Iron phosphate synthesis reaction kettle

Abstract

The utility model relates to the technical field of iron phosphate preparation, in particular to an iron phosphate synthesis reaction kettle which comprises a reaction kettle body, a stirrer, a heating coil, a pH monitor probe, a particle morphology analyzer probe and a metering and batching assembly. A stirrer connected with a frequency modulation motor is arranged in the reaction kettle, a heating coil is arranged between the outer wall and the inner wall of the reaction kettle in a sleeved mode, a discharging port with a first valve is formed in the bottom of the reaction kettle, a pH monitor probe and a particle morphology analyzer probe are inserted into the side wall of the reaction kettle in a penetrating mode, the pH monitor probe is connected with a pH monitor, and the particle morphology analyzer probe is connected with a second valve. The particle morphology analyzer probe is connected with a particle morphology analyzer, and the pH monitor and the particle morphology analyzer are respectively connected with a metering and batching assembly at the top of the reaction kettle through a controller I; the problems that in the iron phosphate slurry synthesis process, the particle morphology and the pH value of iron phosphate cannot be corrected in time, and consequently the synthesized iron phosphate slurry is unstable in product performance and poor in quality are solved.

Description

Technical Field

[0001] The utility model relates to the technical field of ferric phosphate synthesis, in particular to a ferric phosphate synthesis reaction kettle. Background Art

[0002] Among lithium-ion batteries, lithium iron phosphate batteries have many advantages such as long cycle life, high safety, low cost, non-toxicity and easy battery recycling, and have relatively good energy density. They are suitable as power batteries and energy storage batteries. Especially in recent years, with the rapid development of the new energy vehicle industry, they have been widely used in the field of electric vehicles as power batteries and have received great attention. Battery-grade iron phosphate is the most commonly used precursor for preparing positive electrode materials for lithium iron phosphate batteries. The crystal type (morphology), particle size and distribution of battery-grade iron phosphate have a great influence on the tap density, specific surface area and electrochemical properties of battery-grade iron phosphate.

[0003] At present, the process technologies for preparing battery-grade iron phosphate are homogeneous precipitation method and rapid precipitation method. The process operation technologies of both methods are determined through small-scale tests or simulation experiments, such as the raw material ratio, feeding rate and pH value of the production process. The preliminary processes are then applied to the actual production equipment for verification. Afterwards, the raw material ratio, pH value and other process conditions of the production equipment are corrected according to the analysis data and performance test results of the output products. Only after the products produced are tested to be qualified, the control range of the appropriate process conditions is determined. Finally, a standardized operating procedure is formed to implement production operations.

[0004] The existing patent CN202320614136.6 discloses an iron phosphate synthesis reactor. Although the device can also complete the synthesis of iron phosphate, the reactor body in the device is not equipped with a monitoring device for monitoring the pH value of iron phosphate and a monitoring device for monitoring the morphology of iron phosphate particles. In addition, when various raw materials of iron phosphate are added to the reactor body, the proportions of various raw materials are inaccurate, resulting in different quality and performance of the synthesized iron phosphate. The morphology and pH value of the iron phosphate particles during the synthesis process cannot be corrected in time, resulting in poor quality of the iron phosphate slurry product.

[0005] Therefore, it is necessary to improve and optimize the iron phosphate synthesis process technology to solve the problem that the particle morphology and pH of iron phosphate cannot be corrected in time during the synthesis of iron phosphate slurry, resulting in unstable product performance and poor quality of the synthesized iron phosphate slurry. Utility Model Content

[0006] The utility model aims to provide an iron phosphate synthesis reactor to solve the problem that during the synthesis process of iron phosphate slurry, the particle morphology and pH of iron phosphate cannot be corrected in time, resulting in unstable product performance and poor quality of the synthesized iron phosphate slurry.

