Benzisothiazolinone zinc acrylate resin production device

Abstract

The utility model belongs to the technical field of chemical production, and discloses a benzisothiazolinone zinc acrylate resin production device which comprises an intermediate reaction kettle, a distillation device, a drying device, a total reaction kettle and a filtering device which are sequentially communicated through a pipeline, a valve and a pump, each of the intermediate reaction kettle and the total reaction kettle is provided with a temperature control device, a stirring device, a temperature sensor and a nitrogen protection device, and the total reaction kettle is also provided with a pH sensor and a dropwise adding device. 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 benzisothiazolinone zinc acrylate resin. Background Technology

[0002] Benzisothiazolinone (BIT) is a highly effective broad-spectrum bactericide that can effectively kill a variety of bacteria and fungi. Acrylic resin coatings exhibit excellent performance, with good light and weather resistance, heat resistance, resistance to over-baking, chemical resistance, and corrosion resistance; therefore, coatings made from acrylic resins have a wide range of applications and are available in numerous varieties.

[0003] The preparation of benzisothiazolinone-zinc acrylate resin by combining benzisothiazolinone with zinc acrylate resin can effectively combine the bactericidal properties of benzisothiazolinone with the film-forming properties of zinc acrylate resin, and has both long-lasting antibacterial and weather-resistant properties, which can be used in marine coatings, wood preservation and other fields.

[0004] Currently, although some preparation methods for benzisothiazolinone zinc acrylate resin have been disclosed both domestically and internationally, they are all limited to theoretical research and no corresponding industrial production equipment has been disclosed, which hinders the market development and application of this product. Summary of the Invention

[0005] The technical problem to be solved by this utility model is to provide a production device for benzisothiazolinone zinc acrylate resin, which overcomes the defects in the prior art. It uses benzisothiazolinone, maleic anhydride and acrylic resin to prepare benzisothiazolinone zinc acrylate resin. The production device is reasonably designed, simple in structure, easy to operate and easy to industrialize.

[0006] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:

[0007] A production apparatus for benzisothiazolinone zinc acrylate resin includes an intermediate reaction vessel, a distillation device, a drying device, a main reaction vessel, and a filtration device, which are connected in sequence by pipes, valves, and pumps. The intermediate reaction vessel and the main reaction vessel are equipped with a temperature control device, a stirring device, a temperature sensor, and a nitrogen protection device. The main reaction vessel is also equipped with a pH sensor and a dripping device.

[0008] Preferably, the intermediate reactor is a glass-lined reactor, and the main reactor is a stainless steel reactor. This provides corrosion resistance.

[0009] Preferably, the temperature control device is a heating / cooling jacket.

[0010] Preferably, the intermediate reaction vessel is provided with a solid material inlet, a liquid material inlet, a nitrogen inlet, and a gas outlet; the solid material inlet is connected to a maleic anhydride storage tank, a benzisothiazolinone storage tank, and a p-toluenesulfonic acid storage tank via pipelines, respectively; the liquid material inlet is connected to a xylene storage tank via pipelines; and the nitrogen inlet is connected to an external nitrogen storage tank via pipelines and a gas pump.

[0011] Preferably, the main reactor is equipped with a solid material inlet, a liquid material inlet, a nitrogen inlet, and a gas outlet. The solid material inlet is connected via pipelines to an acrylic resin storage tank, a drying device, and a zinc oxide storage tank. The liquid material inlet is connected via pipelines to a xylene storage tank and a dibutyltin dilaurate storage tank. The nitrogen inlet is connected via pipelines and a gas pump to an external nitrogen storage tank. The main reactor is also connected to a dilute acid storage tank and a dilute alkali storage tank for adjusting the pH value.

[0012] Preferably, the nitrogen protection device includes a nitrogen inlet and a gas outlet, with the nitrogen inlet connected to a nitrogen storage tank via a pipeline and a gas pump.

[0013] Preferably, the distillation apparatus is a vacuum distillation apparatus, specifically a thin-film evaporator. The distillation apparatus is also connected to a xylene recovery tank. The distilled xylene is recovered and reused, with a recovery rate of ≥90%.

[0014] Preferably, the drying device is a drying oven.

[0015] Preferably, the filtration device is a filter press.

[0016] Due to the adoption of the above technical solution, the beneficial effects of this utility model are:

[0017] This invention first synthesizes a benzisothiazolinone-maleic anhydride adduct from benzisothiazolinone and maleic anhydride in an intermediate reaction vessel under the action of a catalyst. The adduct is then distilled and dried for later use. Acrylic resin is dissolved in xylene, and the benzisothiazolinone-maleic anhydride adduct, zinc oxide, and a catalyst are added. After the reaction is complete, the mixture is cooled and filtered to remove impurities, yielding the benzisothiazolinone zinc acrylate resin product. The grafting rate of this product is above 85%.

