A kettle type continuous synthesis reaction device for iron phosphate
Patent Information
- Application Number
- CN202522492430.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-25
- Publication Date
- 2026-09-29
- Estimated Expiration
- 2035-11-25
AI Technical Summary
[0005]本实用新型的目的在于提出一种磷酸铁釜式连续合成反应装置,以解决磷酸铁铁法工艺设计的合成装置因生产效率低、能耗高、产品一致性和均一性差、杂质难控制,最终导致磷酸铁产品质量稳定性不好的问题
[0007]本实用新型设计的连续合成反应装置,通过设置滴加组件、多个合成反应釜和陈化釜,设置多个控制器,能够精准控制反应条件,实现物料的连续进料与出料,显著提升生产效率,且设备自动连锁确保反应稳定可控。
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Figure CN224807448U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of iron phosphate preparation technology, and in particular to an iron phosphate continuous synthesis reaction apparatus in a batch reactor. Background Technology
[0002] As research into environmentally friendly new energy sources deepens, the development of energy storage batteries is also progressing rapidly. Among them, lithium-ion batteries have received widespread attention due to their advantages such as high specific capacity, long lifespan, good safety, and environmental friendliness. The positive electrode material of lithium-ion batteries is generally lithium iron phosphate, which has advantages such as low lithium cost, high safety, good cycle performance, and stable high-temperature performance.
[0003] A continuous synthesis reactor is the equipment used in the ferric phosphate process to produce ferric phosphate. Its purpose is to provide the reaction space, temperature, pressure, and homogenization for the reaction between ferrous liquid and hydrogen peroxide, thereby increasing the chemical reaction rate and ensuring the stability of the synthesis slurry composition. Currently, most synthesis reactors designed for the ferric phosphate process employ batch processes (such as liquid-phase precipitation), which suffer from low production efficiency, high energy consumption, poor product consistency and uniformity, and difficulty in controlling impurities. Consequently, the quality stability of ferric phosphate products is poor, making it difficult to meet large-scale market demands.
[0004] Therefore, it is necessary to improve and design the iron phosphate synthesis reaction device and structure to solve the problems of low production efficiency, high energy consumption, poor product consistency and uniformity, and difficulty in controlling impurities in the iron phosphate process design, which ultimately leads to poor quality stability of iron phosphate products. Utility Model Content
[0005] The purpose of this invention is to propose a continuous reactor for the synthesis of iron phosphate in a batch, in order to solve the problems of low production efficiency, high energy consumption, poor product consistency and uniformity, and difficulty in controlling impurities in the design of iron phosphate synthesis devices, which ultimately lead to poor quality stability of iron phosphate products.
[0006] To solve the above-mentioned technical problems, the present invention adopts the following technical solution: A continuous ferric phosphate synthesis reactor includes a ferrous liquid preheating assembly, a filtration assembly, a synthesis reactor assembly, a dropping assembly, and an aging reactor assembly. The outlet of the ferrous molten preheating component is connected to the inlet of the filter component, the outlet of the filter component is connected to the synthesis reactor group, the upper end of the synthesis reactor group is equipped with a dripping component, the synthesis reactor group is connected to the aging reactor group, and the slurry coming out of the aging reactor group enters the next process.
[0007] The continuous synthesis reaction device designed in this utility model, by setting up a dripping component, multiple synthesis reaction vessels and aging vessels, and setting up multiple controllers, can accurately control the reaction conditions, realize the continuous feeding and discharging of materials, significantly improve production efficiency, and the automatic interlocking of the equipment ensures that the reaction is stable and controllable.
[0008] The production of products is of uniform and stable quality. Continuous operation reduces batch differences and ensures product consistency. The continuously synthesized iron phosphate material has uniform particle size and regular morphology, which is superior to the batch method. In the field of battery materials, the continuous method effectively solves the batch stability problem and reduces battery safety hazards. Meanwhile, the continuous synthesis reaction device designed in this utility model is small in size and occupies little space, and reduces side reactions through precise temperature control.