[0007] In order to solve the above technical problems, the utility model adopts the following technical solutions:

[0008] A ferric phosphate synthesis reactor, comprising a reactor body, an agitator, a heating coil, a pH monitor probe, a particle morphology analyzer probe and a metering and dosing component; the reactor body is provided with an agitator connected to a frequency modulation motor, the reactor body is provided with a heating coil between the outer wall and the inner wall, the reactor body is provided with a discharge port with a valve 1 at the bottom, the pH monitor probe and the particle morphology analyzer probe are respectively inserted through the side wall of the reactor body, the pH monitor probe is connected to the pH monitor, the particle morphology analyzer probe is connected to the particle morphology analyzer, and the pH monitor and the particle morphology analyzer are respectively connected to the metering and dosing component on the top of the reactor body through a controller 1;

[0009] The metering and dosing assembly includes four material troughs, a feed pipe and a metering valve; the bottoms of the four material troughs are connected to the top of the reactor body through the feed pipes, each feed pipe is provided with a metering valve for controlling the amount of material discharged, and each metering valve is electrically connected to a pH monitor and a particle morphology analyzer through a controller.

[0010] Furthermore, the monitoring ends of the pH monitor probe and the particle morphology analyzer probe are respectively located near the stirring paddle at the end of the stirrer.

[0011] Furthermore, the pH monitor probe and the particle morphology analyzer probe are respectively inserted obliquely near the bottom side wall of the reactor body, and the pH monitor probe and the particle morphology analyzer probe are respectively installed at an oblique angle of 15°-35°.

[0012] Furthermore, it also includes a temperature monitoring component, which is a thermocouple. The thermocouple is obliquely inserted into the side wall near the bottom of the reactor body, and the thermocouple probe extends into the reactor body. The thermocouple is connected to the air guide component that controls the introduction of hot air and cold air into the heating coil through controller 2.

[0013] Furthermore, the air guide component includes a refrigerator, a heating machine, a cold air duct, a hot air duct, valve two and valve three; the output end of the refrigerator is connected to the first air inlet of the heating coil through the cold air duct equipped with valve two, the heating machine is connected to the second air inlet of the heating coil through the hot air duct equipped with valve three, and valve two and valve three are respectively electrically connected to the thermocouple through controller two.

[0014] Furthermore, the inner wall of the reactor is provided with a raised ring for spreading the raw materials. The raised ring is provided with a cone structure, and the sharp end of the raised ring is provided away from the inner wall of the reactor.

[0015] Furthermore, the bottom of the reactor body is arranged in an arc-shaped structure, and the lowest end of the arc-shaped structure of the reactor body is connected with the discharge port.

[0016] Furthermore, the four material troughs are material trough A, material trough B, material trough C and material trough D respectively. Material trough A, material trough B and material trough C are used to hold powdered raw materials, and material trough D is used to hold liquid raw materials.

[0017] During the working process, first close the valve at the discharge port of the reactor body and stop the pH monitor and particle morphology analyzer probes. Then, refer to the parameters of the traditional ratio of ferric phosphate raw materials and set the metering valve corresponding to each material tank so that the amount of raw materials in each material tank entering the reactor body conforms to the traditional ratio. Then turn on the frequency-modulated motor to drive the agitator at a suitable speed to stir the mixed slurry in the reactor body so that each component of the raw materials can react fully.

[0018] After the pH monitor probe and particle shape analyzer probe are submerged in the slurry , so that the pH monitor and particle morphology analyzer probes start working. The pH monitor probes and particle morphology analyzer probes monitor the pH and particle morphology of the iron phosphate slurry synthesized in the reactor body, and the monitored information is transmitted back to the particle morphology analyzer and pH monitor.

[0019] If the monitored information does not meet the synthesis standards of iron phosphate slurry, the particle morphology analyzer and the pH monitor will adjust the parameters on the corresponding metering valve of each material tank through the controller, and re-introduce the proportion of one or two or three raw materials of iron phosphate into the reactor body, and re-mix them with the slurry pre-mixed in the reactor body to make the slurry in the reactor body more fully mixed, thereby further improving the quality of the iron phosphate slurry.

