Separation system for bromide

Abstract

The utility model discloses a separation system for bromides, which belongs to the technical field of bromide production and comprises a reaction kettle, a solid-liquid separator connected to a discharge port of the reaction kettle, a bromine extractor connected to the top of the solid-liquid separator, a liquid phase separator connected to a liquid outlet of the bromine extractor, a bromine outlet arranged at the bottom of the liquid phase separator, and a bromine outlet arranged at the bottom of the liquid phase separator. A water phase outlet in the top of the liquid phase separator is respectively connected with a liquid discharge pipeline and a hydrogen peroxide oxidizer through pipelines, a gas outlet is formed in the top of the hydrogen peroxide oxidizer, a liquid outlet is formed in the bottom of the hydrogen peroxide oxidizer, and the liquid outlet of the hydrogen peroxide oxidizer is communicated with the top of the bromine extractor; an air inlet of the air blower is communicated with the top of the hydrogen peroxide oxidizer, and an air outlet of the air blower is connected with a bromine recovery tank. According to the utility model, bromine in the waste liquid is separated out before oxidation, and bromine gas generated by oxidation is taken away by arranging the air blower, so that side reactions in the hydrogen peroxide oxidizer are reduced, and the recovery rate of the bromine in the waste liquid is improved.

Description

Technical Field

[0001] This utility model relates to the field of bromide production technology, specifically to a bromide separation system. Background Technology

[0002] Bromination is a reaction in which hydrogen atoms in an organic compound molecule are replaced by bromine to form a bromine-containing compound. Bromine, as a commonly used brominating agent, is widely used in high-efficiency flame retardants, refrigerants, petroleum finishing fluids, pharmaceuticals, fuel intermediates, and chemical reagents. After the reaction, the products are separated from the waste liquid through solid-liquid separation. However, some unreacted bromine is discharged with the waste liquid after the reaction, resulting in waste of bromine and environmental impact. Furthermore, the waste liquid also contains some bromide ions.

[0003] Existing technologies mostly utilize the reaction of hydrogen peroxide with bromide ions to extract bromine from waste liquid. However, there are side reactions in the process of hydrogen peroxide reacting with bromide ions to generate bromine. Bromine in the reaction system will react with hydrogen peroxide to generate bromide ions, thereby reducing the amount of bromine recovered.

[0004] Bromine is a highly volatile liquid. The reaction between hydrogen peroxide and bromide ions is exothermic, which causes the bromine in the reaction system to volatilize into a gas. Current technology extracts bromine from the organic phase and recovers the bromine from the waste liquid through multiple fractionation, but ignores the gaseous bromine.

[0005] In view of the problems existing in the prior art, this utility model combines years of design and use experience in related fields to design and manufacture a bromide separation system to overcome the above defects. Utility Model Content

[0006] To address the problems existing in the prior art, this utility model provides a separation system for bromides that separates the product from the waste liquid after the bromide reaction is completed, and recycles the bromine in the waste liquid, thereby reducing the occurrence of side reactions between hydrogen peroxide and bromine and improving the bromine recovery rate.

[0007] To achieve the above objectives, the technical solution adopted by this utility model is as follows: A bromide separation system includes a reaction vessel, a solid-liquid separator connected to the bottom outlet of the reaction vessel, a bromine extractor connected to the top of the solid-liquid separator, the bromine extractor being used to extract bromine from waste liquid into an organic solvent, a liquid phase separator connected to the bottom outlet of the bromine extractor, a bromine outlet at the bottom of the liquid phase separator, an aqueous phase outlet at the top of the liquid phase separator, a liquid discharge pipe and a hydrogen peroxide oxidizer connected to the aqueous phase outlet of the liquid phase separator respectively via pipes, a gas outlet at the top of the hydrogen peroxide oxidizer, a liquid outlet at the bottom of the hydrogen peroxide oxidizer, and the liquid outlet of the hydrogen peroxide oxidizer communicating with the top of the bromine extractor;

[0008] A blower, the air inlet of which is connected to the gas outlet at the top of the hydrogen peroxide oxidizer, and the air outlet of which is connected to a bromine recovery tank.

[0009] Preferably, the top of the bromine extractor is connected to an organic solvent storage tank via an organic solvent inlet.

[0010] Preferably, the organic solvent storage tank is provided with a non-polar organic solvent.

[0011] Preferably, the top of the hydrogen peroxide oxidizer is connected to a hydrogen peroxide storage tank via a hydrogen peroxide inlet.

[0012] Preferably, the blower's outlet is connected to a water removal tank, and the blower is connected to the bromine recovery tank through the water removal tank.

[0013] Preferably, both the liquid phase separator and the hydrogen peroxide oxidizer are equipped with cooling jackets.