[0009] As a preferred embodiment, the ferrous molten metal preheating tank has an inlet at the center of its top, a circulation inlet at the top, a circulation outlet at the bottom, and a liquid outlet at the lower end of the circulation outlet. The circulation outlet is connected to the inlet of a circulation pump, the circulation pump is connected to a graphite heat exchanger, the graphite heat exchanger is connected to the circulation inlet, and a temperature measuring device is installed on the conduit between the graphite heat exchanger and the circulation inlet. The liquid outlet is connected to the inlet of a filter assembly. This ensures that the ferrous molten metal meets the conditions for subsequent reactions.
[0010] As a preferred embodiment, the filtration assembly includes a filter and a filtration assembly pump. The precision microporous membrane filter is connected to the outlet of the ferrous liquid preheating assembly via a conduit, and the outlet of the filter is connected to the synthesis reactor assembly via another conduit. The filtration assembly pump is mounted on the other conduit.
[0011] The filter in this invention can be a precision microporous membrane filter, which can precisely filter out ultrafine particles in the ferrous melt, better removing them without affecting subsequent oxidation synthesis processes. During the heating of the ferrous melt, some ferrous iron inevitably oxidizes to form precipitates; the purpose here is to filter out these precipitates, thus stabilizing the ferrous melt during the reaction.
[0012] As a preferred embodiment, the synthesis reactor group includes at least one synthesis reactor, each synthesis reactor is equipped with two stirrers located in the middle and bottom respectively, each synthesis reactor is also equipped with a temperature measuring element, the synthesis reactors are connected to each other by a pump, the liquid outlet of the filter assembly is connected to the liquid inlet of the first synthesis reactor by a pump, and the last synthesis reactor is connected to the first aging reactor by a pump.
[0013] This invention comprises at least one synthesis reactor assembly with controllable rotation speed, which further ensures complete reaction and allows for precise temperature control of the synthesis reactor assembly. This enables precise control of crystal nucleation and growth during the synthesis of iron phosphate, facilitating control of the final crystal morphology and particle size. The use of dual stirrers in the storage tank, agitating at the middle and bottom, eliminates backmixing issues that can occur during continuous production.
[0014] As a preferred embodiment, the dripping assembly includes at least one storage tank, each storage tank being positioned above each synthesis reactor. A spray pipe is connected below the storage tank, and a controller for controlling the dripping speed of the spray liquid is provided between the spray pipe and the storage tank. The spray pipe is annular or other shape that ensures that the spray liquid enters the synthesis reactor from multiple points. The spray pipe is located at the top of the synthesis reactor or at a certain distance from the top, and the synthesis reactor has corresponding holes for receiving the spray liquid.
[0015] The annular pipe can be installed at the top of the synthesis reactor or at a certain height above the top of the reactor, ensuring that hydrogen peroxide enters the reactor. The receiving port for the spray liquid should avoid the mounting holes for the agitator motor, temperature sensing elements, and the liquid inlet of the previous process or equipment at the top of the reactor.
[0016] This invention pre-calculates the feed ratio and flow rate of ferrous liquid and hydrogen peroxide based on process parameters and completes the controller settings, performing the synthesis reaction multiple times. The hydrogen peroxide spraying method reduces the local concentration of hydrogen peroxide upon contact with the ferrous liquid, making the reaction process more controllable.
[0017] As a preferred embodiment, the aging reactor assembly includes at least one aging reactor, each equipped with dual stirrers located in the middle and bottom respectively, and each reactor also has a temperature sensing element. The aging reactors are connected to each other via pumps, and the last synthesis reactor is connected to the next process stage via a pump. This ensures thorough aging.