[0020] If the monitored information meets the synthesis standard of the iron phosphate slurry, valve 1 on the discharge port is opened to discharge the synthesized iron phosphate slurry out of the reactor body.

[0021] Compared with the prior art, the utility model has at least one of the following beneficial effects:

[0022] The utility model arranges a pH monitor probe and a particle morphology analyzer probe on the side wall of the reactor body, and the pH monitor probe is connected to the pH monitor, and the particle morphology analyzer probe is connected to the particle morphology analyzer. The pH monitor and the particle morphology analyzer are respectively connected to the metering and batching components on the top of the reactor body through a controller. In the process of synthesizing ferric phosphate, the pH monitor probe and the particle morphology analyzer probe can monitor the pH value of the ferric phosphate slurry and the morphology of the ferric phosphate particles, and then transmit the information back to the particle morphology analyzer and the pH monitor, and the particle morphology analyzer and the pH monitor can control the reaction. The metering and batching component on the top of the kettle body re-introduces the proportion of one or two or three raw materials of iron phosphate into the reactor body, and re-mixes them with the slurry pre-mixed in the reactor body to make the slurry in the reactor body more fully mixed, further improve the quality of the iron phosphate slurry, timely control and correct the particle size and morphology of the iron phosphate slurry, eliminate unnecessary raw and auxiliary consumption and reduce production costs, so as to solve the problem that during the synthesis process of iron phosphate slurry, the particle morphology and pH of iron phosphate cannot be corrected in time, resulting in unstable product performance and poor quality of the synthesized iron phosphate slurry. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a schematic diagram of the internal structure of the utility model.

[0024] Figure 2 It is a schematic diagram of the external structure of the utility model.

[0025] Figure 3 For the partial circuit control in the structure of the utility model Figure 1 .

[0026] Figure 4 For the partial circuit control in the structure of the utility model Figure 2 .

[0027] In the figure, 1-reactor body, 2-agitator, 3-heating coil, 4-frequency modulation motor, 5-discharging port, 6-pH monitor probe, 7-particle morphology analyzer probe, 8-feeding tank, 9-feeding pipe, 10-metering valve, 11-thermocouple, 12-refrigerating machine, 13-heating machine, 14-cold air duct, 15-hot air duct, 16-valve two, 17-valve three, 18-raised ring. DETAILED DESCRIPTION

[0028] like Figure 1-4 In order to make the purpose, technical solution and advantages of the utility model more clear, the utility model is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described here are only used to explain the utility model and are not used to limit the utility model. Example

[0029] See also Figure 1 and Figure 3 A ferric phosphate synthesis reactor body comprises a reactor body 1, an agitator 2, a heating coil 3, a pH monitor probe 6, a particle morphology analyzer probe 7 and a metering and dosing component; an agitator 2 connected to a frequency modulation motor 4 is arranged inside the reactor body 1, a heating coil 3 is sleeved between the outer wall and the inner wall of the reactor body 1, a discharge port 5 with a valve 1 is arranged at the bottom of the reactor body 1, a pH monitor probe 6 and a particle morphology analyzer probe 7 are respectively inserted through the side wall of the reactor body 1, the pH monitor probe 6 is connected to the pH monitor, the particle morphology analyzer probe 7 is connected to the particle morphology analyzer, and the pH monitor and the particle morphology analyzer are respectively connected to the metering and dosing component at the top of the reactor body 1 through a controller 1.

[0030] The metering and dosing assembly includes four material troughs 8, a feed pipe 9 and a metering valve 10; the bottoms of the four material troughs 8 are connected to the top of the reactor body 1 through the feed pipes 9, and each feed pipe 9 is provided with a metering valve 10 for controlling the amount of material discharged, and each metering valve 10 is electrically connected to the pH monitor and the particle morphology analyzer through a controller.

