Separation and purification device for producing poly-pentabromobenzyl acrylate

Abstract

The utility model discloses a kind of separating and purifying device for poly (5-bromo benzyl acrylate) production, it is related to poly (5-bromo benzyl acrylate) production technical field, material after polymerization is first removed solid impurities by first filter, then remove organic colorant, trace high molecular impurities etc. by the adsorption of activated carbon in first decoloring tank, subsequently remove activated carbon by second filter, then recover solvent in first vacuum distillation tank and obtain crude product, crude product enters heavy crystallization tank and is mixed with ethanol heavy crystallization, after crystal is separated out by suction filter tank, finished product is obtained by drying machine drying. Whole process is linked, by filtering, decoloring, distillation, heavy crystallization etc. multi-step operation, gradually remove different types of impurities, significantly improve the purity of poly (5-bromo benzyl acrylate) product, while each device is communicated by pipeline, realizes continuous operation, improves production efficiency.

Description

Technical Field

[0001] This utility model relates to the field of poly(pentabromobenzyl) acrylate production technology, specifically to a separation and purification device for the production of poly(pentabromobenzyl) acrylate. Background Technology

[0002] Pentabromobenzyl polyacrylate (PBAPO) is a highly efficient brominated flame retardant widely used in the fields of plastics, rubber, and other polymer materials. Current production processes primarily involve the esterification of acrylic acid with pentabromobenzyl alcohol, followed by polymerization of the esterified product under the action of an initiator. The final polymerized product is then filtered to obtain PBAPO. However, this process suffers from low product purity, low solvent recovery rates, and significant environmental pollution. Summary of the Invention

[0003] The technical problem to be solved by this utility model is to provide a separation and purification device for the production of pentabromobenzyl polyacrylate, which provides products with high purity and is environmentally friendly, in order to address the shortcomings of the existing technology.

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

[0005] A separation and purification apparatus for the production of pentabromobenzyl polyacrylate includes a polymerization reactor. The bottom outlet of the polymerization reactor is connected via a pipeline to a first filter. The liquid phase outlet of the first filter is connected via a pipeline to a first decolorization tank. The inlet of the first decolorization tank is connected via a pipeline to an activated carbon tank. The outlet of the first decolorization tank is connected via a pipeline to a second filter. The liquid phase outlet of the second filter is connected via a pipeline to a first vacuum distillation tank. The bottom gas phase outlet of the first vacuum distillation tank is connected via a pipeline to a recrystallization tank. The inlet of the recrystallization tank is connected via a pipeline to an ethanol tank. The outlet of the recrystallization tank is connected via a pipeline to a vacuum filtration tank. The bottom outlet of the vacuum filtration tank is connected via a pipeline to a dryer. The outlet of the dryer is connected via a pipeline to a pentabromobenzyl polyacrylate tank.

[0006] As an improved technical solution, the outlet of the second filter is connected to a second decolorizing tank via a pipeline, the inlet of the second decolorizing tank is connected to a diatomaceous earth tank via a pipeline, the outlet of the second decolorizing tank is connected to a third filter via a pipeline, and the liquid phase outlet of the third filter is connected to the first vacuum distillation tank via a pipeline.

[0007] As an improved technical solution, the top gas phase outlet of the first vacuum distillation tank is connected to a solvent recovery tank via a pipeline.

[0008] As an improved technical solution, the top outlet of the filtration tank is connected to a first ethanol recovery tank via a pipeline.

[0009] As an improved technical solution, the bottom outlet of the filtration tank is connected to a rinsing tank via a pipeline, the inlet of the rinsing tank is connected to an ice-containing anhydrous ethanol tank via a pipeline, and the outlet of the rinsing tank is connected to the dryer via a pipeline.

[0010] As an improved technical solution, the outlet of the flushing tank is connected to a second ethanol recovery tank via a pipeline.

[0011] As a preferred technical solution, the first ethanol recovery tank and the second ethanol recovery tank are respectively connected to the distillation kettle through pipelines, and the top gas phase outlet of the distillation kettle is connected to an ethanol purification tank through a pipeline.

[0012] As a preferred technical solution, the outlet of the ethanol purification tank is connected to the ethanol tank via a pipeline.

[0013] As a preferred technical solution, the bottom outlet of the distillation kettle is connected to a second vacuum distillation tank via a pipe, and the bottom outlet of the second vacuum distillation tank is connected to a concentrate tank via a pipe.