[0018] As a preferred option, both the reactor in the synthesis reactor group and the aging reactor in the aging reactor group are jacketed enamel reactors, which can be heated by steam and the temperature is controllable. Attached Figure Description
[0019] Figure 1 This is a schematic diagram of the structure of one embodiment of the present utility model; Figure 2 This is a schematic diagram of the preheating component structure according to an embodiment of the present invention; Figure 3 This is a schematic diagram of the structure of a filter assembly according to an embodiment of the present invention; Figure 4 This is a schematic diagram of the hydrogen peroxide droplet addition component structure according to an embodiment of the present invention; Figure 5This is a schematic diagram of the synthesis reactor assembly structure according to an embodiment of the present invention; Figure 6 This is a schematic diagram of a spray pipe structure connected to a pipeline according to an embodiment of the present invention; Figure 7 This is a schematic diagram of the aging kettle assembly structure according to an embodiment of the present invention; In the picture: 1-Ferrous molten preheating assembly, 11-Ferrous molten preheating storage tank, 12-Circulating pump, 13-Graphite heat exchanger, 14-Liquid inlet, 15-Temperature measuring control, 16-Circulation inlet, 17-Circulation outlet, 18-Liquid outlet; 2-Filter assembly, 21-Precision microporous membrane filter, 22-Filter assembly pump, 23-First conduit, 24-Second conduit; 3-Hydrogen peroxide dripping assembly, 31-First hydrogen peroxide storage tank, 32-Second hydrogen peroxide storage tank, 33-Third hydrogen peroxide storage tank, 34-First spray pipe, 35-Second spray pipe, 36-Third spray pipe, 37-First controller, 38-Second controller, 39-Third controller, 310-Hydrogen peroxide delivery pipe; 4-Synthesis reactor group, 41-First synthesis reactor, 42-Second synthesis reactor, 43-Third synthesis reactor, 44-First synthesis pump, 45-Second synthesis pump, 46-Third synthesis pump, 47-First stirrer, 48-Second stirrer, 49-Third stirrer, 410-First temperature sensing element, 411-Second temperature sensing element, 412-Third temperature sensing element, 413-First synthesis conduit, 414-Second synthesis conduit, 415-Third synthesis conduit, 416-First variable frequency motor, 417-Second variable frequency motor, 418-Third variable frequency motor; 5-Aging kettle assembly, 51-First aging kettle, 52-Second aging kettle, 53-First aging pump, 54-Second aging pump, 55-Fourth stirrer, 56-Fifth stirrer, 57-Fourth variable frequency motor, 58-Fifth variable frequency motor, 59-Fourth temperature measuring element, 510-Fifth temperature measuring element, 511-First aging conduit, 512-Second aging conduit. Detailed Implementation
[0020] The technical solutions in the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. Based on the embodiments, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of this application.
[0021] Unless otherwise defined, the technical or scientific terms used in the embodiments of this application shall have the ordinary meaning understood by one of ordinary skill in the art. The terms "first," "second," and similar terms used in this embodiment do not indicate any order, quantity, or importance, but are merely used to distinguish different components. Terms such as "comprising" or "including" mean that the element or object preceding the word encompasses the elements or objects listed after the word and their equivalents, without excluding other elements or objects. "Installed," "connected," and "linked" should be interpreted broadly; for example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal connection of two elements. Terms such as "upper," "lower," "left," "right," "horizontal," and "vertical" are used only relative to the orientation of the components in the accompanying drawings. These directional terms are relative concepts used for relative description and clarification, and they may change accordingly depending on the orientation of the components in the accompanying drawings.
[0022] In this application, "at least one" means one or more, and "more than one" means two or more. "And / or" describes the relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A alone, A and B simultaneously, or B alone, where A and B can be singular or plural. The character " / " generally indicates an "or" relationship between the preceding and following related objects; in formulas, the character " / " indicates a "division" relationship. "At least one of the following" or similar expressions refer to any combination of these items, including any combination of single or plural items. For example, at least one of a, b, or c can represent: a, b, c, ab, ac, bc, or abc, where a, b, and c can be single or multiple.
[0023] It is understood that the various numerical designations used in the embodiments of this application are merely for descriptive convenience and are not intended to limit the scope of the embodiments of this application.
[0024] It is understood that, in the embodiments of this application, the order of the above-mentioned process numbers does not imply the order of execution. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of this application.
