Hydrobromic acid production device

Abstract

The utility model discloses a hydrobromic acid production device, and relates to the technical field of hydrobromic acid production, an inlet of a reaction kettle is respectively communicated with a formic acid tank, a purified water tank and a bromine tank, an outlet of the reaction kettle is communicated with a heat preservation kettle through a feeding pump, and an outlet of the heat preservation kettle is communicated with a distillation kettle through a pipeline; a top gas phase outlet of the distillation kettle is communicated with a cooler through a pipeline; a material outlet of the cooler is communicated with a hydrobromic acid storage tank through a pipeline. The preparation method comprises the following steps: adding formic acid and purified water into a reaction kettle, uniformly mixing, dropwise adding bromine into the reaction kettle, and controlling the dropwise adding speed to prevent the bromine from overflowing; after the reaction is completed, reaction feed liquid enters a heat preservation kettle for heat preservation, the materials further react, finally, the reaction feed liquid enters a distillation kettle, hydrobromic acid is distilled out through distillation, and the product is obtained. The whole process is simple to operate, the raw material formic acid is easier to store compared with phosphorus and sulfur dioxide, the safety is high, no hazardous waste such as precipitate is generated, the method is environment-friendly, the treatment cost is reduced, and the economic benefit is improved.

Description

Technical Field

[0001] The utility model relates to the technical field of hydrobromic acid production, in particular to a hydrobromic acid production device. Background Technique

[0002] Hydrobromic acid is an inorganic acid widely used in organic synthesis and the electronics industry. A series of bromine series products such as monomers of nylon-11, dibromomethane, 1-bromopropane, β-bromoethylbenzene, etc. can be synthesized from it. Among them, dibromomethane, 1-bromopropane, and β-bromoethylbenzene are important organic solvents and intermediates for pesticides and pharmaceuticals.

[0003] At present, the current situation of hydrobromic acid production processes includes:

[0004] 1. Red phosphorus method: First, put red phosphorus into a reactor filled with water, and slowly add bromine while stirring to react to produce hydrobromic acid and phosphorous acid. The chemical equation is:

[0005] 3Br2 + 2P + 6H2O → 6HBr + 2H3PO3 ①

[0006] Phosphorous acid continues to react with bromine and water to produce phosphoric acid and hydrobromic acid. The chemical equation is:

[0007] Br2 + H3PO3 + H2O → 2HBr + H3PO4 ②

[0008] Combining Equation ① and Equation ②, the chemical equation is:

[0009] 5Br2 + 2P + 8H2O → 10HBr + 2H3PO4 ③

[0010] The hydrobromic acid product and the by-product phosphoric acid are obtained through sedimentation, filtration, and distillation.

[0011] 2. Sulfur dioxide method: Pass sulfur dioxide into a reaction kettle containing bromine and crushed ice, keep the temperature below 20 °C for the reaction until the solution turns yellow. Distill the mixed solution, add barium hydroxide solution to the distilled solution to react with the generated sulfuric acid to form barium sulfate precipitate. After standing and filtering to remove the precipitate, distill the filtrate to obtain the finished product of hydrobromic acid. The chemical equation for the reaction of sulfur dioxide and bromine water is:

[0012] SO2 + Br2 + 2H2O → H2SO4 + 2HBr ④

[0013] 3. Direct synthesis method of bromine and hydrogen: Bromine and hydrogen are directly synthesized into hydrogen bromide in the presence of an activated carbon catalyst or by combustion. Then, it is distilled and purified to obtain hydrogen bromide, which is absorbed by pure water to obtain hydrobromic acid. The chemical equation is:

[0014] Br2 + H2 → 2HBr ⑤

[0015] Among them, the raw material phosphorus in the red phosphorus method is prone to spontaneous combustion and difficult to store. In the sulfur dioxide method, sulfur dioxide itself is a toxic gas, which is highly harmful to humans and the environment, has great potential safety hazards in storage, and both the red phosphorus method and the sulfur dioxide method produce precipitates that are difficult to treat, causing serious environmental pollution. The synthesis of hydrogen bromide from bromine and hydrogen under the action of a catalyst is still in the theoretical research stage, and direct combustion synthesis is only carried out on a small scale. Summary of the Invention

[0016] The technical problem to be solved by the present utility model is: aiming at the deficiencies existing in the prior art, to provide a hydrogen bromide production device that does not generate hazardous waste and is environmentally friendly.

