Isothiazolinone quaternary ammonium salt production device

Abstract

The utility model belongs to the technical field of chemical production, and discloses an isothiazolinone quaternary ammonium salt production device which comprises an amination reaction kettle, a distillation kettle, a quaternization reaction kettle, a cooling crystallization kettle, a filtering device, a recrystallization kettle and a drying device which are sequentially communicated through pipelines, valves and pumps, the amination reaction kettle is provided with a temperature control device, a stirring device, a temperature sensor, a condensation reflux device and a material dripping device, and an air suction cover is arranged outside the amination reaction kettle; a diethylenetriamine inlet and a bromo-undecanoic acid methyl ester inlet are further formed, the diethylenetriamine inlet is externally connected with a diethylenetriamine storage tank through a pipeline, and the bromo-undecanoic acid methyl ester inlet is outwards connected to a bromo-undecanoic acid methyl ester storage tank through a pipeline and is inwards connected with a dropwise adding device; the quaternization reaction kettle is provided with a temperature control device, a stirring device, a temperature sensor and a pH sensor. The device is reasonable in design, simple in structure, convenient to operate and easy for industrial production.

Description

Technical Field

[0001] This utility model belongs to the field of chemical production technology, specifically relating to a production device for isothiazolinone quaternary ammonium salt. Background Technology

[0002] Isothiazolinones are a novel type of broad-spectrum fungicide, possessing advantages such as high efficiency, broad spectrum, low toxicity, and biodegradability in the environment, making them widely applicable. Isothiazolinone quaternary ammonium salts are one type of isothiazolinone compound, primarily used in the industrial fungicide field. Currently, although some preparation methods for isothiazolinone quaternary ammonium salts have been published both domestically and internationally, these are limited to theoretical research, and corresponding industrial-scale production equipment has not been disclosed, hindering the market development and application of this product. Summary of the Invention

[0003] The technical problem to be solved by this utility model is to provide an isothiazolinone quaternary ammonium salt production device, which overcomes the defects in the prior art. It uses methyl bromoundecanoate, isothiazolinone and diethylenetriamine to prepare isothiazolinone quaternary ammonium salt. The production device is reasonably designed, simple in structure, easy to operate and easy to industrialize.

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

[0005] An apparatus for producing isothiazolinone quaternary ammonium salts includes an amination reactor, a distillation reactor, a quaternization reactor, a cooling crystallization reactor, a filtration device, a recrystallization reactor, and a drying device, which are connected sequentially by pipes, valves, and pumps. The amination reactor is equipped with a temperature control device (circulating water bath or electric heating mantle), a stirring device, a temperature sensor, a condensation reflux device, and a material dripping device. An exhaust hood is installed outside the amination reactor (diethylenetriamine and methyl bromide are odorous and irritating, and any overflowing odors and materials need to be promptly removed and treated). It also has a diethylenetriamine inlet and a methyl bromide inlet. The diethylenetriamine inlet is connected to a diethylenetriamine storage tank via a pipe, and the methyl bromide inlet is connected to the methyl bromide storage tank via a pipe and connected to a dripping device. The quaternization reactor is equipped with a temperature control device (circulating water bath or electric heating mantle), a stirring device, a temperature sensor, and a pH sensor.

[0006] Preferably, the amination reactor is a glass-lined reactor, and the quaternization reactor is a porcelain-lined reactor. It is corrosion-resistant.

[0007] Preferably, the quaternization reactor is equipped with an isothiazolinone inlet, a solvent inlet, and a hydrochloric acid inlet. The isothiazolinone inlet is connected to an isothiazolinone storage tank via a pipeline, and the solvent inlet and the hydrochloric acid inlet are respectively connected to an ethanol-water mixed solvent storage tank and a hydrochloric acid storage tank via pipelines.

[0008] Preferably, the quaternization reactor is equipped with an external suction hood, which, together with the suction hood on the outside of the amination reactor, is connected to an external exhaust gas treatment device.

[0009] Preferably, the distillation vessel is a vacuum distillation vessel, and the distillation vessel is also connected to a methanol storage tank. The distilled methanol is then recovered and reused.

[0010] Preferably, both the cooling crystallization kettle and the recrystallization kettle are equipped with a temperature control device. The temperature control device is a circulating water bath or an electric heating mantle.

[0011] Preferably, the recrystallization vessel is connected to the ethanol-water storage tank via a pipeline.

[0012] Preferably, the filtration device is a filter press.

[0013] Preferably, the drying device is a vacuum drying oven or a spray drying tower.

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

[0015] In this invention, diethylenetriamine and methyl bromide undecanoate are first subjected to an amination reaction in an amination reactor. After distillation, a tertiary amine intermediate is obtained. The tertiary amine intermediate is then subjected to a quaternization reaction with isothiazolinone. After cooling and crystallization, filtration, recrystallization, and drying, the isothiazolinone quaternary ammonium salt product is obtained.

