A purification device for five bromine toluene, which is a raw material for producing poly five bromine benzyl acrylate

Abstract

The utility model discloses a kind of poly (5-bromobenzyl acrylate) production raw material five bromine toluene's purification device, it is related to poly (5-bromobenzyl acrylate) production technical field, reaction tank outlet is communicated distillation tank, can be distilled to reaction liquid, the recovery of unreacted bromine and toluene is realized;Distillation tank bottom outlet connects first filter, can separate out solid crude product five bromine toluene;Washing tank is washed to crude product in conjunction with first purified water tank, removes water-soluble impurity;Recrystallization tank and dichloroethane tank cooperate to complete recrystallization purification, improve product purity;After centrifuge separates out crystal, high-purity five bromine toluene is obtained by drying machine drying and is stored in five bromine toluene tank.The whole device realizes the automation and continuous of five bromine toluene purification, reduces manual operation error, improves production efficiency, simultaneously through the orderly link of each link, the stability of product purification effect is guaranteed.

Description

Technical Field

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

[0002] Pentabromobenzyl polyacrylate is a high-molecular-weight brominated flame retardant with a bromine content exceeding 70%. This flame retardant offers numerous advantages, such as good compatibility with the flame-retarded material, good processability, and can act as a processing aid. It enhances the weather resistance and thermal stability of flame-retardant materials, providing fatigue resistance, flexural strength, and anti-whitening properties. It also improves impact strength, gives the material excellent chemical resistance and electrical properties, and prevents frosting during use.

[0003] The production of pentabromobenzyl acrylate requires the reaction of pentabromotoluene with bromine and an initiator to obtain pentabromobenzyl bromide, which is then reacted with acrylic acid to produce pentabromobenzyl acrylate monomer. Finally, polypolymerization yields pentabromobenzyl acrylate. However, pentabromotoluene is primarily produced by reacting toluene and bromine with iron powder as a catalyst. This reaction product contains residual bromide ions and other organic impurities, directly affecting the purity of the pentabromotoluene and consequently negatively impacting the quality of the final product, pentabromobenzyl acrylate. Summary of the Invention

[0004] The technical problem to be solved by this utility model is to provide a purification device for pentabromotoluene, a raw material for the production of pentabromobenzyl polyacrylate, which improves the quality of the product, in order to address the shortcomings of the existing technology.

[0005] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:

[0006] A purification apparatus for pentabromotoluene, a raw material for the production of pentabromobenzyl polyacrylate, includes a reaction vessel. The outlet of the reaction vessel is connected to a distillation vessel via a pipeline. The top gas phase outlet of the distillation vessel is connected to a first bromine recovery vessel and a toluene recovery vessel via pipelines. The bottom outlet of the distillation vessel is connected to a first filter via a pipeline. The solid phase outlet of the first filter is connected to a washing vessel via a pipeline. The inlet of the washing vessel is connected to a first purified water vessel via a pipeline. The outlet of the washing vessel is connected to a recrystallization vessel via a pipeline. The inlet of the recrystallization vessel is connected to a dichloroethane vessel via a pipeline. The outlet of the recrystallization vessel is connected to a centrifuge via a pipeline. The solid phase outlet of the centrifuge is connected to a dryer via a pipeline. The outlet of the dryer is connected to a pentabromotoluene vessel via a pipeline.

[0007] As an improved technical solution, the top gas phase outlet of the distillation tank is connected to a monobromotoluene recovery tank, a dibromotoluene recovery tank, a tribromotoluene recovery tank, and a tetrabromotoluene recovery tank via pipelines.

[0008] As an improved technical solution, the inlet of the washing tank is connected to a sodium bisulfite solution tank via a pipe.

[0009] As an improved technical solution, the liquid phase outlet of the centrifuge is connected to a mother liquor tank via a pipeline.

[0010] As an improved technical solution, the liquid phase outlet of the first filter is connected to a precipitation tank via a pipeline, the inlet of the precipitation tank is connected to a sodium hydroxide solution tank via a pipeline, the outlet of the precipitation tank is connected to a second filter via a pipeline, and the solid phase outlet of the second filter is connected to an iron hydroxide tank via a pipeline.