[0017] To solve the above technical problem, the technical solution of the present utility model is:

[0018] The hydrogen bromide production device includes a reaction kettle. The inlets of the reaction kettle are respectively connected to a formic acid tank, a purified water tank, and a bromine tank. The outlet of the reaction kettle is connected to a heat preservation kettle through a feeding pump. The outlet of the heat preservation kettle is connected to a distillation kettle through a pipeline. The gas-phase outlet at the top of the distillation kettle is connected to a cooler through a pipeline. The material outlet of the cooler is connected to a hydrogen bromide storage tank through a pipeline.

[0019] As an improved technical solution, the material outlet of the cooler is connected to a fore-fraction tank through a pipeline, and the outlet of the fore-fraction tank is connected to the reaction kettle through a pipeline.

[0020] As an improved technical solution, the bottom material outlet of the distillation kettle is connected to a kettle residue tank through a pipeline, and the outlet of the kettle residue tank is connected to the reaction kettle through a pipeline.

[0021] As an improved technical solution, the formic acid tank and the purified water tank are respectively connected to a mixing tank through pipelines, and the outlet of the mixing tank is connected to the reaction kettle through a pipeline.

[0022] As an improved technical solution, the outlet of the mixing tank is connected to a circulation pump, and the outlet of the circulation pump is respectively connected to the reaction kettle and the mixing tank through pipelines.

[0023] As an improved technical solution, the outlet of the circulation pump is connected to a mixer through a pipeline, and the outlet of the mixer is connected to the mixing tank through a pipeline.

[0024] As a preferred technical solution, the mixer is provided with a conical liquid inlet cavity and a liquid outlet cavity. The liquid inlet cavity is provided with a first conical head facing downward, and the liquid outlet cavity is provided with a second conical head facing upward. The first conical head is embedded in the second conical head. A mixing pipe is provided on one side of the mixer, one end of the mixing pipe extends into the outside of the joint of the first conical head and the second conical head, and the other end of the mixing pipe is connected to the outlet of the formic acid tank.

[0025] As a preferred technical solution, the outlet of the bromine tank is connected to a condenser through a pipeline, and the outlet of the condenser is connected to the reaction kettle through a pipeline.

[0026] As a preferred technical solution, an automatic regulating valve and a flow sensor are provided on the pipeline between the bromine tank and the reaction kettle, and the automatic regulating valve and the flow sensor are interlocked to a control system.

[0027] As a preferred technical solution, the outlet of the feeding pump is connected to the inlet of the reaction kettle through a pipeline.

[0028] Due to the adoption of the above technical solution, the beneficial effects of the present utility model are as follows:

[0029] A hydrobromic acid production device of the present utility model includes a reaction kettle. The inlet of the reaction kettle is respectively connected to a formic acid tank, a purified water tank and a bromine tank. The outlet of the reaction kettle is connected to a heat preservation kettle through a feeding pump. The outlet of the heat preservation kettle is connected to a distillation kettle through a pipeline. The gas-phase outlet at the top of the distillation kettle is connected to a cooler through a pipeline. The material outlet of the cooler is connected to a hydrobromic acid storage tank through a pipeline. After formic acid and purified water are added to the reaction kettle and mixed evenly, bromine is then dropped into the reaction kettle for reaction, and the dropping speed is controlled to prevent bromine from overflowing. The reaction material liquid after the reaction is fed into the heat preservation kettle for heat preservation to enable the material to further react. Finally, the reaction material liquid enters the distillation kettle, and hydrobromic acid is distilled out through distillation to obtain the product. The whole process is simple to operate, and the raw material formic acid is easier to store than phosphorus and sulfur dioxide, with high safety, no hazardous wastes such as precipitation generated, being environmentally friendly, reducing the treatment cost and improving the economic benefit.

[0030] The material outlet of the cooler of the present utility model is connected to a fore-fraction tank through a pipeline, and the outlet of the fore-fraction tank is connected to the reaction kettle through a pipeline. A small amount of bromine is contained in the material after the reaction and will be distilled out first during the distillation process. By separately collecting the bromine-containing fore-fraction, the chromaticity of the product is improved, the quality of the product is higher, and at the same time, the obtained fore-fraction can be recycled back to the reaction kettle for reaction, improving the yield of the product.

