Iron-method iron phosphate iron dissolving device and iron phosphate production device
By adding water vapor and condenser separation technology to the iron iron phosphate dissolved device, the problems of hydrogen emission safety risks and lengthy processes are solved, efficient and stable iron phosphate production is achieved, and product quality and production efficiency are improved.
Patent Information
- Application Number
- CN202421784876.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-26
- Publication Date
- 2025-06-24
- Estimated Expiration
- 2034-07-26
AI Technical Summary
In the production process of lithium iron phosphate, when high-purity iron blocks or iron powder react with high-purity purified phosphoric acid in the iron method iron phosphate process, a large amount of hydrogen is generated, resulting in safety risks, and the iron purification device process is lengthy, affecting the product quality stability.
By adding water vapor to the iron iron phosphate dissolved device of iron method, a micro negative pressure state is formed, hydrogen and water vapor are discharged through the exhaust pipe, separated by a condenser, and hydrogen is recovered, which solves the problem of hydrogen emission. At the same time, the circulation operation is used to ensure uniform mixing and continuous flow of the material liquid, improving production efficiency and product quality.
It effectively solves the safety risks of hydrogen emissions, simplifies production processes, improves the quality stability of iron phosphate products, and reduces energy consumption.
Smart Images
Figure CN223010518U_ABST
Abstract
Description
Technical Field
[0001] This application relates to the technical field of iron phosphate production, and in particular to an iron dissolution device for iron phosphate by the iron method and an iron phosphate production device. Background Art
[0002] With the gradual saturation of the lithium iron phosphate market, lithium iron phosphate continues to develop towards the direction of low cost, high density, high purity, and high compaction density. The iron method iron phosphate process with a relatively high compaction density and low wastewater treatment cost has gradually attracted attention. Different from the ammonium method iron phosphate process that uses industrial monoammonium phosphate and ferrous sulfate as raw materials, the iron method process uses high-purity iron blocks or iron powder as raw materials to react with high-purity purified phosphoric acid, and then oxidizes with hydrogen peroxide. During the production process, only phosphorus-containing wastewater needs to be treated, and there is no discharge of waste such as ammonium sulfate in the ammonium method process. Moreover, the discharged phosphorus-containing wastewater can be used as raw materials in phosphate chemical enterprises to be recycled and processed into by-products such as phosphate fertilizers. Therefore, traditional phosphate chemical enterprises using the iron method to synthesize iron phosphate have relatively high benefits and product quality.
[0003] However, a large amount of hydrogen is generated during the acid dissolution process of dissolving iron blocks with phosphoric acid. The wide explosion limit of hydrogen brings greater safety risks. Moreover, the current iron dissolution device still has the defect of a long production process, resulting in large fluctuations in the composition of the iron dissolution liquid and affecting the quality stability of iron phosphate products.
[0004] Therefore, this application provides an iron dissolution device for iron phosphate by the iron method and an iron phosphate production device. Utility Model Content
[0005] In order to overcome the deficiencies of the prior art, this application provides an iron dissolution device for iron phosphate by the iron method and an iron phosphate production device. By adding water vapor through a steam pipeline, when the entire iron dissolution device for iron phosphate by the iron method is in a slightly negative pressure state, the water vapor and the generated hydrogen are discharged through an exhaust pipe, and then the hydrogen and water are separated by a condenser, thereby recovering the hydrogen and solving the problem of hydrogen emission.
[0006] The technical solution adopted by this application to solve its technical problems is as follows:
[0007] On the one hand, this application provides an iron dissolution device for iron phosphate by the iron method, including a reaction kettle. An exhaust pipe for discharging hydrogen and water vapor is provided at the top of the reaction kettle, and a feeding port is provided on the reaction kettle; a steam pipeline for introducing water vapor into the reaction kettle is provided outside the reaction kettle.
[0008] Preferably, the exhaust pipe is connected to a condenser, the exhaust port of the condenser is connected to the exhaust pipe; the liquid discharge port of the condenser is connected to a liquid distribution tank.
[0009] More preferably, the liquid preparation tank is connected to the feeding port on the reaction kettle; the exhaust pipe is connected to an exhaust fan or a vacuum pump.