[0025] Continuous synthesis technology achieves automation and continuity of the production process by precisely controlling reaction conditions such as temperature, pH, and flow rate, and has the following significant advantages: 1) Continuous synthesis achieves continuous feeding and discharging of materials through fully automated operation, significantly improving production efficiency, and the automatic interlocking of equipment ensures stable and controllable reaction; 2) Product quality is uniform and stable. Continuous operation reduces batch differences and ensures product consistency. The iron phosphate material produced by continuous synthesis has uniform particle size and regular morphology, which is superior to batch method products. In the field of battery materials, the continuous method effectively solves the batch stability problem and reduces battery safety hazards; 3) Continuous synthesis equipment is small in size and occupies little space. It also reduces energy consumption through precise temperature control and reduction of side reactions, which is in line with the trend of green production.
[0026] Therefore, we improved and designed the iron phosphate synthesis reaction device and structure, and proposed an iron phosphate continuous synthesis reaction device in a kettle, including a ferrous liquid preheating component, a filtration component, a synthesis reaction kettle group, a dropping component and an aging kettle group. The outlet of the ferrous molten preheating component is connected to the inlet of the filter component, the outlet of the filter component is connected to the synthesis reactor group, the upper end of the synthesis reactor group is equipped with a dripping component, the synthesis reactor group is connected to the aging reactor group, and the slurry coming out of the aging reactor group enters the next process.
[0027] The continuous synthesis reaction device designed in this utility model, by setting up a dripping component, multiple synthesis reaction vessels and aging vessels, and setting up multiple controllers, can accurately control the reaction conditions, realize the continuous feeding and discharging of materials, significantly improve production efficiency, and the automatic interlocking of the equipment ensures that the reaction is stable and controllable.
[0028] The continuous production process ensures consistent and uniform product quality, reducing batch variations and guaranteeing product consistency. The continuously synthesized iron phosphate material exhibits superior particle size and morphology compared to batch-process products. In the battery materials field, the continuous method effectively addresses batch stability issues and reduces battery safety hazards. It also solves the problems of low production efficiency, high energy consumption, poor product consistency and uniformity, and difficulty in controlling impurities in the iron-method synthesis reactor, which ultimately leads to poor quality stability of iron phosphate products. The pipes, conduits, or tubing connecting the inlet and outlet are commercially available products; the appropriate model can be selected as needed. Furthermore, the continuous synthesis reactor designed in this invention is small in size and requires minimal space. Through precise temperature control and reduction of side reactions, the number of synthesis reactors and aging reactors can be adjusted as needed.
[0029] As a preferred embodiment, the ferrous molten metal preheating tank has an inlet at the center of its top, a circulation inlet at the top, a circulation outlet at the bottom, and a liquid outlet at the lower end of the circulation outlet. The circulation outlet is connected to the inlet of a circulation pump, the circulation pump is connected to a graphite heat exchanger, the graphite heat exchanger is connected to the circulation inlet, and a temperature measuring device is installed on the conduit between the graphite heat exchanger and the circulation inlet. The liquid outlet is connected to the inlet of a filter assembly. This ensures that the ferrous molten metal meets the conditions for subsequent reactions. The graphite heat exchanger is a commercially available product.
[0030] As a preferred embodiment, the filtration assembly includes a filter and a filtration assembly pump. The precision microporous membrane filter is connected to the outlet of the ferrous melt preheating assembly via a conduit, and the outlet of the filter is connected to the synthesis reactor assembly via another conduit, on which the filtration assembly pump is mounted. The pump used here is a commercially available product; the appropriate model should be selected as needed.
[0031] The filter in this invention can be an existing precision microporous membrane filter, which can precisely filter out ultrafine particles in the ferrous melt, better removing them without affecting subsequent oxidation synthesis processes. During the heating of the ferrous melt, some ferrous iron inevitably oxidizes to form precipitates; the purpose here is to filter out these precipitates, thus stabilizing the ferric melt during the reaction.
[0032] As a preferred embodiment, the synthesis reactor assembly includes at least one synthesis reactor, each equipped with dual stirrers located in the middle and bottom respectively. Each reactor also includes a temperature sensing element. The reactors are connected via pumps. The outlet of the filter assembly is connected to the inlet of the first synthesis reactor via a pump, and the last synthesis reactor is connected to the first aging reactor via a pump. The stirrers in the middle and bottom can be impellers, a conventional structure, simply with one stirrer in the middle and one at the bottom.