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

[0015] This utility model discloses a separation and purification device for the production of pentabromobenzyl polyacrylate, comprising a polymerization reactor, a first filter connected to the bottom outlet of the polymerization reactor via a pipeline, a first decolorization tank connected to the liquid phase outlet of the first filter via a pipeline, an activated carbon tank connected to the inlet of the first decolorization tank via a pipeline, a second filter connected to the outlet of the first decolorization tank via a pipeline, a first vacuum distillation tank connected to the liquid phase outlet of the second filter via a pipeline, a recrystallization tank connected to the bottom gas phase outlet of the first vacuum distillation tank via a pipeline, an ethanol tank connected to the inlet of the recrystallization tank via a pipeline, a vacuum filtration tank connected to the bottom outlet of the vacuum filtration tank via a pipeline, a dryer connected to the bottom outlet of the dryer via a pipeline, and a pentabromobenzyl polyacrylate tank connected to the outlet of the dryer via a pipeline. After polymerization, the material first passes through a first filter to remove solid impurities. Then, in a first decolorization tank, activated carbon adsorption removes organic pigments and trace amounts of polymeric impurities. Next, the activated carbon is removed through a second filter. The solvent is then recovered in a first vacuum distillation tank to obtain a crude product. This crude product is then mixed with ethanol in a recrystallization tank for recrystallization. After crystal separation in a vacuum filtration tank, the product is dried in a dryer to obtain the final product. The entire process is interconnected, using multiple steps such as filtration, decolorization, distillation, and recrystallization to gradually remove different types of impurities, significantly improving the purity of the pentabromobenzyl polyacrylate product. Furthermore, the interconnected systems via pipelines enable continuous operation, increasing production efficiency.

[0016] The outlet of the second filter of this invention is connected to a second decolorizing tank via a pipeline. The inlet of the second decolorizing tank is connected to a diatomaceous earth tank via a pipeline. The outlet of the second decolorizing tank is connected to a third filter via a pipeline. The liquid phase outlet of the third filter is connected to the first vacuum distillation tank via a pipeline. Diatomaceous earth has a porous structure and a large specific surface area, which can adsorb colloidal impurities not completely removed by activated carbon, some polar small molecule impurities, and trace mechanical impurities, forming a complementary adsorption effect with activated carbon. After treatment by the second decolorizing tank and the third filter, the impurity content in the material is further reduced, providing a purer raw material for subsequent vacuum distillation and recrystallization, thereby further improving the purity of the final product. Especially for applications requiring extremely high purity, this improvement can effectively meet quality requirements.

[0017] The top vapor outlet of the first vacuum distillation tank is connected to a solvent recovery tank via a pipeline. This achieves efficient recovery of environmentally friendly solvents, avoiding resource waste and environmental pollution caused by direct solvent discharge. The recovered solvent can be reused in production processes such as esterification reactions after simple treatment, reducing raw material procurement costs and minimizing the potential health impact of solvent evaporation on operators, thus aligning with the concept of green production.

[0018] The top outlet of the filtration tank is connected to a first ethanol recovery tank via a pipeline. During the separation and recrystallization of crystals, the top of the filtration tank discharges an ethanol solution containing a small amount of product and impurities, which is then collected in the first ethanol recovery tank. This not only avoids direct ethanol loss, reducing ethanol consumption and production costs, but also allows for further processing of the recovered ethanol solution to extract a small amount of non-crystallized product, improving the overall utilization rate of raw materials and reducing the environmental impact of wastewater discharge.

[0019] The bottom outlet of the filtration tank is connected to a rinsing tank via a pipe. The inlet of the rinsing tank is connected to an ice-cold anhydrous ethanol tank via a pipe, and the outlet of the rinsing tank is connected to the dryer via a pipe. The crystals obtained through filtration may have a small amount of impurities adsorbed on their surface. Introducing ice-cold anhydrous ethanol into the rinsing tank washes the crystals. The low temperature of the ice-cold anhydrous ethanol reduces dissolution loss during rinsing and effectively dissolves and removes impurities from the crystal surface. The rinsed crystals directly enter the dryer, ensuring the continuity of impurity removal, further improving product purity, and making the final product quality more stable and reliable.

[0020] The outlet of the rinsing tank is connected to a second ethanol recovery tank via a pipeline. After rinsing the crystals, the rinsing tank discharges an anhydrous ethanol solution containing impurities, which is then collected in the second ethanol recovery tank. This design achieves the recovery of ethanol used for rinsing. In conjunction with the first ethanol recovery tank, it comprehensively recovers ethanol waste generated at different stages of the production process, minimizing ethanol waste and reducing the amount of ethanol purchased. Simultaneously, it provides raw materials for subsequent ethanol purification and reuse, enhancing the economic and environmental benefits of the production process.