[0010] Preferably, a circulation pipeline outlet is provided on the bottom side of the reaction kettle, the circulation pipeline outlet is connected to a circulation pipeline, a circulation pump is arranged on the circulation pipeline, and the circulation pipeline outlet is connected to the feeding port through the circulation pipeline.
[0011] Preferably, a heating device is arranged inside the reaction kettle.
[0012] More preferably, the heating device comprises two heating coils; one heating coil is located at the upper part of the reaction kettle and the other heating coil is located at the bottom of the reaction kettle.
[0013] Preferably, a stirring paddle is arranged inside the reaction kettle.
[0014] Preferably, a distributor is arranged at the top of the reaction kettle, and the steam pipeline is connected to the distributor.
[0015] Preferably, a manhole is arranged on the side of the reaction kettle, and an acid hydrolysis support is arranged inside the reaction kettle corresponding to the manhole.
[0016] On the other hand, the present application provides a ferric phosphate production device, comprising the above-mentioned iron process ferric phosphate iron dissolving device, and the bottom of the reaction kettle is connected to an oxidation tank.
[0017] The beneficial effects of the present application are as follows:
[0018] 1. For the iron process ferric phosphate iron dissolving device of the present application, water vapor is added through the steam pipeline, and the whole iron process ferric phosphate iron dissolving device is in a slightly negative pressure state through an exhaust device, so that the generated hydrogen and water vapor are discharged through the exhaust pipe, and the discharged hydrogen and water vapor are separated through a condenser to recover hydrogen, solving the problem of hydrogen emission.
[0019] 2. For the iron process ferric phosphate iron dissolving device of the present application, the circulating operation is used to ensure the uniform mixing and continuous flow of the liquid material, guarantee the quality of the ferric phosphate product, reduce the reaction time, improve the production efficiency, and also reduce the additional energy consumption required due to uneven local temperature or uneven liquid material mixing, thereby reducing the overall energy consumption. Description of the Drawings
[0020] The present application will be further described below with reference to the drawings and embodiments.
[0021] Figure 1 is a schematic structural diagram of an iron process ferric phosphate iron dissolving device described in the present application;
[0022] Figure 2It is a schematic structural diagram of the iron phosphate production device described in this application;
[0023] Figure 3 It is a schematic structural diagram of the connection between the exhaust pipe and the condenser in an iron method iron phosphate iron dissolving device;
[0024] Figure 4 It is a schematic diagram of the material flow direction of an iron method iron phosphate iron dissolving device described in this application;
[0025] Wherein: 1. Reaction kettle; 2. Exhaust pipe; 3. Steam pipeline; 4. Condenser; 5. Liquid preparation tank; 6. Heating equipment; 7. Exhaust fan; 8. Vacuum pump; 9. Circulation pipeline; 10. Circulation pump; 12. Heating coil; 13. Oxidation tank; 101. Feeding port; 102. Circulation pipeline outlet; 103. Stirring paddle; 104. Distributor; 105. Acid hydrolysis support; 106. Manhole. Detailed implementation mode
[0026] The following will clearly and completely describe the concept, specific structure and technical effects generated by this application in combination with the embodiments and drawings, so as to fully understand the purpose, features and effects of this application. Obviously, the described embodiments are only a part of the embodiments of this application, rather than all embodiments. Based on the embodiments of this application, other embodiments obtained by those skilled in the art without creative efforts all belong to the scope protected by this application. In addition, all the connection / connection relationships involved in the patent do not simply refer to the direct connection of components, but refer to the more optimal connection structure that can be formed by adding or reducing connection accessories according to the specific implementation situation. Each technical feature in this application can be combined interactively without conflicting with each other.
[0027] As Figure 1 shown, an iron method iron phosphate iron dissolving device includes a reaction kettle 1, an exhaust pipe 2 for discharging hydrogen and water vapor is arranged at the top of the reaction kettle 1, and a feeding port 101 is arranged on the reaction kettle 1; a steam pipeline 3 for introducing steam into the reaction kettle 1 is arranged outside the reaction kettle 1.
[0028] Specifically, the reaction kettle is also provided with several different feeding ports, and phosphoric acid and pure water are put into the reaction kettle through the feeding ports;
[0029] A manhole 106 is arranged on the side of the reaction kettle 1, and an acid hydrolysis support 105 is arranged in the reaction kettle corresponding to the manhole 106. More specifically, there is a manhole with a larger opening on the side of the reaction kettle, and the bundled iron source can be placed on the support in the reaction kettle through this manhole.