[0031] During operation, first close the valve of the discharge port 5 of the reactor body 1 and stop the pH monitor and the particle morphology analyzer probe 7, then refer to the parameters of the traditional ratio of the ferric phosphate raw materials, set the metering valve 10 corresponding to each material tank 8, so that the amount of raw materials in each material tank 8 entering the reactor body 1 conforms to the traditional ratio, and then turn on the frequency-modulated motor 4, so that the frequency-modulated motor 4 drives the stirrer 2 at a suitable speed to stir the mixed slurry in the reactor body 1, so that each component raw material can fully react.

[0032] After the pH monitor probe and particle shape analyzer probe are submerged in the slurry , so that the pH monitor and particle morphology analyzer probe 7 start working, the pH monitor probe 6 and the particle morphology analyzer probe 7 monitor the pH and particle morphology of the iron phosphate slurry synthesized in the reactor body 1, and the monitored information is transmitted back to the particle morphology analyzer and the pH monitor.

[0033] If the monitored information does not meet the synthesis standard of iron phosphate slurry, the particle morphology analyzer and the pH monitor will adjust the parameters on the corresponding metering valve 10 of each material tank 8 through the controller, and re-introduce the amount of one or two or three raw materials of the proportioned iron phosphate into the reactor body 1, and re-mix them with the slurry pre-mixed in the reactor body 1 to make the slurry in the reactor body 1 more fully mixed, thereby further improving the quality of the iron phosphate slurry.

[0034] If the monitored information meets the synthesis standard of the ferric phosphate slurry, the valve 1 on the discharge port 5 is opened to discharge the synthesized ferric phosphate slurry out of the reactor body 1 .

[0035] In this way, by penetrating the side wall of the reactor body 1 with a pH monitor probe 6 and a particle morphology analyzer probe 7, and the pH monitor probe 6 is connected to the pH monitor, the particle morphology analyzer probe 7 is connected to the particle morphology analyzer, and the pH monitor and the particle morphology analyzer are respectively connected to the metering and dosing component on the top of the reactor body 1 through the controller 1, the pH monitor probe 6 and the particle morphology analyzer probe 7 can monitor the pH value of the iron phosphate slurry and the morphology of the iron phosphate particles during the synthesis of iron phosphate, and then transmit them back to the particle morphology analyzer and the pH monitor, and the particle morphology analyzer and the pH monitor control the metering and dosing component on the top of the reactor body 1, re-introduce the amount of one raw material, two raw materials or three raw materials of the proportioned iron phosphate into the reactor body 1, and re-mix and synthesize with the slurry pre-mixed in the reactor body 1, so that the slurry in the reactor body 1 is mixed more fully, the quality of the iron phosphate slurry is further improved, the particle size and morphology of the iron phosphate slurry are timely controlled and corrected, and unnecessary raw and auxiliary consumption is eliminated and the production cost is reduced.

[0036] See also Figure 1 The monitoring end of the pH monitor probe 6 for monitoring the pH value of the ferric phosphate slurry and the monitoring end of the particle morphology analyzer probe 7 for monitoring the particle size and morphology of the ferric phosphate slurry are respectively located near the stirring paddle at the end of the agitator 2, so as to better monitor the pH value and particle morphology of the ferric phosphate slurry in the reactor body 1.

[0037] It should be noted that the pH monitor probe 6 and the particle morphology analyzer probe 7 are respectively inserted in an inclined manner near the bottom side wall of the reactor body 1, and the angles of the pH monitor probe 6 and the particle morphology analyzer probe 7 are respectively 15°-35°.

[0038] It should be noted that the pH monitor and the particle morphology analyzer are both existing technologies, and no improvement or design has been made thereto, so their structures are not described in detail.

