3-one intermediate. Then, an activated sodium hypochlorite solution is added to a secondary microchannel reactor 6, and the reaction continues for approximately 2 minutes. Finally, the reaction is terminated by adding sodium thiosulfate solution to a tertiary stabilizer 7, ultimately yielding the Kathon product. This process significantly improves product yield and shortens the reaction cycle. The small liquid holdup in the microchannel reactors greatly reduces the possibility of boiling over, enhancing safety. Furthermore, the use of a phosphate buffer solution instead of an organic solvent is environmentally friendly. The microchannel reactors ensure efficient mass and heat transfer, reducing side reactions and improving product purity. The tertiary stabilizer 7 ensures complete removal of residual chlorine, improving product stability.

[0027] The outlet of the 2-methyl-4-isothiazolin-3-one tank 1 is connected to a distillation tank 10 via a pipeline. The gas phase outlet of the distillation tank 10 is connected to a purification tank 11 via a pipeline. The outlet of the purification tank 11 is connected to the dissolution tank 2 via a pipeline. This process removes organic impurities (such as esters and solvents) from 2-methyl-4-isothiazolin-3-one, reduces subsequent side reactions, avoids impurities interfering with the chlorination process, and improves the Kathon yield.

[0028] The inlet of the activating chlorinating agent tank 5 is connected to a plasma activation tank 12 via a pipe, and the inlet of the plasma activation tank 12 is connected to a sodium hypochlorite solution tank 13 via a pipe. Plasma activation of NaClO generates highly reactive chlorine species (Cl+ / Cl·), eliminating the need for hazardous gas storage and reducing excessive chlorination byproducts.

[0029] A flow sensor 14 and a switching valve 15 are installed on the pipeline between the activated chlorinating agent tank 5 and the primary microchannel reactor 4. The flow sensor 14 and the switching valve 15 are interlocked to the control system. The feed of activated sodium hypochlorite is dynamically adjusted according to the added flow rate of 2-methyl-4-isothiazolin-3-one (MIT) to ensure a stable Cl:MIT molar ratio and prevent excessive chlorination from causing a runaway reaction.

[0030] A shut-off valve 16 is installed on the pipeline between the primary microchannel reactor 4 and the secondary microchannel reactor 6. A UV sensor 17 is installed inside the secondary microchannel reactor 6. The shut-off valve 16 and the UV sensor 17 are interlocked to the control system. The reaction progress is determined by the absorbance at 285 nm, and the amount of 5-chloro-2-methyl-4-isothiazolin-3-one produced is monitored in real time to ensure the quality of Kathon.

[0031] The inlet of the three-stage stabilizer 7 is connected to a nitrogen tank 18, and the outlet of the three-stage stabilizer 7 is connected to a chlorine recovery tank 19 via a pipeline. The three-stage stabilizer 7 is bubbled with nitrogen gas, and the outlet is connected to the chlorine recovery tank 19. The nitrogen gas carries away the dissolved Cl2, leaving residual chlorine <1ppm. The recovered Cl2 is converted into NaClO for recycling, reducing waste.

[0032] The outlet of the Kathon product tank 9 is connected to a thin-film evaporator 20 via a pipe, and the outlet of the thin-film evaporator 20 is connected to a Kathon pure product tank 21 via a pipe. Through low-temperature, high-efficiency concentration (operating temperature ≤50℃), thermal decomposition of Kathon is avoided, the effective ingredient retention rate is >99%, and energy saving is also achieved.

[0033] The outlet of the Kathon product tank 9 is connected to a molecular sieve adsorber 22 via a pipe, and the outlet of the molecular sieve adsorber 22 is connected to the thin-film evaporator 20 via a pipe. Through deep impurity removal, trace amounts of colored impurities (such as metal ions) are removed, improving the product's light transmittance and stability.

[0034] 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. A Kathon production apparatus, comprising a 2-methyl-4-isothiazolin-3-one tank, characterized in that: The outlet of the 2-methyl-4-isothiazolin-3-one tank is connected to a dissolving tank via a pipeline. The inlet of the dissolving tank is connected to a phosphate buffer solution tank via a pipeline. The outlet of the dissolving tank is connected to a primary microchannel reactor via a pipeline. The inlet of the primary microchannel reactor is connected to an activating chlorinator tank via a pipeline. The outlet of the primary microchannel reactor is connected to a secondary microchannel reactor via a pipeline. The inlet of the secondary microchannel reactor is connected to the activating chlorinator tank via a pipeline. The outlet of the secondary microchannel reactor is connected to a tertiary stabilizer via a pipeline. The inlet of the tertiary stabilizer is connected to a sodium thiosulfate solution tank via a pipeline. The outlet of the tertiary stabilizer is connected to a Kathon product tank via a pipeline.

2. The Kathon production apparatus as described in claim 1, characterized in that: The outlet of the 2-methyl-4-isothiazolin-3-one tank is connected to a distillation tank via a pipeline, the gas phase outlet of the distillation tank is connected to a purification tank via a pipeline, and the outlet of the purification tank is connected to the dissolving tank via a pipeline.

3. The Kathon production apparatus as described in claim 1, characterized in that: The inlet of the activating chlorinating agent tank is connected to a plasma activation tank via a pipe, and the inlet of the plasma activation tank is connected to a sodium hypochlorite solution tank via a pipe.

4. The Kathon production apparatus as described in claim 1, characterized in that: A flow sensor and a switching valve are installed on the pipeline between the activated chlorinating agent tank and the primary microchannel reactor. The flow sensor and the switching valve are interlocked to the control system.

5. The Kathon production apparatus as described in claim 1, characterized in that: A shut-off valve is installed on the pipeline between the primary microchannel reactor and the secondary microchannel reactor. A UV sensor is installed inside the secondary microchannel reactor. The shut-off valve and the UV sensor are interlocked to the control system.

6. The Kathon production apparatus as described in claim 1, characterized in that: The inlet of the three-stage stabilizer is connected to a nitrogen tank, and the outlet of the three-stage stabilizer is connected to a chlorine recovery tank via a pipeline.

7. The Kathon production apparatus as described in claim 1, characterized in that: The outlet of the Kathon product tank is connected to a thin-film evaporator via a pipe, and the outlet of the thin-film evaporator is connected to a Kathon pure product tank via a pipe.

8. The Kathon production apparatus as described in claim 7, characterized in that: The outlet of the Kathon product tank is connected to a molecular sieve adsorber via a pipe, and the outlet of the molecular sieve adsorber is connected to the thin film evaporator via a pipe.

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