[0030] In this application, after iron and phosphoric acid react in a reaction kettle, hydrogen is generated; air is extracted through an exhaust pipe, making the reaction kettle in a slightly negative pressure state, so that the water vapor and hydrogen in the reaction kettle can be discharged together to the outside of the reaction kettle, thus completing the discharge of hydrogen; the slightly negative pressure state helps to draw out / discharge the hydrogen generated during the reaction process and prevent it from accumulating in the reaction kettle, thereby reducing the safety risk.
[0031] Specifically, in this application, water vapor is introduced through a steam pipeline. During the process of discharging hydrogen through the exhaust pipe, since the hydrogen contains some water vapor, the presence of water vapor will dilute the hydrogen and reduce the volume fraction of hydrogen in the mixed gas. At the same time, water vapor itself is an inert substance and will not participate in the combustion reaction of hydrogen; moreover, since the explosion of hydrogen requires the participation of oxygen, the presence of water vapor will reduce the actual concentration of oxygen in the mixed gas, making it more difficult for the mixture of hydrogen and oxygen to reach the conditions required for explosion.
[0032] More specifically, the iron source is in the form of iron rods, iron ingots, and iron filings, avoiding the uncontrollable iron dissolution caused by too fast reaction rate when using iron powder, and reducing the raw material cost of iron.
[0033] More specifically, the reaction kettle can be designed in a cylindrical shape, and the material is stainless steel, lined with PE carbon steel, fiberglass, etc.
[0034] More specifically, the input end of the steam pipeline is arranged outside the reaction kettle and connected to an external water vapor generator (existing and common water vapor generators can be used, such as water tube boilers, bubbling bed boilers, etc.); the output end of the steam pipeline is located inside the reaction kettle. Therefore, through the steam pipeline, external water vapor can be introduced into the reaction kettle.
[0035] In one embodiment, the exhaust pipe 2 is connected to the condenser 4, the exhaust port of the condenser 4 is connected to the exhaust pipe 2; the liquid discharge port of the condenser 4 is connected to the liquid distribution tank 5.
[0036] Specifically, the water formed after the water vapor is condensed by the condenser flows into the liquid distribution tank through the liquid discharge port. The liquid distribution tank can use the water flowing in from the liquid discharge port to prepare a phosphoric acid solution, that is, dilute concentrated phosphoric acid and water to prepare a phosphoric acid solution with a corresponding concentration.
[0037] Therefore, by connecting the exhaust pipe set at the top of the reaction kettle to the condenser, the hydrogen and water vapor generated during the process of dissolving iron blocks in phosphoric acid are discharged in time, avoiding accumulation in the reaction kettle, thereby reducing the safety risk; the liquid discharge port of the condenser is connected to the liquid distribution tank, and the condensed water is collected and used to prepare a phosphoric acid solution, reducing the waste of water resources and improving the efficiency of the production process.
[0038] In one embodiment, as Figure 3As shown, the liquid preparation tank 5 is connected to the feeding port 101 on the reaction kettle 1; the exhaust pipe 2 is connected to the exhaust fan 7 or the vacuum pump 8.
[0039] Specifically, the exhaust pipe is evacuated by an exhaust fan or a vacuum pump, so that the reaction kettle is in a slightly negative pressure state. The water vapor and the generated hydrogen in the reaction kettle can be pumped into the condenser. The water vapor and hydrogen are separated by the different dew points of hydrogen and steam. The hydrogen can be collected by a collection device; the water vapor turns into water and flows out through the liquid discharge port of the condenser.
[0040] In one embodiment, a circulation pipeline outlet 102 is arranged on the bottom side of the reaction kettle 1. The circulation pipeline outlet 102 is connected to the circulation pipeline 9. A circulation pump 10 is arranged on the circulation pipeline 9. The circulation pipeline outlet 102 is connected to the feeding port 101 through the circulation pipeline 9.
[0041] Specifically, on the bottom side of the reaction kettle, a circulation pipeline outlet is arranged. The circulation pipeline outlet can lead the liquid material at the bottom of the reaction kettle into the circulation pipeline. The liquid material at the bottom of the reaction kettle is introduced into the feeding port by the circulation pump, thus completing the circulation process.