[0039] It should be noted that the agitator 2 is rotatably connected to the reactor body 1 , and the agitator 2 includes a stirring shaft and a stirring paddle. The stirring shaft is rotatably connected to the reactor body 1 , and the stirring shaft is connected to the stirring paddle.

[0040] See also Figure 1 , Figure 2 and Figure 4 In order to monitor and adjust the temperature during the synthesis process of iron phosphate, a temperature monitoring device is also arranged on the side wall of the reactor body 1. The temperature monitoring device is a thermocouple 11, wherein the thermocouple 11 is obliquely inserted into the side wall near the bottom of the reactor body 1, and the thermocouple probe end extends into the reactor body 1. The thermocouple is connected to the air guide component that controls the introduction of hot air and cold air into the heating coil 3 through the controller 2.

[0041] Specifically, the air guide component for introducing cold air or hot air into the heating coil 3 includes a refrigerator 12, a heater 13, a cold air duct 14, a hot air duct 15, a second valve 16 and a third valve 17; wherein the refrigerator 12 is used to generate cold air; the cold air duct 14 is used to transport the cold air generated by the refrigerator 12; the second valve 16 is used to control the transport state of the cold air in the cold air duct 14; the heater 13 is used to generate hot air; the hot air duct 15 is used to transport the hot air generated by the heater 13; the third valve 17 is used to control the transport state of the hot air in the hot air duct 15.

[0042] More specifically, the output end of the refrigerator 12 is connected to the first air inlet of the heating coil 3 through a cold air duct 14 equipped with a valve 2 16, and the heating machine 13 is connected to the second air inlet of the heating coil 3 through a hot air duct 15 equipped with a valve 3 17. The valve 2 16 and the valve 3 17 are electrically connected to the thermocouple 11 through the controller 2 respectively.

[0043] In actual use, during the synthesis of iron phosphate slurry, if the thermocouple 11 detects that the temperature in the reactor body 1 is too high, the thermocouple 11 controls the valve 2 16 to open through the controller 2, and the cold air generated by the refrigerator 12 is introduced into the heating coil 3 by means of the cold air duct 14. The cold air in the heating coil 3 cools down the temperature in the reactor body 1 by heat conduction, so that the temperature in the reactor body 1 is at a suitable temperature for the reaction of the iron phosphate slurry, thereby indirectly improving the quality of the synthesis of the iron phosphate slurry.

[0044] If the thermocouple 11 detects that the temperature in the reactor body 1 is too low, the thermocouple 11 controls the valve 3 17 to open through the controller 2, and the hot air generated by the heater 13 is introduced into the heating coil 3 by means of the hot air conduit 15. The hot air in the heating coil 3 raises the temperature in the reactor body 1 by heat conduction, so that the temperature in the reactor body 1 is at a suitable temperature for the reaction of the ferric phosphate slurry, thereby indirectly improving the quality of the synthesis of the ferric phosphate slurry.

[0045] It should be noted that the refrigerator 12, the heater 13 and the thermocouple 11 are existing technologies, and no improvement or design has been made thereto, so their structures will not be described in detail.

[0046] It should be noted that in order to increase the flow rate of the gas discharged by the refrigerator 12 and the heater 13, a guide pump can be set on the cold air duct 14 and the hot air duct 15 to guide the cold air or hot air into the heating coil 3 in a short time with the help of the guide pump.

[0047] See also Figure 1In order to improve the fineness of the mixed slurry in the reactor body 1, a plurality of raised rings 18 for breaking up the raw materials are arranged on the inner wall of the reactor body 1, wherein the raised rings 18 are arranged as a cone structure, and the sharp end of the raised rings 18 is arranged toward the end away from the inner wall of the reactor body 1.

[0048] In actual use, the slurry in the reactor body 1 rotates in a vortex manner along the reactor body 1 under the stirring of the agitator 2. Since a raised ring 18 is provided on the inner wall of the reactor body 1, the sharp end of the raised ring 18 breaks up the mixed slurry rotating in a vortex manner, making the mixed slurry finer in particle size, thereby improving the mixing degree of the iron phosphate mixed slurry.