[0033] This invention relates to at least one synthesis reactor assembly with controllable rotation speed, which further ensures complete reaction and allows for precise temperature control of the synthesis reactor assembly. This enables precise control of crystal nucleation and growth during the iron phosphate synthesis process, facilitating control of the final crystal morphology and particle size. The inclusion of dual stirrers in the storage tank eliminates backmixing during continuous production. The stirrer motors are commercially available products and can be frequency-controlled. The temperature sensing elements are commercially available temperature sensors or thermometers.
[0034] As a preferred embodiment, the dripping assembly includes at least one storage tank, each storage tank being positioned above each synthesis reactor. A spray pipe is connected below the storage tank, and a controller for controlling the dripping speed of the spray liquid is provided between the spray pipe and the storage tank. The spray pipe is annular or other shape that ensures that the spray liquid enters the synthesis reactor from multiple points. The spray pipe is located at the top of the synthesis reactor or at a certain distance from the top, and the synthesis reactor has corresponding holes for receiving the spray liquid.
[0035] The controller can be an existing product such as a solenoid valve for controlling flow. For a more complete reaction, the spray pipe can be a ring pipe or a pipe of other shapes, such as elliptical, semi-circular, rectangular, triangular, etc., to ensure that hydrogen peroxide enters the synthesis reactor from multiple points.
[0036] This invention pre-calculates the feed ratio and flow rate of ferrous liquid and hydrogen peroxide based on process parameters and sets the controller accordingly, performing the synthesis reaction multiple times. The hydrogen peroxide spraying method reduces the local concentration of hydrogen peroxide in contact with ferrous liquid, increases the contact area between them, and makes the reaction process more controllable.
[0037] As a preferred embodiment, the aging reactor assembly includes at least one aging reactor, each equipped with dual stirrers located in the middle and bottom respectively. Each aging reactor also contains a temperature sensing element. The aging reactors are connected via pumps, and the final synthesis reactor is connected to the next process stage via a pump. This ensures thorough aging. The dual stirrers, temperature sensing elements, and stirrer control motors are the same as described above.
[0038] As a preferred option, both the reactor in the synthesis reactor group and the aging reactor in the aging reactor group are jacketed enamel reactors, which can be heated by steam and the temperature is controllable.
[0039] Unless otherwise specified, the temperature measuring controls, various pumps, stirrers, controllers, various conduits, temperature measuring elements, spray pipes, motors, and other non-improvement devices or equipment involved in this embodiment are all existing commercially available products. Those skilled in the art can select the appropriate model of product as needed.
[0040] To make the objectives, technical solutions, and advantages of this utility model clearer, the following detailed description is provided in conjunction with the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the scope of the utility model. Three synthesis reactors and two aging reactors are used as an example. The dripping assembly is used for adding hydrogen peroxide.
[0041] like Figure 1 As shown, the continuous synthesis reaction apparatus for iron phosphate in this embodiment includes a ferrous liquid preheating component 1, a filtration component 2, a hydrogen peroxide dripping component 3, a synthesis reaction vessel group 4, and an aging vessel group 5.
[0042] As one implementation method, such as Figure 2 As shown, the ferrous molten metal preheating assembly 1 includes a ferrous molten metal preheating storage tank 11, a circulating pump 12, a graphite heat exchanger 13, a liquid inlet 14, a temperature measuring control 15, a circulation inlet 16, a circulation outlet 17, and a liquid outlet 18.
[0043] The ferrous molten metal preheating storage tank 11 has an inlet 14 at the center of the top, a circulation inlet 16 on the right side of the top, a circulation outlet 17 on the right side of the bottom, an outlet 18 at the lower end of the circulation outlet 17, the circulation outlet 17 is connected to the inlet of the circulation pump 12, the outlet of the circulation pump 12 is connected to the inlet of the graphite heat exchanger 13, the outlet of the graphite heat exchanger 13 is connected to the circulation inlet 16, and a temperature measuring control 15 is provided on the conduit between the outlet of the graphite heat exchanger 13 and the circulation inlet 16.