[0011] As an improved technical solution, the top gas phase outlet of the reaction vessel is connected to an absorption tank via a pipeline, and the inlet of the absorption tank is connected to a second purified water tank via a pipeline.

[0012] As a preferred technical solution, the outlet of the absorption tank is connected to an oxidation tank via a pipeline, the inlet of the oxidation tank is connected to a hydrogen peroxide tank via a pipeline, the outlet of the oxidation tank is connected to a distillation kettle via a pipeline, and the top gas phase outlet of the distillation kettle is connected to a second bromine recovery tank via a pipeline.

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

[0014] This invention relates to a purification device for pentabromotoluene, a raw material for the production of pentabromobenzyl polyacrylate. The device includes a reaction vessel, the outlet of which is connected to a distillation vessel via a pipeline. The top gas phase outlet of the distillation vessel is connected to a first bromine recovery vessel and a toluene recovery vessel via pipelines. The bottom outlet of the distillation vessel is connected to a first filter via a pipeline. The solid phase outlet of the first filter is connected to a washing vessel via a pipeline. The inlet of the washing vessel is connected to a first purified water tank via a pipeline. The outlet of the washing vessel is connected to a recrystallization vessel via a pipeline. The inlet of the recrystallization vessel is connected to a dichloroethane tank via a pipeline. The outlet of the recrystallization vessel is connected to a centrifuge via a pipeline. The solid phase outlet of the centrifuge is connected to a dryer via a pipeline. The outlet of the dryer is connected to a pentabromotoluene tank via a pipeline. The reaction vessel outlet is connected to a distillation tank, allowing for distillation of the reaction solution to recover unreacted bromine and toluene. The bottom outlet of the distillation tank is connected to a first filter, separating the crude solid pentabromotoluene. A washing tank, combined with a first purified water tank, washes the crude product to remove water-soluble impurities. A recrystallization tank, working in conjunction with a dichloroethane tank, completes recrystallization purification, improving product purity. After centrifugation to separate the crystals, a dryer is used to obtain high-purity pentabromotoluene, which is then stored in a pentabromotoluene tank. The entire system achieves automated and continuous pentabromotoluene purification, reducing human error and improving production efficiency. Furthermore, the orderly connection of each stage ensures the stability of the product purification effect.

[0015] The top gas phase outlet of the distillation tank of this invention is connected via pipelines to a monobromotoluene recovery tank, a dibromotoluene recovery tank, a tribromotoluene recovery tank, and a tetrabromotoluene recovery tank. Utilizing the differences in boiling points of different bromotoluenes, intermediate products in the reaction solution can be precisely separated and individually recovered. This not only avoids waste of intermediate products and improves the comprehensive utilization rate of raw materials, reducing production costs, but also provides high-purity raw materials for the production of pentabromobenzyl polyacrylate, expanding the application range of resources, while reducing waste emissions and conforming to the concept of green production.

[0016] The inlet of the washing tank is connected to a sodium bisulfite solution tank via a pipe. The crude pentabromotoluene is washed with sodium bisulfite solution before being washed with water. Sodium bisulfite reacts with free bromine adsorbed on the surface of the crude product, effectively removing residual bromine. This avoids interference from free bromine in subsequent purification steps, prevents bromine contamination of the product, improves the purity and quality stability of pentabromotoluene, and reduces bromine corrosion of the equipment, extending its service life.

[0017] The liquid outlet of the centrifuge is connected to a mother liquor tank via a pipeline. This allows for the centralized collection of the recrystallized mother liquor. The mother liquor contains a small amount of uncrystallized pentabromotoluene and other impurities. Collecting this mother liquor allows for further processing (such as redistillation and recrystallization) to recover the pentabromotoluene, improving product yield, reducing resource waste, and facilitating the unified treatment of impurities in the mother liquor, thus reducing environmental pressure.