[0014] Preferably, the top of the reactor is provided with a gas phase outlet and a liquid inlet, the gas phase outlet of the reactor is connected to a condenser, and the outlet end of the condenser is connected to the liquid inlet of the reactor.

[0015] Preferably, the water removal tank is equipped with phosphorus pentoxide.

[0016] Preferably, both the bromine extractor and the hydrogen peroxide oxidizer are equipped with stirring components.

[0017] Preferably, the stirring component includes a motor, the output end of which is connected to a rotating rod. The rotating rod is vertically arranged, and the lower ends of the two rotating rods respectively penetrate the top of the bromine extractor and the hydrogen peroxide oxidizer. The two rotating rods are rotatably connected to the bromine extractor and the hydrogen peroxide oxidizer respectively.

[0018] The rotating rod is equipped with several stirring rods, which are located inside the bromine extractor and the hydrogen peroxide oxidizer, respectively.

[0019] The advantages of this utility model are:

[0020] 1. This utility model separates bromine from the waste liquid before oxidation by installing a bromine extractor and a liquid phase separator before the hydrogen peroxide oxidizer, thus avoiding side reactions between the bromine in the waste liquid and hydrogen peroxide. By installing a blower to carry away the bromine gas generated during oxidation in the hydrogen peroxide oxidizer, the volatilization of bromine in the solution is promoted, and the reaction between hydrogen peroxide and bromide ions is also promoted, thereby reducing the occurrence of side reactions in the hydrogen peroxide oxidizer and improving the recovery rate of bromine in the waste liquid.

[0021] 2. This utility model absorbs water carried in bromine gas by removing phosphorus pentoxide in the water removal tank, and the bromine carried away by the blower is purified by water removal and then recycled back to the bromine recovery tank, thereby improving the purity of bromine. Attached Figure Description

[0022] Figure 1 This is a schematic diagram of a bromide separation system.

[0023] In the diagram: 1-Reaction vessel, 2-Solid-liquid separator, 3-Bromine extractor, 4-Organic solvent storage tank, 5-Liquid phase separator, 6-Hydrogen peroxide oxidizer, 7-Blower, 8-Water removal tank, 9-Bromine recovery tank, 10-Liquid discharge pipe, 11-Hydrogen peroxide storage tank, 12-Motor, 13-Rotating rod, 14-Stirring rod, 15-Three-way valve, 16-Condenser. Detailed Implementation

[0024] To facilitate understanding by those skilled in the art, the present invention will be further described below with reference to the accompanying drawings.

[0025] like Figure 1 As shown, a bromide separation system includes a reaction vessel 1. A solid-liquid separator 2 is connected to the outlet at the bottom of the reaction vessel 1. The solid-liquid separator 2 has a liquid outlet at the top and a solid outlet at the bottom. The liquid outlet at the top of the solid-liquid separator 2 is connected to a bromine extractor 3, which extracts bromine from waste liquid into an organic solvent. The bromine extractor 3 has a liquid outlet at the bottom, which is connected to a liquid phase separator 5. The liquid phase separator 5 has a bromine outlet at the bottom and an aqueous phase outlet at the top. The aqueous phase outlet of the liquid phase separator 5 is connected to a liquid discharge pipe 10 and a hydrogen peroxide oxidizer 6 via pipes. Specifically, the aqueous phase outlet of the liquid phase separator 5 is connected to both the liquid discharge pipe 10 and the hydrogen peroxide oxidizer 6 via a three-way valve 15 on the pipe.

[0026] This invention first utilizes the principle of "like dissolves like" to extract bromine from the waste liquid into an organic solvent using a bromine extractor 3, and then separates the bromine by separating the aqueous and organic phases. Next, the waste liquid containing bromide ions is passed into a hydrogen peroxide oxidizer 6 to prevent side reactions between the bromine in the waste liquid and hydrogen peroxide. Finally, the bromine is separated from the organic phase through multiple fractionation processes.

[0027] The top of the hydrogen peroxide oxidizer 6 is connected to a hydrogen peroxide storage tank 11 via a hydrogen peroxide inlet. The top of the hydrogen peroxide oxidizer 6 has a gas outlet, and the bottom of the hydrogen peroxide oxidizer 6 has a liquid outlet. The liquid outlet of the hydrogen peroxide oxidizer 6 is connected to the top of the bromine extractor 3. A blower 7 has its air inlet connected to the gas outlet at the top of the hydrogen peroxide oxidizer 6, and its air outlet connected to a bromine recovery tank 9.