[0031] The bottom material outlet of the distillation kettle is provided with a kettle residue tank through a pipeline, and the outlet of the kettle residue tank is connected to the reaction kettle through a pipeline. A small amount of hydrobromic acid and formic acid are contained in the distillation kettle residue. Recycling it back to the reaction kettle can avoid waste of raw materials and improve the yield of the product.

[0032] The formic acid tank and the purified water tank are respectively connected to the mixing tank through pipelines, and the outlet of the mixing tank is connected to the reaction kettle through a pipeline. By pre-mixing formic acid and purified water in the mixing tank and then entering the reaction kettle to react with bromine, the mixing and contact effect between the materials is better, the reaction is more complete, and the yield of the product is high.

[0033] A circulation pump is connected to the outlet of the mixing tank, and the outlet of the circulation pump is respectively connected to the reaction kettle and the mixing tank through pipelines. By forcing the external circulation of the materials in the mixing tank by the circulation pump, the mixing effect of formic acid and purified water is better, and the mixing time is shortened.

[0034] A mixer is connected to the outlet of the circulation pump through a pipeline, and the outlet of the mixer is connected to the mixing tank through a pipeline. The materials that are not easily stirred at the bottom of the mixing tank are transported to the mixer through the circulation pump for forced mixing and finally enter the mixing tank, shortening the mixing time of the materials in the mixing tank and achieving a better mixing effect.

[0035] The mixer is provided with a conical liquid inlet cavity and a liquid outlet cavity. The liquid inlet cavity is provided with a first conical head facing downwards, the liquid outlet cavity is provided with a second conical head facing upwards, the first conical head is embedded in the second conical head, and a mixing pipe is provided on one side of the mixer passing through. One end of the mixing pipe extends to the outside of the joint of the first conical head and the second conical head, and the other end of the mixing pipe is connected to the outlet of the formic acid tank. Purified water is pre-put into the mixing tank, and then the circulation pump is started. The materials in the mixing tank enter from the liquid inlet cavity of the mixer under the action of the circulation pump, generating negative pressure at the outlet of the first conical head. Under the action of the negative pressure, formic acid is sucked into the mixer, and the purified water and formic acid are mixed while flowing out from the liquid outlet cavity and entering the mixing tank, increasing the mixing effect of formic acid and purified water and shortening the mixing time.

[0036] The outlet of the bromine tank is connected to a condenser through a pipeline, and the outlet of the condenser is connected to the reaction kettle through a pipeline. By cooling the bromine entering the reaction kettle through the condenser, the increase in side reactions or the decrease in the main reaction efficiency that may occur under high-temperature conditions can be avoided.

[0037] An automatic regulating valve and a flow sensor are provided on the pipeline between the bromine tank and the reaction kettle, and the automatic regulating valve and the flow sensor are interlocked to the control system. The control system controls the opening degree of the automatic regulating valve according to the value of the flow sensor to keep the bromine added at a stable speed, preventing the overflow of bromine and the occurrence of side reactions caused by too fast reaction.

[0038] The outlet of the feeding pump is connected to the inlet of the reaction kettle through a pipeline, and the external circulation is maintained during the reaction process, and the mixing and reaction effect of the materials is better. Description of the Drawings

[0039] The present utility model will be further described below in conjunction with the accompanying drawings and embodiments.

[0040] Figure 1 is a schematic structural diagram of an embodiment of the present utility model;

[0041] Figure 2 is Figure 1 a schematic structural diagram of the mixer in

[0042] Wherein: 1, reaction kettle; 2, formic acid tank; 3, purified water tank; 4, bromine tank; 5, feeding pump; 6, heat preservation kettle; 7, distillation kettle; 8, cooler; 9, hydrobromic acid storage tank; 10, pre-fraction tank; 11, mixing tank; 12, circulation pump; 13, mixer; 14, liquid inlet chamber; 15, liquid outlet chamber; 16, first cone head; 17, second cone head; 18, mixing pipe; 19, condenser; 20, automatic regulating valve; 21, flow sensor; 22, residue tank; 23, reflux cooling device. Specific embodiments

[0043] The present utility model will be further elaborated below in conjunction with the accompanying drawings and embodiments.