[0018] The liquid phase outlet of the first filter is connected to a sedimentation tank via a pipeline. The inlet of the sedimentation tank is connected to a sodium hydroxide solution tank via a pipeline. The outlet of the sedimentation tank is connected to a second filter via a pipeline. The solid phase outlet of the second filter is connected to an iron hydroxide tank via a pipeline. For the filtered liquid phase (containing spent catalyst), sodium hydroxide solution is added to cause iron ions to precipitate as iron hydroxide. After separation by the second filter, the precipitate is collected in the iron hydroxide tank. This process achieves the recovery and utilization of metal elements from the spent catalyst, turning waste into treasure, reducing solid waste treatment costs, and simultaneously reducing heavy metal ion pollution to the environment, thus improving the environmental friendliness of the production process.

[0019] The top gas outlet of the reaction vessel is connected to an absorption tank via a pipeline, and the inlet of the absorption tank is connected to a second purified water tank via a pipeline. This allows for the efficient absorption of hydrogen bromide gas generated during the reaction. Hydrogen bromide is highly soluble in water, forming a hydrobromic acid solution. This avoids the environmental pollution and harm to personnel caused by the direct emission of hydrogen bromide gas into the air, while simultaneously recovering hydrogen bromide resources, laying the foundation for the subsequent regeneration and utilization of bromine, and improving the recycling rate of bromine.

[0020] The outlet of the absorption tank is connected to an oxidation tank via a pipeline. The inlet of the oxidation tank is connected to a hydrogen peroxide tank via a pipeline. The outlet of the oxidation tank is connected to a distillation kettle via a pipeline. The top gas phase outlet of the distillation kettle is connected to a second bromine recovery tank via a pipeline. The hydrobromic acid solution produced in the absorption tank enters the oxidation tank, reacts with hydrogen peroxide to produce bromine, and is then distilled in the distillation kettle to obtain high-purity bromine, which is then recovered to the second bromine recovery tank. This achieves the conversion and recovery of hydrogen bromide to bromine, forming a closed-loop cycle of bromine, maximizing the utilization of bromine resources, significantly reducing raw material procurement costs, and simultaneously reducing the discharge of bromine-containing wastewater, further improving the economic and environmental benefits of production. Attached Figure Description

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

[0022] Figure 1 This is a structural schematic diagram of an embodiment of the present utility model;

[0023] The components are as follows: 1. Reaction vessel; 2. Distillation vessel; 3. Bromine recovery vessel; 4. Toluene recovery vessel; 5. First filter; 6. Washing vessel; 7. First purified water vessel; 8. Recrystallization vessel; 9. Dichloroethane vessel; 10. Centrifuge; 11. Dryer; 12. Pentabromotoluene vessel; 13. Monobromotoluene recovery vessel; 14. Dibromotoluene recovery vessel; 15. Tribromotoluene recovery vessel; 16. Tetrabromotoluene recovery vessel; 17. Sodium bisulfite solution vessel; 18. Mother liquor vessel; 19. Precipitation vessel; 20. Sodium hydroxide solution vessel; 21. Second filter; 22. Ferric hydroxide vessel; 23. Absorption vessel; 24. Second purified water vessel; 25. Oxidation vessel; 26. Hydrogen peroxide vessel; 27. Distillation kettle; 28. Bromine recovery vessel. Detailed Implementation