[0016] In summary, this utility model has a reasonable design, simple structure, convenient operation, and is easy to industrialize. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the structure of Embodiment 1 of this utility model;

[0018] In the diagram, 1 is an amination reactor; 2 is a distillation vessel; 3 is a quaternization reactor; 4 is a cooling crystallization vessel; 5 is a filtration device; 6 is a recrystallization vessel; 7 is a drying device; 8 is a suction hood; 9 is a diethylenetriamine storage tank; 10 is a methyl bromide storage tank; 11 isothiazolinone storage tank; 12 is an ethanol-water mixed solvent storage tank; 13 is a hydrochloric acid storage tank; and 14 is a methanol storage tank. Detailed Implementation

[0019] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0020] Example 1:

[0021] like Figure 1As shown, an apparatus for producing isothiazolinone quaternary ammonium salts includes an amination reactor 1, a distillation reactor 2, a quaternization reactor 3, a cooling crystallization reactor 4, a filtration device 5, a recrystallization reactor 6, and a drying device 7, which are sequentially connected by pipes (not shown), valves (not shown), and pumps (not shown). The amination reactor is equipped with a temperature control device (not shown), a stirring device (not shown), a temperature sensor (not shown), a reflux condenser (not shown), and a material dripping device (not shown). 1. An external suction hood 8 is provided; it is also equipped with a diethylenetriamine inlet (not marked) and a methyl bromide inlet (not marked). The diethylenetriamine inlet is connected to the diethylenetriamine storage tank 9 through a pipeline, and the methyl bromide inlet is connected to the methyl bromide storage tank 10 through a pipeline, and is connected to a dripping device (not marked) inward; the quaternization reactor 3 is equipped with a temperature control device (not marked), a stirring device (not marked), a temperature sensor (not marked), and a pH sensor (not marked).

[0022] The quaternization reactor 3 is equipped with an isothiazolinone inlet (not labeled), a solvent inlet, and a hydrochloric acid inlet (not labeled). The isothiazolinone inlet is connected to the isothiazolinone storage tank 11 via a pipeline, and the solvent inlet and the hydrochloric acid inlet are connected to the ethanol-water mixed solvent storage tank 12 and the hydrochloric acid storage tank 13 via pipelines, respectively. The distillation reactor 2 is also connected to the methanol storage tank 14. The recrystallization reactor 6 is connected to the ethanol-water mixed solvent storage tank 12 via a pipeline. The quaternization reactor is equipped with an exhaust hood 8, which, together with the exhaust hood 8 on the outside of the amination reactor 1, is connected to an external tail gas treatment device (not labeled).

[0023] In actual production, diethylenetriamine is first added to amination reactor 1, and the temperature is raised to 60-80°C. Then, methyl bromide (diethylenetriamine to methyl bromide molar ratio 1:1-1.2) is slowly added dropwise, controlling the dropping rate to avoid violent exothermic reactions. After the addition is complete, the temperature is raised to 100-120°C, and the reaction is carried out for 4-6 hours. The reacted material is then transferred to distillation reactor 2 for vacuum distillation to obtain a tertiary amine intermediate. The tertiary amine intermediate is then transferred to quaternization reactor 3, and ethanol (volume ratio 1:1) is added. An ethanol / water mixture is used as a solvent, followed by the addition of isothiazolinone in a 1:1 molar ratio to the tertiary amine intermediate. The pH is adjusted to 3-5 with hydrochloric acid, and the temperature is raised to 70-90℃ for 3-5 hours. The reactants are then transferred to a cooling crystallization vessel 4 to cool to room temperature for crystallization. The crystallized material is then conveyed to a filtration device 5 (filter press) for filtration. The crystals are then conveyed to a recrystallization vessel 6, where an ethanol / water mixture is added for recrystallization. After removing the solvent, the crystals are spray-dried to obtain the isothiazolinone quaternary ammonium salt product. The exhaust gas generated during the production process is treated by an exhaust gas treatment device, and the wastewater is neutralized and then sent to a wastewater treatment plant for further treatment.

[0024] 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 an isothiazolinone quaternary ammonium salt, characterized by: The system includes an amination reactor, a distillation reactor, a quaternization reactor, a cooling crystallization reactor, a filtration device, a recrystallization reactor, and a drying device, all connected sequentially by pipes, valves, and pumps. The amination reactor is equipped with a temperature control device, a stirring device, a temperature sensor, a reflux condenser, and a material dripping device, and is fitted with an external suction hood. It also has a diethylenetriamine inlet and a methyl bromide inlet. The diethylenetriamine inlet is connected to a diethylenetriamine storage tank via a pipe, and the methyl bromide inlet is connected to the methyl bromide storage tank via a pipe and has a dripping device connected internally. The quaternization reactor is equipped with a temperature control device, a stirring device, a temperature sensor, and a pH sensor.

2. The isothiazolone quaternary ammonium salt production apparatus according to claim 1, characterized by: The amination reactor is a glass-lined reactor, and the quaternization reactor is a porcelain-lined reactor.

3. The isothiazolone quaternary ammonium salt production apparatus according to claim 1, characterized by: The quaternization reactor is equipped with an isothiazolinone inlet, a solvent inlet, and a hydrochloric acid inlet. The isothiazolinone inlet is connected to the isothiazolinone storage tank via a pipeline, and the solvent and hydrochloric acid inlets are connected to the ethanol-water mixed solvent storage tank and the hydrochloric acid storage tank via pipelines, respectively.

4. The isothiazolone quaternary ammonium salt production apparatus according to claim 1, characterized by: The quaternization reactor is equipped with an external suction hood, which, together with the suction hood outside the amination reactor, is connected to an external exhaust gas treatment device.

5. The isothiazolone quaternary ammonium salt production apparatus according to claim 1, characterized by: The distillation vessel is a vacuum distillation vessel, and the distillation vessel is also connected to a methanol storage tank.

6. The isothiazolone quaternary ammonium salt production apparatus according to claim 1, characterized by: Both the cooling crystallization kettle and the recrystallization kettle are equipped with temperature control devices.

7. The isothiazolone quaternary ammonium salt production apparatus according to claim 1, characterized by: The recrystallization vessel is connected to the ethanol-water storage tank via a pipeline.

8. The isothiazolone quaternary ammonium salt production apparatus according to claim 1, characterized by: The filtration device is a filter press.

9. The isothiazolone quaternary ammonium salt production apparatus according to claim 1, characterized by: The drying device is a vacuum drying box or a spray drying tower.

Images