[0044] As Figure 1-2 shown, a hydrobromic acid production device includes a reaction kettle 1. The inlets of the reaction kettle 1 are respectively connected to a formic acid tank 2, a purified water tank 3, and a bromine tank 4. The outlet of the reaction kettle 1 is connected to a heat preservation kettle 6 through a feeding pump 5. The outlet of the heat preservation kettle 6 is connected to a distillation kettle 7 through a pipeline. The gas-phase outlet at the top of the distillation kettle 7 is connected to a cooler 8 through a pipeline. The material outlet of the cooler 8 is connected to a hydrobromic acid storage tank 9 through a pipeline. During the discharge process of carbon dioxide generated by the reaction, a small amount of bromine vapor will be carried away. By adding a reflux cooling device 23 to the exhaust pipeline, the discharged carbon dioxide is cooled, and the bromine vapor is condensed and then flows back into the reaction kettle 1 for reaction, avoiding waste of raw materials and environmental pollution. After formic acid and purified water are added to the reaction kettle 1 and mixed evenly, bromine is then dropped into the reaction kettle 1 for reaction, and the dropping speed is controlled to prevent bromine from overflowing. The reaction material liquid after the reaction enters the heat preservation kettle 6 for heat preservation to enable the material to further react. Finally, the reaction material liquid enters the distillation kettle 7, and hydrobromic acid is distilled out through distillation to obtain the product. The whole process is simple to operate, and the raw material formic acid is easier to store than phosphorus and sulfur dioxide, with high safety, no hazardous waste such as precipitation generated, being environmentally friendly, reducing the treatment cost, and improving the economic benefit.

[0045] The material outlet of the cooler 8 is connected to the pre-fraction tank 10 through a pipeline, and the outlet of the pre-fraction tank 10 is connected to the reaction kettle 1 through a pipeline. A small amount of bromine is contained in the post-reaction material, which will be distilled out first during the distillation process. By separately collecting the pre-fraction containing bromine, the chromaticity of the product is improved, and the quality of the product is higher. At the same time, the obtained pre-fraction can be recycled back to the reaction kettle 1 for reaction, improving the yield of the product.

[0046] The bottom material outlet of the distillation kettle 7 is connected to the residue tank 22 through a pipeline, and the outlet of the residue tank 22 is connected to the reaction kettle 1 through a pipeline. A small amount of hydrobromic acid and formic acid are contained in the residue of the distillation kettle 7. Recycling it back to the reaction kettle 1 can avoid waste of raw materials and improve the yield of the product.

[0047] The formic acid tank 2 and the purified water tank 3 are respectively connected to the mixing tank 11 through pipelines, and the outlet of the mixing tank 11 is connected to the reaction kettle 1 through a pipeline. The formic acid and purified water are pre-mixed in the mixing tank 11 and then enter the reaction kettle 1 to react with bromine. The mixing and contact effect between the materials is better, the reaction is more complete, and the yield of the product is high.

[0048] The outlet of the mixing tank 11 is connected to a circulation pump 12, and the outlet of the circulation pump 12 is respectively connected to the reaction kettle 1 and the mixing tank 11 through pipelines. The materials in the mixing tank 11 are forced to circulate externally through the circulation pump 12, and the mixing effect of formic acid and purified water is better, shortening the mixing time.

[0049] The outlet of the circulation pump 12 is connected to a mixer 13 through a pipeline, and the outlet of the mixer 13 is connected to the mixing tank 11 through a pipeline. The materials at the bottom of the mixing tank 11 that are not easily stirred are transported to the mixer 13 through the circulation pump 12 for forced mixing and finally enter the mixing tank 11, shortening the mixing time of the materials in the mixing tank 11 and having a better mixing effect.