[0028] Since the reaction is exothermic and bromine is a volatile liquid, some bromine will evaporate into gas. This invention uses a blower 7 to extract the gaseous bromine from the hydrogen peroxide oxidizer 6. This serves two purposes: firstly, it allows for the recovery and reuse of the gaseous bromine, avoiding direct discharge that could harm the environment; secondly, by continuously extracting the gaseous bromine, it promotes the evaporation of bromine from the solution, thereby accelerating the reaction between hydrogen peroxide and bromide ions, reducing side reactions between hydrogen peroxide and bromine, and increasing the recovery rate of bromine in the wastewater. After the reaction between bromide ions and hydrogen peroxide in the wastewater is complete, the wastewater enters the bromine extractor 3 to extract bromine. In the liquid phase separator 5, the aqueous phase and the bromine-containing organic phase separate. The lower layer of bromine-containing organic phase is discharged and then subjected to multiple fractionation to separate the bromine for recovery. Finally, the bromine-free wastewater is discharged through the liquid discharge pipe 10.

[0029] The reactor 1 has a gas phase outlet and a liquid inlet at the top. The gas phase outlet of the reactor 1 is connected to a condenser 16, and the outlet of the condenser 16 is connected to the liquid inlet of the reactor 1. Specifically, the condenser 16 is preferably a two-stage tube condenser connected in series. The bromine is condensed by the condenser 16 to achieve efficient bromine reflux.

[0030] The top of the bromine extractor 3 is connected to an organic solvent storage tank 4 via an organic solvent inlet. The organic solvent storage tank 4 contains a non-polar organic solvent. Both the bromine extractor 3 and the hydrogen peroxide oxidizer 6 are equipped with stirring components, including a motor 12. The output end of the motor 12 is connected to a rotating rod 13, which is vertically positioned. The lower ends of the two rotating rods 13 penetrate the tops of the bromine extractor 3 and the hydrogen peroxide oxidizer 6, respectively, and are rotatably connected to them. Several stirring rods 14 are mounted on the rotating rods 13, and these stirring rods 14 are located within the bromine extractor 3 and the hydrogen peroxide oxidizer 6.

[0031] Specifically, bromine is more soluble in nonpolar organic solvents than in water, and bromide ions are insoluble in nonpolar organic solvents, thus extracting bromine into the organic phase. A stirring component is installed in the bromine extractor 3 to facilitate faster and more complete entry of bromine from the waste liquid into the organic solvent. A stirring component is also installed in the hydrogen peroxide oxidizer 6 to accelerate the oxidation reaction and ensure complete reaction.

[0032] The blower 7 has a water removal tank 8 connected to its outlet. The blower 7 is connected to the bromine recovery tank 9 via the water removal tank 8, which contains phosphorus pentoxide. Both the liquid phase separator 5 and the hydrogen peroxide oxidizer 6 are equipped with cooling jackets.

[0033] In this invention, the gaseous bromine carried by the blower 7 contains some water, which is removed by phosphorus pentoxide before the bromine is recovered. A cooling jacket is installed outside the liquid phase separator 5 to lower the temperature of the solution inside, reducing the solubility of bromine in water and effectively improving the bromine extraction efficiency. The oxidation reaction releases a large amount of heat; the cooling jacket accelerates the heat release from the hydrogen peroxide oxidizer 6, preventing excessive temperature.

[0034] Detailed operation process

[0035] After the reaction in reactor 1 is completed, the material is fed into solid-liquid separator 2 for solid-liquid separation. The solid product is discharged from the bottom outlet of solid-liquid separator 2, and the liquid layer is bromine-containing waste liquid, which enters bromine extractor 3 from the outlet of solid-liquid separator 2. Carbon tetrachloride organic solvent is added to bromine extractor 3 through organic solvent storage tank 4, and motor 12 on bromine extractor 3 is started. Stirring rod 14 and rotating rod 13 rotate and thoroughly stir the bromine-containing waste liquid and carbon tetrachloride, extracting bromine into carbon tetrachloride. Then, the liquid in bromine extractor 3 is discharged into liquid phase separator 5 and allowed to stand. The aqueous phase and carbon tetrachloride phase separate into layers, with the upper layer being the aqueous phase and the lower layer being the carbon tetrachloride phase.

[0036] Open the connection between the water phase outlet of the liquid phase separator 5 in the three-way valve 15 and the hydrogen peroxide oxidizer 6. Separate the upper water phase from the upper part of the liquid phase separator 5 and discharge it into the hydrogen peroxide oxidizer 6. Start the motor 12 on the hydrogen peroxide oxidizer 6. The motor 12 drives the stirring rod 14 and the rotating rod 13 to rotate. Hydrogen peroxide is introduced into the hydrogen peroxide oxidizer 6 through the hydrogen peroxide storage tank 11. The stirring component stirs the bromine-containing water phase and hydrogen peroxide. The hydrogen peroxide reacts with bromide ions to generate bromine and water. After the reaction has been going on for a period of time, start the blower 7. The blower 7 extracts the bromine gas in the hydrogen peroxide oxidizer 6 and discharges it into the dewatering tank 8. After being dehydrated by phosphorus pentoxide in the dewatering tank 8, it enters the bromine recovery tank 9 for recovery.