[0018] In summary, this utility model has a reasonable design, simple structure, convenient operation, and is easy to industrialize. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the structure of Embodiment 1 of this utility model;

[0020] In the diagram, 1 is the intermediate reaction vessel; 2 is the distillation apparatus; 3 is the drying apparatus; 4 is the main reaction vessel; 5 is the filtration apparatus; 6 is the maleic anhydride storage tank; 7 is the benzisothiazolinone storage tank; 8 is the p-toluenesulfonic acid storage tank; 9 is the xylene storage tank; 10 is the acrylic resin storage tank; 11 is the zinc oxide storage tank; 12 is the dibutyltin dilaurate storage tank; 13 is the nitrogen storage tank; and 14 is the xylene recovery tank. Detailed Implementation

[0021] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0022] Example 1:

[0023] like Figure 1 As shown, a benzisothiazolinone zinc acrylate resin production apparatus includes an intermediate reaction vessel 1, a distillation device 2, a drying device 3, a main reaction vessel 4, and a filtration device 5, which are connected in sequence by pipes (not shown), valves (not shown), and pumps (not shown). The intermediate reaction vessel 1 and the main reaction vessel 4 are each equipped with a temperature control device (not shown), a stirring device (not shown), a temperature sensor (not shown), and a nitrogen protection device (not shown). The main reaction vessel 4 is also equipped with a pH sensor (not shown) and a dripping device (not shown).

[0024] The solid inlet (not labeled) of intermediate reactor 1 is connected via pipelines to maleic anhydride storage tank 6, benzisothiazolinone storage tank 7, and p-toluenesulfonic acid storage tank 8, respectively; the liquid inlet (not labeled) is connected via pipelines to xylene storage tank 9. The solid inlet of main reactor 4 is connected via pipelines to acrylic resin storage tank 10, drying device 3, and zinc oxide storage tank 11, respectively; the liquid inlet is connected via pipelines to xylene storage tank 9, dibutyltin dilaurate storage tank 12, dilute acid storage tank (not labeled), and dilute alkali storage tank (not labeled). The nitrogen inlets (not labeled) of both intermediate reactor 1 and main reactor 4 are connected via pipelines and a gas pump (not labeled) to an external nitrogen storage tank 13. Distillation device 2 is also connected to xylene recovery tank 14.

[0025] In actual production, maleic anhydride is dissolved in xylene in intermediate reaction vessel 1 and heated to 60-80°C. Then, benzisothiazolinone powder (molar ratio of maleic anhydride to benzisothiazolinone 1:1 to 1:1.2) is slowly added and stirred for 4-6 hours. Then, a small amount of toluenesulfonic acid catalyst (0.5-1% of the mass of benzisothiazolinone) is added and the reaction continues until the acid value stabilizes (final acid value ≤50mg KOH / g). The material is then transferred to distillation device 2, where xylene is removed by distillation. The remaining material is dried in drying device 3 at 40°C for 24 hours to obtain a light yellow powder benzisothiazolinone-maleic anhydride adduct.

[0026] In the main reactor 4, acrylic resin is dissolved in xylene (mass ratio 3:7) and heated to 80-90°C. While maintaining the pH at 6.5-7.5, benzisothiazolinone-maleic anhydride adduct (5-15% of the resin solids content) is added and stirred. ZnO (molar ratio 1:1 with the carboxyl group of the benzisothiazolinone-maleic anhydride adduct) is slowly added, and the reaction is carried out for 2-3 hours. Then, dibutyltin dilaurate (0.1-0.3%) is added as a catalyst, and the reaction continues until the viscosity reaches the target (Ford cup 4, 25°C, 60-80 seconds). The material is cooled to below 40°C in the main reactor 4, and impurities are filtered out through filter 5 to obtain the finished benzisothiazolinone zinc acrylate resin.

[0027] 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 device for producing a zinc benzisothiazolinone acrylate resin, characterized by: It includes an intermediate reaction vessel, a distillation device, a drying device, a main reaction vessel, and a filtration device, which are connected in sequence by pipes, valves, and pumps; the intermediate reaction vessel and the main reaction vessel are equipped with a temperature control device, a stirring device, a temperature sensor, and a nitrogen protection device; the main reaction vessel is also equipped with a pH sensor and a dripping device.

2. The apparatus for producing a benzisothiazolinone zinc acrylate resin according to claim 1, characterized by: The intermediate reaction vessel is equipped with a solid material inlet, a liquid material inlet, a nitrogen inlet, and a gas outlet. The solid material inlet is connected to a maleic anhydride storage tank, a benzisothiazolinone storage tank, and a p-toluenesulfonic acid storage tank via pipelines. The liquid material inlet is connected to a xylene storage tank via pipelines. The nitrogen inlet is connected to an external nitrogen storage tank via pipelines and a gas pump.

3. The apparatus for producing a benzisothiazolinone zinc acrylate resin according to claim 1, characterized by: The main reactor is equipped with a solid material inlet, a liquid material inlet, a nitrogen inlet, and a gas outlet. The solid material inlet is connected to an acrylic resin storage tank, a drying device, and a zinc oxide storage tank via pipelines. The liquid material inlet is connected to a xylene storage tank and a dibutyltin dilaurate storage tank via pipelines. The nitrogen inlet is connected to an external nitrogen storage tank via pipelines and a gas pump. The main reactor is also connected to a dilute acid storage tank and a dilute alkali storage tank for adjusting pH value.

4. The apparatus for producing a benzisothiazolinone zinc acrylate resin according to claim 1, characterized by: The distillation apparatus is a vacuum distillation apparatus.

5. The apparatus for producing a benzisothiazolinone zinc acrylate resin according to claim 1, characterized by: The drying device is a drying oven.

6. The apparatus for producing a benzisothiazolinone zinc acrylate resin according to claim 1, characterized by: The filtration device is a filter press.

Images