[0021] The first and second ethanol recovery tanks are connected to a distillation vessel via pipelines. The top vapor outlet of the distillation vessel is connected to an ethanol purification tank via a pipeline. The ethanol solution collected in the first and second ethanol recovery tanks is introduced into the distillation vessel for distillation, separating the ethanol from impurities. The ethanol vapor produced during distillation enters the ethanol purification tank for further purification, yielding ethanol with higher purity. This process achieves the regeneration and reuse of ethanol. The recovered ethanol can be reused in steps such as recrystallization, reducing the amount of new ethanol used, lowering production costs, and preventing the indiscriminate discharge of ethanol waste, thus meeting the requirements of a circular economy.

[0022] The outlet of the ethanol purification tank is connected to the ethanol tank via a pipeline. The high-purity ethanol purified in the purification tank is directly transferred to the ethanol tank, achieving a closed-loop recycling of ethanol. This eliminates the need to transport the recovered ethanol to external processing facilities for repurchase, simplifying the production process, reducing transportation costs and losses in intermediate stages, ensuring stable quality of ethanol used for recrystallization, further reducing environmental pollution, and improving the sustainability of the production process.

[0023] The bottom outlet of the distillation kettle is connected via a pipe to a second vacuum distillation tank, and the bottom outlet of the second vacuum distillation tank is connected via a pipe to a concentrate tank. The residual liquid discharged from the bottom of the distillation kettle contains a small amount of uncrystallized product and impurities. This liquid is introduced into the second vacuum distillation tank for vacuum distillation concentration, which removes some of the solvent from the residual liquid, yielding a concentrate that is collected in the concentrate tank. The concentrate contains a certain amount of product, which can be returned to the esterification reaction stage to participate in the reaction again, realizing the secondary recycling of the product, improving the overall conversion rate and utilization rate of raw materials, reducing resource waste, and minimizing material loss during the production process. Attached Figure Description

[0024] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0025] Figure 1 This is a structural schematic diagram of an embodiment of the present utility model;

[0026] The components are as follows: 1. Polymerization reactor; 2. First filter; 3. First decolorization tank; 4. Activated carbon tank; 5. Second filter; 6. First vacuum distillation tank; 7. Recrystallization tank; 8. Ethanol tank; 9. Vacuum filtration tank; 10. Dryer; 11. Pentabromobenzyl polyacrylate tank; 12. Second decolorization tank; 13. Diatomaceous earth tank; 14. Third filter; 15. Solvent recovery tank; 16. First ethanol recovery tank; 17. Washing tank; 18. Ice anhydrous ethanol tank; 19. Second ethanol recovery tank; 20. Distillation kettle; 21. Ethanol purification tank; 22. Second vacuum distillation tank; 23. Concentrate tank. Detailed Implementation

[0027] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0028] like Figure 1 As shown, a separation and purification device for the production of pentabromobenzyl polyacrylate includes a polymerization reactor 1. The bottom outlet of the polymerization reactor 1 is connected to a first filter 2 via a pipeline. The liquid phase outlet of the first filter 2 is connected to a first decolorization tank 3 via a pipeline. The inlet of the first decolorization tank 3 is connected to an activated carbon tank 4 via a pipeline. The outlet of the first decolorization tank 3 is connected to a second filter 5 via a pipeline. The liquid phase outlet of the second filter 5 is connected to a first vacuum distillation tank 6 via a pipeline. The bottom gas phase outlet of the first vacuum distillation tank 6 is connected to a recrystallization tank 7 via a pipeline. The inlet of the recrystallization tank 7 is connected to an ethanol tank 8 via a pipeline. The outlet of the recrystallization tank 7 is connected to a vacuum filtration tank 9 via a pipeline. The bottom outlet of the vacuum filtration tank 9 is connected to a dryer 10 via a pipeline. The outlet of the dryer 10 is connected to a pentabromobenzyl polyacrylate tank 11 via a pipeline. After polymerization, the material first passes through a first filter 2 to remove solid impurities. Then, it undergoes adsorption by activated carbon in a first decolorization tank 3 to remove organic pigments and trace amounts of polymeric impurities. Next, it passes through a second filter 5 to remove activated carbon. Following this, the solvent is recovered in a first vacuum distillation tank 6 to obtain a crude product. The crude product then enters a recrystallization tank 7 to be mixed with ethanol for recrystallization. After crystal separation in a suction filtration tank 9, the product is dried in a dryer 10 to obtain the final product. The entire process is interconnected, with multiple steps including filtration, decolorization, distillation, and recrystallization to gradually remove different types of impurities, significantly improving the purity of the pentabromobenzyl polyacrylate product. Furthermore, the interconnected equipment enables continuous operation, improving production efficiency.