[0037] After the oxidation reaction is complete, the liquid in the hydrogen peroxide oxidizer 6 is discharged into the bromine extractor 3. Carbon tetrachloride is added to the bromine extractor 3 to extract bromine, and the aqueous phase and carbon tetrachloride phase separate into layers. Then, the liquid in the bromine extractor 3 is discharged into the liquid phase separator 5 and allowed to stand. Then, the two portions of carbon tetrachloride are mixed and separated into layers with the aqueous phase. The aqueous phase is a bromine-free waste liquid. The connection between the water tank outlet of the liquid phase separator 5 and the liquid discharge pipe 10 in the three-way valve 15 is opened to discharge the bromine-free waste liquid. The lower carbon tetrachloride phase undergoes multiple fractionation to separate bromine, and the separated bromine enters the bromine recovery tank 9 for recovery.

[0038] It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of protection of this utility model. Furthermore, it should be understood that after reading the technical description of this utility model, those skilled in the art can make various alterations, modifications, and / or variations to this utility model, and all such equivalent forms also fall within the scope of protection defined by the appended claims.

Claims

1. A bromide separation system characterized by, The utility model relates to a kind of bromine extraction device, including reactor (1), the outlet of the bottom of the reactor (1) is connected with solid-liquid separator (2), the top of the solid-liquid separator (2) is connected with bromine extractor (3), the bromine extractor (3) is used to extract bromine in waste liquid into organic solvent, the outlet of the bottom of the bromine extractor (3) is connected with liquid phase separator (5), the bottom of the liquid phase separator (5) is equipped with bromine outlet, the top of the liquid phase separator (5) is equipped with water phase outlet, the water phase outlet of the liquid phase separator (5) is connected with liquid discharge pipeline (10) and hydrogen peroxide oxidizer (6) respectively by pipeline, the top of the hydrogen peroxide oxidizer (6) is equipped with gas outlet, the bottom of the hydrogen peroxide oxidizer (6) is equipped with outlet, the outlet of the hydrogen peroxide oxidizer (6) is communicated with the top of the bromine extractor (3); Blower (7), the air inlet of the blower (7) is communicated with the gas outlet of the top of the hydrogen peroxide oxidizer (6), the air outlet of the blower (7) is connected with bromine recovery tank (9).

2. A separation system for bromide according to claim 1, characterized in that, The top of the bromine extractor (3) is connected with organic solvent storage tank (4) by organic solvent inlet.

3. A separation system for bromide according to claim 2, characterized in that, Nonpolar organic solvent is arranged in the organic solvent storage tank (4).

4. A separation system for bromide according to claim 1, characterized in that, The top of the hydrogen peroxide oxidizer (6) is connected with hydrogen peroxide storage tank (11) by hydrogen peroxide inlet.

5. A separation system for bromide according to claim 1, characterized in that, The air outlet of the blower (7) is connected with water removal tank (8), and the blower (7) is connected with the bromine recovery tank (9) through the water removal tank (8).

6. A separation system for bromide according to claim 1, characterized in that, Cooling jacket is equipped on the liquid phase separator (5) and the hydrogen peroxide oxidizer (6).

7. A separation system for bromide according to claim 1, characterized in that, Gas phase outlet and liquid inlet are equipped on the top of the reactor (1), and the gas phase outlet of the reactor (1) is connected with condenser (16), and the outlet end of the condenser (16) is connected with the liquid inlet of the reactor (1).

8. A separation system for bromide according to claim 5, characterized in that, Phosphorus pentoxide is arranged in the water removal tank (8).

9. A separation system for bromide according to claim 1, characterized in that, Stirring parts are arranged in the bromine extractor (3) and the hydrogen peroxide oxidizer (6).

10. A separation system for bromide according to claim 9, characterized in that, The stirring parts include motor (12), the output end of the motor (12) is connected with rotating rod (13), the rotating rod (13) is vertically arranged, the lower end of two rotating rods (13) penetrates the top of the bromine extractor (3) and the hydrogen peroxide oxidizer (6) respectively, and the rotating rod (13) is rotatably connected with the bromine extractor (3) and the hydrogen peroxide oxidizer (6) respectively. A plurality of stirring rods (14) are arranged on the rotating rod (13), and the stirring rods (14) are arranged in the bromine extractor (3) and the hydrogen peroxide oxidizer (6) respectively.

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