[0044] The outlet 18 is connected to the inlet end of the filter assembly 2, and the outlet end of the filter assembly 2 is connected to the synthesis reactor group 4. Three hydrogen peroxide dripping components 3 are assembled on the upper end of the synthesis reactor group 4. The last synthesis reactor is connected to the first aging reactor 51. The slurry that comes out of the last aging reactor can enter the next process.
[0045] As one implementation method, such as Figure 3 As shown, the filter assembly 2 includes a precision microporous membrane filter 21, a filter assembly pump 22, a first conduit 23, and a second conduit 24.
[0046] The inlet of the precision microporous membrane filter 21 is connected to the outlet 18 of the ferrous liquid preheating assembly 1 via the second conduit 24. The outlet of the precision microporous membrane filter 21 is connected to the synthesis reactor assembly 4 via the first conduit 23, on which a filter assembly pump 22 is installed.
[0047] As one implementation method, such as Figure 4 As shown, the hydrogen peroxide dripping assembly 3 includes a first hydrogen peroxide storage tank 31, a second hydrogen peroxide storage tank 32, and a third hydrogen peroxide storage tank 33. A first spray pipe 34, a second spray pipe 35, and a third spray pipe 36 are sequentially arranged below each hydrogen peroxide storage tank. Each spray pipe is equipped with a first controller 37, a second controller 38, and a third controller 39 to control the hydrogen peroxide dripping acceleration on its connecting pipe. The inlets of the first hydrogen peroxide storage tank 31, the second hydrogen peroxide storage tank 32, and the third hydrogen peroxide storage tank 33 are connected to a hydrogen peroxide delivery pipe 310, which may be equipped with a control valve. Taking a ring pipe as an example, the upper end of the ring pipe has a hole for connecting to a pipeline, and the bottom has several spray holes. Each synthesis reactor in the synthesis reactor assembly 4 has a corresponding hole for receiving the sprayed liquid. The diameter of the hole connecting to the pipeline can be larger than the diameter of the spray nozzle to ensure that hydrogen peroxide can be sprayed from at least some of the spray nozzles. The hydrogen peroxide comes out from below the hydrogen peroxide storage tank, passes through a pipeline equipped with a controller, and enters the spray pipe, such as... Figure 6 As shown.
[0048] As one implementation method, such as Figure 5As shown, the synthesis reactor group 4 includes a first synthesis reactor 41, a second synthesis reactor 42, and a third synthesis reactor 43. The liquid inlet at the top of the first synthesis reactor 41 is connected to the outlet of the precision microporous membrane filter 21. The three synthesis reactors are connected in series via pumps and conduits. Specifically: The bottom outlet of the first synthesis reactor 41 is connected to one end of the first synthesis pump 44. The other end of the first synthesis pump 44 is connected to the top inlet of the second synthesis reactor 42 through the first synthesis conduit 413. The bottom outlet of the second synthesis reactor 42 is connected to one end of the second synthesis pump 45. The other end of the second synthesis pump 45 is connected to the top inlet of the third synthesis reactor 43 through the second synthesis conduit 414. The bottom outlet of the third synthesis reactor 43 is connected to one end of the third synthesis pump 46. The other end of the third synthesis pump 46 is connected to the aging reactor group 5 through the third synthesis conduit 415.
[0049] The first synthesis reactor 41, the second synthesis reactor 42, and the third synthesis reactor 43 are respectively equipped with a first stirrer 47, a second stirrer 48, and a third stirrer 49. The stirrers used in each reactor are dual stirrers, with one pair of stirring blades located at the bottom and one pair in the middle. The first stirrer 47, the second stirrer 48, and the third stirrer 49 are controlled by a first variable frequency motor 416, a second variable frequency motor 417, and a third variable frequency motor 418, respectively. A first temperature measuring element 410, a second temperature measuring element 411, and a third temperature measuring element 412 are also respectively installed on one side of each of the three synthesis reactors.