[0029] The outlet of the second filter 5 is connected to the second decolorization tank 12 via a pipeline. The inlet of the second decolorization tank 12 is connected to the diatomaceous earth tank 13 via a pipeline. The outlet of the second decolorization tank 12 is connected to the third filter 14 via a pipeline. The liquid phase outlet of the third filter 14 is connected to the first vacuum distillation tank 6 via a pipeline. Diatomaceous earth has a porous structure and a large specific surface area, which can adsorb colloidal impurities not completely removed by activated carbon, some polar small molecule impurities, and trace mechanical impurities, forming a complementary adsorption effect with activated carbon. After treatment by the second decolorization tank 12 and the third filter 14, the impurity content in the material is further reduced, providing a purer raw material for subsequent vacuum distillation and recrystallization, thereby further improving the purity of the final product. Especially for applications requiring extremely high purity, this improvement can effectively meet quality requirements.

[0030] The top vapor outlet of the first vacuum distillation tank 6 is connected to a solvent recovery tank 15 via a pipeline. This achieves efficient recovery of environmentally friendly solvents, avoiding resource waste and environmental pollution caused by direct solvent discharge. The recovered solvent can be reused in production processes such as esterification reactions after simple treatment, reducing raw material procurement costs and minimizing the potential health impact of solvent volatilization on operators, which aligns with the concept of green production.

[0031] The top outlet of the filtration tank 9 is connected to the first ethanol recovery tank 16 via a pipeline. During the separation of recrystallized crystals, the top of the filtration tank 9 discharges an ethanol solution containing a small amount of product and impurities, which is then introduced into the first ethanol recovery tank 16 for collection. This not only avoids direct ethanol loss, reducing ethanol consumption and production costs, but also allows for further processing of the recovered ethanol solution to extract a small amount of uncrystallized product, improving the overall utilization rate of raw materials and reducing the environmental impact of wastewater discharge.

[0032] The bottom outlet of the filtration tank 9 is connected to a rinsing tank 17 via a pipe. The inlet of the rinsing tank 17 is connected to an ice-cold anhydrous ethanol tank 18 via a pipe, and the outlet of the rinsing tank 17 is connected to the dryer 10 via a pipe. The crystals obtained by filtration may have a small amount of impurities adsorbed on their surface. The rinsing tank 17 introduces ice-cold anhydrous ethanol to rinse the crystals. The low temperature of the ice-cold anhydrous ethanol reduces the dissolution loss of the crystals during rinsing, while effectively dissolving and removing impurities from the crystal surface. The rinsed crystals directly enter the dryer 10, ensuring the continuity of impurity removal, further improving the purity of the product, and making the final product quality more stable and reliable.

[0033] The outlet of the rinsing tank 17 is connected to a second ethanol recovery tank 19 via a pipeline. After rinsing the crystals, the rinsing tank 17 discharges an anhydrous ethanol solution containing impurities, which is then introduced into the second ethanol recovery tank 19 for collection. This design achieves the recovery of ethanol used for rinsing. In conjunction with the first ethanol recovery tank 16, it comprehensively recovers ethanol waste generated at different stages of the production process, minimizing ethanol waste and reducing the amount of ethanol purchased. Simultaneously, it provides raw materials for subsequent ethanol purification and reuse, enhancing the economic and environmental benefits of the production process.

[0034] The first ethanol recovery tank 16 and the second ethanol recovery tank 19 are respectively connected to a distillation vessel 20 via pipelines. The top vapor outlet of the distillation vessel 20 is connected to an ethanol purification tank 21 via a pipeline. The ethanol solution collected in the first ethanol recovery tank 16 and the second ethanol recovery tank 19 is introduced into the distillation vessel 20 for distillation, which separates the ethanol from its impurities. The ethanol vapor generated during distillation enters the ethanol purification tank 21 for further purification, yielding ethanol with higher purity. This process realizes the regeneration and reuse of ethanol. The recovered ethanol can be reused in steps such as recrystallization, reducing the amount of new ethanol used, lowering production costs, and avoiding the indiscriminate discharge of ethanol waste liquid, which is in line with the development requirements of a circular economy.