[0042] In the above technical solution, through the circulation operation, the uniform mixing and continuous flow of the liquid material are ensured, the reaction time is reduced, the production efficiency is improved, and the additional energy consumption required due to uneven local temperature or uneven mixing of the liquid material is reduced, thereby reducing the overall energy consumption.
[0043] In one embodiment, a heating device 6 is arranged in the reaction kettle 1. The heating device 6 includes two heating coils 12; one heating coil 12 is located in the upper part of the reaction kettle 1, and the other heating coil 12 is located at the bottom of the reaction kettle 1.
[0044] Specifically, a heating device is arranged in the reaction kettle to provide the necessary heat to ensure that the chemical reaction in the production process of iron phosphate can proceed at an appropriate temperature; during the process of dissolving iron blocks in phosphoric acid, the reaction liquid material needs to be heated to 95 - 100 °C.
[0045] The traditional single heating method may cause uneven temperature distribution in the reaction kettle, affecting the reaction efficiency and product quality. The design of two heating coils solves this problem by independently controlling the temperature of the upper and lower parts of the reaction kettle.
[0046] Moreover, in the reaction kettle, the viscosity of phosphoric acid gradually decreases with the increase of temperature. By using two steam coils in the reaction kettle, the lower heating coil can be preferentially used for heating during use, avoiding the slow heating situation caused by the overall temperature decrease after subsequent addition of phosphoric acid, and improving the iron dissolution effect.
[0047] In one embodiment, a stirring paddle 103 is provided inside the reaction kettle 1. Specifically, the stirring paddle is a spiral stirring paddle, which extends down from the middle of the top of the reaction kettle. After the spiral stirring paddle is started, it can press the liquid inside the reaction kettle downward. Through mechanical movement, the iron source and phosphoric acid inside the reaction kettle can be fully contacted, promoting the progress of the chemical reaction.
[0048] In one embodiment, a distributor 104 is provided at the top of the reaction kettle 1, and the steam pipeline 3 is connected to the distributor 104. The distributor is a circular distributor, and pure water or steam can be evenly sprayed into the kettle through a valve. The steam can be accurately transported to the distributor and evenly distributed inside the reaction kettle.
[0049] In one embodiment, the acidolysis support is a load-bearing and corrosion-resistant support.
[0050] In the present application, when the iron source is an iron block or a relatively large iron block, if it is directly put in, it will deposit at the bottom of the reaction kettle, easily blocking the bottom of the reaction kettle and affecting the progress of the circulating operation. Moreover, for the iron source located at the bottom, it is relatively difficult to be stirred in place through conventional stirring, resulting in a relatively slow dissolution efficiency. In order to improve the dissolution efficiency, in the present application, through the acidolysis support, the iron source is put into the acidolysis support. The acidolysis support is a corrosion-resistant stainless steel mesh, which is convenient for the phosphoric acid solution to enter. Moreover, the acidolysis support uses a load-bearing and corrosion-resistant support and will not be damaged by phosphoric acid. Therefore, the acidolysis support helps to increase the rate of the chemical reaction, thereby improving the production efficiency.
[0051] On the other hand, as Figure 2 shown, the present application provides a ferric phosphate production device, including the above-mentioned iron-method ferric phosphate iron-dissolving device. The bottom of the reaction kettle 1 is connected to an oxidation tank 13. There is an acidolysis liquid outlet pipeline at the bottom of the acidolysis tank, which is connected to the oxidation process. After the iron source is dissolved in the iron-method ferric phosphate iron-dissolving device, the reacted material liquid is introduced into the oxidation tank for the next reaction.
[0052] In summary, as Figure 4 shown, for the iron-method ferric phosphate iron-dissolving device described in the present application, the specific working process is as follows:
[0053] Raw material preparation: First, fix the iron source (such as iron blocks, iron ingots or iron filings) on the acidolysis support inside the reaction kettle 1 through 106 and then close the manhole;
[0054] Put the phosphoric acid solution into the reaction kettle 1 through the feed port 101 of the reaction kettle.
[0055] Heating control: Heating equipment 6 is provided inside the reaction kettle 1, including two heating coils 12, which are respectively located at the upper and lower parts of the reaction kettle to provide the necessary heat to ensure that the chemical reaction proceeds at an appropriate temperature; control the temperature to 95 - 100 °C.