[0050] The annular pipe is set at the top of the synthesis reactor, surrounding the motor mounting hole of the agitator and the hole for receiving the spray liquid, while avoiding the motor mounting hole of the agitator, the mounting hole for placing the temperature measuring element, and the liquid inlet of the previous process or equipment at the top of the synthesis reactor.
[0051] As one implementation method, such as Figure 7As shown, the aging reactor group 5 includes a first aging reactor 51 and a second aging reactor 52. A fourth stirrer 55 and a fifth stirrer 56 are respectively installed in the first aging reactor 51 and the second aging reactor 52. The fourth stirrer 55 and the fifth stirrer 56 are controlled by a fourth variable frequency motor 57 and a fifth variable frequency motor 58, respectively. A fourth temperature measuring element 59 and a fifth temperature measuring element 510 are respectively installed on one side of the fourth stirrer 55 and the fifth stirrer 56. The two aging reactors are connected in series via pumps and conduits. One end of the bottom outlet of the first aging reactor 51 is connected to one end of the first aging pump 53. The other end of the first aging pump 53 is connected to the top inlet of the second aging reactor 52 via the first aging conduit 511. One end of the bottom outlet of the second aging reactor 52 is connected to one end of the second aging pump 54. The other end of the second aging pump 54 can be connected to the inlet of the next process equipment via the second aging conduit 512. The fourth stirrer 55 and the fifth stirrer 56 are the same as the stirrers in the synthesis reactor group 4.
[0052] As one option, both the reactor in the synthesis reactor group and the aging reactor in the aging reactor group are jacketed enamel reactors.
[0053] One possible working process of this utility model embodiment is: The ferrous molten metal is transported through the inlet pipe and fed into the ferrous molten metal preheating tank 11 through the inlet port 14. The valve on the circulation outlet 17 on the bottom right side of the ferrous molten metal preheating tank 11 is then opened, and the circulation pump 12 is started to preheat the ferrous molten metal. The temperature is monitored by the temperature measuring control 15 until the temperature reaches the required set value for the process. The ferrous molten metal preheating component 1 preheats the metal to the required temperature. Simultaneously, the feed ratio and flow rate of ferrous molten metal and hydrogen peroxide are calculated in advance based on the process parameters, and the controller settings are completed. The stirring speeds and required temperatures for each reactor in the synthesis reactor group 4 and the aging reactor group 5 are also set. The stirring speed can be 240~250 r / min, and stirring is started simultaneously with the introduction of the slurry.
[0054] When the temperature reaches the set value, ferrous molten metal begins to continuously enter the ferrous molten metal preheating tank 11. The temperature of the ferrous molten metal inside the tank is kept constant by controlling the graphite heat exchanger 13, and the outlet 18 is opened. The filter assembly 2 is then activated, allowing the ferrous molten metal to pass through the filter assembly 2 and enter the first synthesis reactor 41. According to the pre-calculated hydrogen peroxide ratio, the first controller 37 is simultaneously activated. At this time, the ferrous molten metal and hydrogen peroxide react in the first synthesis reactor 41 at a certain stirring speed to obtain a preliminary slurry. Once the reaction time reaches the set value and the residence time meets the process requirements, the process is restarted. The first synthesis pump 44 pumps the slurry from the first synthesis reactor 41 into the second synthesis reactor 42. At the same time, the second controller 38 is turned on. At this time, the ferrous liquid and hydrogen peroxide react further in the second synthesis reactor 42 under a certain stirring speed. When the reaction time reaches the set value and the residence time reaches the required process time, the second synthesis pump 45 is turned on, and the slurry from the second synthesis reactor 42 enters the third synthesis reactor 43. At the same time, the third controller 39 is turned on, and the ferrous liquid and hydrogen peroxide react further in the third synthesis reactor 43 under a certain stirring speed.
[0055] In this process, the temperature of the synthesis reactor assembly can be precisely controlled to precisely control the crystal nucleation and crystal growth process in the synthesis of iron phosphate, which facilitates the control of the final crystal morphology and particle size.