[0035] The outlet of the ethanol purification tank 21 is connected to the ethanol tank 8 via a pipeline. The high-purity ethanol purified by the ethanol purification tank 21 is directly transported to the ethanol tank 8, realizing a closed-loop recycling of ethanol. There is no need to transport the recovered ethanol to an external processing facility and then repurchase it, simplifying the production process, reducing transportation costs and losses in intermediate stages, ensuring the stable quality of the ethanol used for recrystallization, further reducing environmental pollution, and improving the sustainability of the production process.

[0036] The bottom outlet of the distillation vessel 20 is connected to a second vacuum distillation tank 22 via a pipe. The bottom outlet of the second vacuum distillation tank 22 is connected to a concentrate tank 23 via a pipe. The residual liquid discharged from the bottom of the distillation vessel 20 contains a small amount of uncrystallized product and impurities. This liquid is introduced into the second vacuum distillation tank 22 for vacuum distillation concentration, which removes some of the solvent from the residual liquid, yielding a concentrate which is collected in the concentrate tank 23. The concentrate contains a certain amount of product, which can be returned to the esterification reaction stage to participate in the reaction again, realizing the secondary recycling of the product, improving the overall conversion rate and utilization rate of raw materials, reducing resource waste, and reducing material loss during the production process.

[0037] 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 separation and purification apparatus for the production of pentabromobenzyl polyacrylate, comprising a polymerization reactor, characterized in that: The bottom outlet of the polymerization reactor is connected to a first filter via a pipeline. The liquid phase outlet of the first filter is connected to a first decolorization tank via a pipeline. The inlet of the first decolorization tank is connected to an activated carbon tank via a pipeline. The outlet of the first decolorization tank is connected to a second filter via a pipeline. The liquid phase outlet of the second filter is connected to a first vacuum distillation tank via a pipeline. The bottom gas phase outlet of the first vacuum distillation tank is connected to a recrystallization tank via a pipeline. The inlet of the recrystallization tank is connected to an ethanol tank via a pipeline. The outlet of the recrystallization tank is connected to a vacuum filtration tank via a pipeline. The bottom outlet of the vacuum filtration tank is connected to a dryer via a pipeline. The outlet of the dryer is connected to a pentabromobenzyl polyacrylate tank via a pipeline.

2. The separation and purification apparatus for the production of pentabromobenzyl polyacrylate as described in claim 1, characterized in that: The outlet of the second filter is connected to a second decolorizing tank via a pipe, the inlet of the second decolorizing tank is connected to a diatomaceous earth tank via a pipe, the outlet of the second decolorizing tank is connected to a third filter via a pipe, and the liquid phase outlet of the third filter is connected to the first vacuum distillation tank via a pipe.

3. The separation and purification apparatus for the production of pentabromobenzyl polyacrylate as described in claim 1, characterized in that: The top gas phase outlet of the first vacuum distillation vessel is connected to a solvent recovery vessel via a pipeline.

4. The separation and purification apparatus for the production of pentabromobenzyl polyacrylate as described in claim 1, characterized in that: The top outlet of the filtration tank is connected to a first ethanol recovery tank via a pipeline.

5. The separation and purification apparatus for the production of pentabromobenzyl polyacrylate as described in claim 4, characterized in that: The bottom outlet of the filtration tank is connected to a rinsing tank via a pipe, the inlet of the rinsing tank is connected to an ice-containing anhydrous ethanol tank via a pipe, and the outlet of the rinsing tank is connected to the dryer via a pipe.

6. The separation and purification apparatus for the production of pentabromobenzyl polyacrylate as described in claim 5, characterized in that: The outlet of the flushing tank is connected to a second ethanol recovery tank via a pipeline.

7. The separation and purification apparatus for the production of pentabromobenzyl polyacrylate as described in claim 6, characterized in that: The first ethanol recovery tank and the second ethanol recovery tank are respectively connected to the distillation vessel via pipelines, and the top gas phase outlet of the distillation vessel is connected to an ethanol purification tank via a pipeline.

8. The separation and purification apparatus for the production of pentabromobenzyl polyacrylate as described in claim 7, characterized in that: The outlet of the ethanol purification tank is connected to the ethanol tank via a pipeline.

9. The separation and purification apparatus for the production of pentabromobenzyl polyacrylate as described in claim 7, characterized in that: The bottom outlet of the distillation vessel is connected to a second vacuum distillation tank via a pipe, and the bottom outlet of the second vacuum distillation tank is connected to a concentrate tank via a pipe.

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