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

[0025] like Figure 1 As shown, a purification device for pentabromotoluene, a raw material for the production of pentabromobenzyl polyacrylate, includes a reaction tank 1. The outlet of the reaction tank 1 is connected to a distillation tank 2 via a pipeline. The top gas phase outlet of the distillation tank 2 is connected to a first bromine recovery tank 3 and a toluene recovery tank 4 via pipelines. The bottom outlet of the distillation tank 2 is connected to a first filter 5 via a pipeline. The solid phase outlet of the first filter 5 is connected to a washing tank 6 via a pipeline. The inlet of the washing tank 6 is connected to a first purified water tank 7 via a pipeline. The outlet of the washing tank 6 is connected to a recrystallization tank 8 via a pipeline. The inlet of the recrystallization tank 8 is connected to a dichloroethane tank 9 via a pipeline. The outlet of the recrystallization tank 8 is connected to a centrifuge 10 via a pipeline. The solid phase outlet of the centrifuge 10 is connected to a dryer 11 via a pipeline. The outlet of the dryer 11 is connected to a pentabromotoluene tank 12 via a pipeline. The outlet of reaction vessel 1 is connected to distillation vessel 2, which allows for distillation of the reaction solution to recover unreacted bromine and toluene. The bottom outlet of distillation vessel 2 is connected to a first filter 5, which separates the crude solid pentabromotoluene. Washing vessel 6, combined with a first purified water vessel 7, washes the crude product to remove water-soluble impurities. Recrystallization vessel 8, in conjunction with a dichloroethane vessel 9, completes recrystallization purification, improving product purity. After the crystals are separated by centrifuge 10, they are dried by dryer 11 to obtain high-purity pentabromotoluene, which is then stored in pentabromotoluene vessel 12. The entire device achieves automated and continuous pentabromotoluene purification, reducing human error and improving production efficiency. Furthermore, the orderly connection of each stage ensures the stability of the product purification effect.

[0026] The top gas phase outlet of distillation tank 2 is connected via pipelines to a bromotoluene recovery tank 13, a dibromotoluene recovery tank 14, a tribromotoluene recovery tank 15, and a tetrabromotoluene recovery tank 16. Utilizing the differences in boiling points of different bromotoluenes, intermediate products in the reaction solution can be precisely separated and individually recovered. This not only avoids waste of intermediate products and improves the comprehensive utilization rate of raw materials, reducing production costs, but also provides high-purity raw materials for the production of pentabromobenzyl polyacrylate, expanding the application range of resources, while reducing waste emissions, aligning with the concept of green production.

[0027] The inlet of washing tank 6 is connected to a sodium bisulfite solution tank 17 via a pipe. The crude pentabromotoluene is washed with sodium bisulfite solution before water washing. Sodium bisulfite reacts with free bromine adsorbed on the surface of the crude product, effectively removing residual bromine. This avoids interference from free bromine in subsequent purification steps, prevents bromine contamination of the product, improves the purity and quality stability of pentabromotoluene, and reduces bromine corrosion of the equipment, extending its service life.

[0028] The liquid outlet of the centrifuge 10 is connected to a mother liquor tank 18 via a pipeline. This allows for the centralized collection of the recrystallized mother liquor. The mother liquor contains a small amount of uncrystallized pentabromotoluene and other impurities. Collecting this mother liquor allows for further processing (such as redistillation and recrystallization) to recover the pentabromotoluene, improving product yield, reducing resource waste, and facilitating the unified treatment of impurities in the mother liquor, thus reducing environmental pressure.

[0029] The liquid phase outlet of the first filter 5 is connected to a sedimentation tank 19 via a pipeline. The inlet of the sedimentation tank 19 is connected to a sodium hydroxide solution tank 20 via a pipeline. The outlet of the sedimentation tank 19 is connected to a second filter 21 via a pipeline. The solid phase outlet of the second filter 21 is connected to an iron hydroxide tank 22 via a pipeline. For the filtered liquid phase (containing spent catalyst), sodium hydroxide solution is added to cause iron ions to precipitate as iron hydroxide. After separation by the second filter 21, the precipitate is collected in the iron hydroxide tank 22. This achieves the recovery and utilization of metal elements in the spent catalyst, turning waste into treasure, reducing solid waste treatment costs, and simultaneously reducing heavy metal ion pollution to the environment, thus improving the environmental friendliness of the production process.

[0030] The top gas outlet of the reaction vessel 1 is connected to an absorption vessel 23 via a pipeline, and the inlet of the absorption vessel 23 is connected to a second purified water tank 24 via a pipeline. This allows for the efficient absorption of hydrogen bromide gas generated during the reaction. Hydrogen bromide is highly soluble in water, forming a hydrobromic acid solution. This avoids the environmental pollution and harm to personnel caused by the direct emission of hydrogen bromide gas into the air, while simultaneously recovering hydrogen bromide resources, laying the foundation for the subsequent regeneration and utilization of bromine, and improving the recycling rate of bromine.