[0050] The mixer 13 is provided with a conical liquid inlet chamber 14 and a liquid outlet chamber 15. The liquid inlet chamber 14 is provided with a first conical head 16 facing downward, and the liquid outlet chamber 15 is provided with a second conical head 17 facing upward. The first conical head 16 is embedded in the second conical head 17. A mixing pipe 18 is provided on one side of the mixer 13. One end of the mixing pipe 18 extends into the outside of the joint of the first conical head 16 and the second conical head 17, and the other end of the mixing pipe 18 is connected to the outlet of the formic acid tank 2. Purified water is pre-injected into the mixing tank 11, and then the circulation pump 12 is started. The materials in the mixing tank 11 enter from the liquid inlet chamber 14 of the mixer 13 under the action of the circulation pump 12, and a negative pressure is generated at the outlet of the first conical head 16. Under the action of the negative pressure, formic acid is sucked into the mixer 13, and the purified water and formic acid flow out from the liquid outlet chamber 15 while mixing and enter the mixing tank 11, which increases the mixing effect of formic acid and purified water and shortens the mixing time.

[0051] The outlet of the bromine tank 4 is connected to a condenser 19 through a pipeline, and the outlet of the condenser 19 is connected to the reactor 1 through a pipeline. The bromine entering the reactor 1 is cooled by the condenser 19 to avoid an increase in side reactions or a decrease in the main reaction efficiency that may occur under high-temperature conditions.

[0052] An automatic regulating valve 20 and a flow sensor 21 are provided on the pipeline between the bromine tank 4 and the reactor 1, and the automatic regulating valve 20 and the flow sensor 21 are interlocked to a control system. The control system controls the opening of the automatic regulating valve 20 according to the value of the flow sensor 21 to keep the bromine added at a stable speed, preventing the overflow of bromine and the occurrence of side reactions caused by too fast a reaction.

[0053] The outlet of the feeding pump 5 is connected to the inlet of the reactor 1 through a pipeline, and an external circulation is maintained during the reaction process, and the mixing and reaction effect of the materials is better.

[0054] It should be understood that these embodiments are only used to illustrate the present invention and not to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of this application.

Claims

1. A hydrobromic acid production device, characterized in that: The invention comprises a reactor, the inlet of which is respectively connected with a formic acid tank, a purified water tank and a bromine tank, the outlet of which is connected with an insulation kettle via a feed pump, the outlet of which is connected with a distillation kettle via a pipeline, the top gas phase outlet of the distillation kettle is connected with a cooler via a pipeline, and the material outlet of the cooler is connected with a hydrobromic acid storage tank via a pipeline.

2. The hydrobromic acid production device according to claim 1, wherein: The material outlet of the cooler is connected to the fore fraction tank through a pipeline, and the outlet of the fore fraction tank is connected to the reactor through a pipeline.

3. The hydrobromic acid production device according to claim 1, characterized in that: The bottom material outlet of the distillation kettle is connected to the kettle residue tank through a pipeline, and the outlet of the kettle residue tank is connected to the reaction kettle through a pipeline.

4. The hydrobromic acid production device according to claim 1, wherein: The formic acid tank and the purified water tank are respectively connected to a mixing tank through pipelines, and an outlet of the mixing tank is connected to the reactor through a pipeline.

5. The hydrobromic acid production device according to claim 4, characterized in that: The outlet of the mixing tank is connected to a circulation pump, and the outlet of the circulation pump is connected to the reactor and the mixing tank through pipelines respectively.

6. The hydrobromic acid production device according to claim 5, characterized in that: The outlet of the circulation pump is connected to a mixer through a pipeline, and the outlet of the mixer is connected to the mixing tank through a pipeline.

7. The hydrobromic acid production device according to claim 6, characterized in that: The mixer is provided with a conical liquid inlet chamber and a liquid outlet chamber, the liquid inlet chamber is provided with a first cone head facing downward, the liquid outlet chamber is provided with a second cone head facing upward, the first cone head is embedded in the second cone head, a mixing tube is provided on one side of the mixer, one end of the mixing tube extends into the outside of the joint between the first cone head and the second cone head, and the other end of the mixing tube is connected to the outlet of the formic acid tank.

8. The hydrobromic acid production device according to claim 1, characterized in that: The outlet of the bromine tank is connected to a condenser through a pipeline, and the outlet of the condenser is connected to the reactor through a pipeline.

9. The hydrobromic acid production device according to claim 1, characterized in that: An automatic regulating valve and a flow sensor are arranged on the pipeline between the bromine tank and the reactor, and the automatic regulating valve and the flow sensor are interlocked to a control system.

10. The hydrobromic acid production device according to claim 1, characterized in that: The outlet of the feed pump is connected to the inlet of the reactor through a pipeline.

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