[0056] Steam injection: Steam is introduced into the reaction kettle 1 through the steam pipeline 3.
[0057] Stirring and mixing: A stirring paddle 103 is arranged in the reaction kettle 1. Through mechanical movement, the iron source and phosphoric acid can be evenly mixed to promote the progress of the chemical reaction.
[0058] Slightly negative pressure state: The reaction kettle 1 is in a slightly negative pressure state by connecting the exhaust pipe 2 to the exhaust fan 7 or the vacuum pump 8, which helps to discharge the generated hydrogen and steam from the reaction kettle.
[0059] Discharge of hydrogen and steam: Under the slightly negative pressure state, the generated hydrogen and steam are drawn out through the exhaust pipe 2 and sent to the condenser 4.
[0060] Condensation and separation: In the condenser 4, hydrogen and steam are separated. The steam condenses into water and flows into the liquid distribution tank 5 through the liquid discharge port of the condenser, while the hydrogen is discharged or recycled through the exhaust pipe.
[0061] Circulation operation: A circulation pipeline outlet 102 is provided at the bottom side of the reaction kettle 1, which is connected to the circulation pipeline 9. A circulation pump 10 is arranged on the circulation pipeline. Through the circulation pump 10, the liquid in the bottom of the reaction kettle is circulated back to the feeding port 101 to ensure the uniform mixing and continuous flow of the liquid.
[0062] After the dissolution of the iron source is completed, the reacted liquid is introduced into the oxidation tank 13 through the acidolysis liquid outlet pipeline at the bottom of the acidolysis tank for the next oxidation reaction.
[0063] The above is a specific description of the preferred embodiment of the present application. However, the present application is not limited to the described embodiment. Those skilled in the art can also make various equivalent deformations or substitutions without departing from the spirit of the present application. These equivalent deformations or substitutions are all included in the scope defined by the claims of the present application.
Claims
1. An iron-based ferric phosphate dissolving device, characterized in that: The invention comprises a reactor (1), wherein an exhaust pipe (2) for discharging hydrogen and water vapor is arranged on the top of the reactor (1), and a feed port (101) is arranged on the reactor (1); and a steam pipeline (3) for introducing water vapor into the reactor (1) is arranged outside the reactor (1).
2. The iron phosphate dissolving device according to claim 1, characterized in that: The exhaust pipe (2) is connected to the condenser (4), and the exhaust port of the condenser (4) is connected to the exhaust pipe (2); the liquid discharge port of the condenser (4) is connected to the liquid distribution tank (5).
3. The iron phosphate dissolving device according to claim 2, characterized in that: The liquid preparation tank (5) is connected to the feeding port (101) on the reaction kettle (1); and the exhaust pipe (2) is connected to an exhaust fan (7) or a vacuum pump (8).
4. The iron phosphate dissolving device according to claim 1, characterized in that: A circulation pipeline outlet (102) is provided on the bottom side of the reaction kettle (1), the circulation pipeline outlet (102) is connected to a circulation pipeline (9), a circulation pump (10) is provided on the circulation pipeline (9), and the circulation pipeline outlet (102) is connected to a feeding port (101) through the circulation pipeline (9).
5. The iron phosphate dissolving device according to claim 1, characterized in that: A heating device (6) is provided in the reaction kettle (1).
6. The iron phosphate dissolving device according to claim 5, characterized in that: The heating device (6) comprises two heating coils (12); one heating coil (12) is located at the top of the reaction kettle (1), and the other heating coil (12) is located at the bottom of the reaction kettle (1).
7. The iron phosphate dissolving device according to claim 1, characterized in that: A stirring paddle (103) is arranged in the reaction kettle (1).
8. The iron phosphate dissolving device according to claim 1, characterized in that: A distributor (104) is provided on the top of the reaction kettle (1), and the steam pipeline (3) is connected to the distributor (104).
9. The iron phosphate dissolving device according to claim 1, characterized in that: A manhole (106) is provided on the side of the reactor, and an acid hydrolysis support (105) is provided in the reactor (1) corresponding to the manhole (106).
10. An iron phosphate production device, characterized in that: It comprises an iron-based ferric phosphate dissolving device as described in any one of claims 1 to 9, wherein the bottom of the reaction kettle (1) is connected to an oxidation tank (13).