[0056] After the synthesis reaction is completed and the residence time reaches the required level, the slurry is continuously fed from the third synthesis reactor 43 to the first aging reactor 51 at a set flow rate via the third synthesis pump 46. The first aging reactor mainly raises the temperature of the slurry to 80°C. It is the same size as the synthesis reactor and discharges the slurry after 20-30 minutes. After the required aging time is reached, the first aging pump 53 is turned on, and the slurry enters the second aging reactor 52 for further aging, which takes about 60 minutes. After aging is completed, the final slurry is obtained. The second aging pump 54 is then turned on, and the slurry can proceed to the next process stage.
[0057] Although the present invention has been described herein with reference to several illustrative embodiments, it should be understood that many other modifications and implementations can be devised by those skilled in the art, which will fall within the scope and spirit of the principles disclosed herein. More specifically, various variations and modifications can be made to the components and / or layout of the subject matter combination within the scope of the disclosure, drawings, and claims. Besides variations and modifications to the components and / or layout, other uses will be apparent to those skilled in the art.
Claims
1. A continuous reactor for the synthesis of iron phosphate, characterized in that: This includes a ferrous molten metal preheating assembly, a filtration assembly, a synthesis reactor assembly, a dropping assembly, and an aging reactor assembly; The outlet of the ferrous molten preheating component is connected to the inlet of the filter component, the outlet of the filter component is connected to the synthesis reactor group, the upper end of the synthesis reactor group is equipped with a dripping component, the synthesis reactor group is connected to the aging reactor group, and the slurry coming out of the aging reactor group enters the next process.
2. The continuous reactor for the synthesis of iron phosphate in a batch as described in claim 1, characterized in that: The ferrous molten metal preheating storage tank has an inlet at the center of the top, a circulation inlet at the top, a circulation outlet at the bottom, and an outlet at the lower end of the circulation outlet. The circulation outlet is connected to the inlet of the circulation pump, the circulation pump is connected to the graphite heat exchanger, the graphite heat exchanger is connected to the circulation inlet, a temperature measuring control is provided on the conduit between the graphite heat exchanger and the circulation inlet, and the outlet is connected to the inlet of the filter assembly.
3. The continuous reactor for the synthesis of iron phosphate according to claim 1, characterized in that: The filtration assembly includes a filter and a filtration assembly pump. The filter is connected to the outlet of the ferrous liquid preheating assembly via a conduit, and the outlet of the filter is connected to the synthesis reactor assembly via another conduit. The filtration assembly pump is installed on the other conduit.
4. The continuous reactor for the synthesis of iron phosphate in a batch as described in claim 1, characterized in that: The synthesis reactor group includes at least one synthesis reactor, each synthesis reactor is equipped with two stirrers, located in the middle and bottom respectively, and each synthesis reactor is also equipped with a temperature measuring element. The synthesis reactors are connected by pumps, the liquid outlet of the filter assembly is connected to the liquid inlet of the first synthesis reactor by a pump, and the last synthesis reactor is connected to the first aging reactor by a pump.
5. The continuous reactor for the synthesis of iron phosphate according to claim 1, characterized in that: The dripping assembly includes at least one storage tank, each storage tank being positioned above each synthesis reactor. A spray pipe is connected below the storage tank, and a controller for controlling the dripping speed of the spray liquid is provided between the spray pipe and the storage tank. The spray pipe is annular or other shape that ensures that the spray liquid enters the synthesis reactor from multiple points. The spray pipe is located at the top of the synthesis reactor or at a certain distance from the top, and the synthesis reactor has corresponding holes for receiving the spray liquid.
6. The continuous reactor for the synthesis of iron phosphate according to claim 1, characterized in that: The aging reactor group includes at least one aging reactor, each aging reactor is equipped with two stirrers, located in the middle and bottom respectively, and each aging reactor is also equipped with a temperature measuring element. The aging reactors are connected by a pump, and the last synthesis reactor is connected to the next process step by a pump.
7. The continuous reactor for the synthesis of iron phosphate according to claim 1, characterized in that: Both the reactor in the synthesis reactor group and the aging reactor in the aging reactor group are jacketed enamel reactors.