[0031] The outlet of the absorption tank 23 is connected to the oxidation tank 25 via a pipeline. The inlet of the oxidation tank 25 is connected to the hydrogen peroxide tank 26 via a pipeline. The outlet of the oxidation tank 25 is connected to the distillation kettle 27 via a pipeline. The top gas phase outlet of the distillation kettle 27 is connected to the second bromine recovery tank 28 via a pipeline. The hydrobromic acid solution produced in the absorption tank 23 enters the oxidation tank 25, reacts with hydrogen peroxide to produce bromine, and is then distilled in the distillation kettle 27 to obtain high-purity bromine, which is then recovered to the second bromine recovery tank 28. This achieves the conversion and recovery of hydrogen bromide to bromine, forming a closed-loop cycle of bromine, maximizing the utilization of bromine resources, significantly reducing raw material procurement costs, and reducing the discharge of bromine-containing wastewater, further improving the economic and environmental benefits of production.

[0032] 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 purification apparatus for pentabromotoluene, a raw material for the production of pentabromobenzyl polyacrylate, comprising a reaction vessel, characterized in that: The outlet of the reaction vessel is connected to a distillation vessel via a pipeline. The top gas phase outlet of the distillation vessel is connected to a first bromine recovery vessel and a toluene recovery vessel via pipelines. The bottom outlet of the distillation vessel is connected to a first filter via a pipeline. The solid phase outlet of the first filter is connected to a washing vessel via a pipeline. The inlet of the washing vessel is connected to a first purified water vessel via a pipeline. The outlet of the washing vessel is connected to a recrystallization vessel via a pipeline. The inlet of the recrystallization vessel is connected to a dichloroethane vessel via a pipeline. The outlet of the recrystallization vessel is connected to a centrifuge via a pipeline. The solid phase outlet of the centrifuge is connected to a dryer via a pipeline. The outlet of the dryer is connected to a pentabromotoluene vessel via a pipeline.

2. The purification apparatus for pentabromotoluene, a raw material for the production of pentabromobenzyl polyacrylate, as described in claim 1, is characterized in that: The top gas phase outlet of the distillation tank is connected to a monobromotoluene recovery tank, a dibromotoluene recovery tank, a tribromotoluene recovery tank, and a tetrabromotoluene recovery tank via pipelines.

3. The purification apparatus for pentabromotoluene, a raw material for the production of pentabromobenzyl polyacrylate, as described in claim 1, is characterized in that: The inlet of the washing tank is connected to a sodium bisulfite solution tank via a pipe.

4. The purification apparatus for pentabromotoluene, a raw material for the production of pentabromobenzyl polyacrylate, as described in claim 1, is characterized in that: The liquid phase outlet of the centrifuge is connected to a mother liquor tank via a pipeline.

5. The purification apparatus for pentabromotoluene, a raw material for the production of pentabromobenzyl polyacrylate, as described in claim 1, is characterized in that: The liquid phase outlet of the first filter is connected to a sedimentation tank via a pipeline, the inlet of the sedimentation tank is connected to a sodium hydroxide solution tank via a pipeline, the outlet of the sedimentation tank is connected to a second filter via a pipeline, and the solid phase outlet of the second filter is connected to an iron hydroxide tank via a pipeline.

6. The purification apparatus for pentabromotoluene, a raw material for the production of pentabromobenzyl polyacrylate, as described in claim 1, is characterized in that: The top gas phase outlet of the reaction vessel is connected to an absorption vessel via a pipeline, and the inlet of the absorption vessel is connected to a second purified water tank via a pipeline.

7. The purification apparatus for pentabromotoluene, a raw material for the production of pentabromobenzyl polyacrylate, as described in claim 6, is characterized in that: The outlet of the absorption tank is connected to an oxidation tank via a pipeline, the inlet of the oxidation tank is connected to a hydrogen peroxide tank via a pipeline, the outlet of the oxidation tank is connected to a distillation kettle via a pipeline, and the top gas phase outlet of the distillation kettle is connected to a second bromine recovery tank via a pipeline.

Images