[0049] See also Figure 1 In order to discharge the iron phosphate slurry synthesized in the reactor body 1 from the reactor body 1 , the bottom of the reactor body 1 is arranged in an arc-shaped structure, and the lowest end of the arc-shaped structure of the reactor body 1 is connected to the discharge port 5 .

[0050] In actual use, after the iron phosphate slurry in the reactor body 1 is synthesized, the iron phosphate slurry flows along the arc-shaped inner surface at the bottom of the reactor body 1 to the lowest discharge port 5, and then the valve 1 on the discharge port 5 is opened, and the synthesized iron phosphate slurry is discharged from the discharge port 5.

[0051] See also Figure 1 and Figure 2 The four material troughs 8 for containing the synthetic ferric phosphate raw material are material trough A, material trough B, material trough C and material trough D. The material trough A, material trough B, material trough C and material trough D are all rectangular groove structures, wherein:

[0052] The material tank A, material tank B and material tank C are used to hold the powdered raw materials for preparing ferric phosphate, and the material tank D is used to hold the liquid raw materials for preparing ferric phosphate.

[0053] In actual application, in the early stage of synthesizing iron phosphate, the three powdered raw materials used to synthesize iron phosphate are loaded into trough A, trough B and trough C in advance, and the liquid raw materials are loaded into trough D, to assist the subsequent powdered raw materials and liquid raw materials to be introduced into the reactor body 1 for the process of synthesizing iron phosphate slurry.

[0054] Although the utility model is described herein with reference to a plurality of illustrative embodiments of the utility model, it should be understood that those skilled in the art may devise many other modifications and implementations that fall within the scope and spirit of the principles disclosed herein. More specifically, within the scope of the disclosure, drawings, and claims of the present application, various modifications and improvements may be made to the components and / or layout of the subject combination layout. In addition to the modifications and improvements made to the components and / or layout, other uses will also be apparent to those skilled in the art.

Claims

1. A ferric phosphate synthesis reactor, comprising a reactor body (1), an agitator (2) and a heating coil (3); the reactor body (1) is provided with an agitator (2) connected to a frequency modulation motor (4), the heating coil (3) is sleeved between the outer wall and the inner wall of the reactor body (1), and the bottom of the reactor body (1) is provided with a discharge port (5) with a valve 1; the characteristics are as follows: It also includes a pH monitor probe (6), a particle morphology analyzer probe (7) and a metering and dosing component; The pH monitor probe (6) and the particle morphology analyzer probe (7) are respectively inserted through the side wall of the reactor body (1); the pH monitor probe (6) is connected to the pH monitor, and the particle morphology analyzer probe (7) is connected to the particle morphology analyzer; the pH monitor and the particle morphology analyzer are respectively connected to the metering and dosing component on the top of the reactor body (1) via controller 1; The metering and dosing assembly comprises four material storage tanks (8), a feed pipe (9) and a metering valve (10); the bottoms of the four material storage tanks (8) are connected to the top of the reaction kettle body (1) via the feed pipes (9), each feed pipe (9) is provided with a metering valve (10) for controlling the amount of material discharged, and each metering valve (10) is electrically connected to a pH monitor and a particle morphology analyzer via a controller 1.

2. The ferric phosphate synthesis reactor according to claim 1, characterized in that: The monitoring ends of the pH monitor probe (6) and the particle morphology analyzer probe (7) are respectively located near the stirring paddle at the end of the stirrer (2).

3. A ferric phosphate synthesis reactor according to claim 2, characterized in that: The pH monitor probe (6) and the particle morphology analyzer probe (7) are respectively inserted in an inclined manner near the bottom side wall of the reaction kettle body (1), and the inclined installation angles of the pH monitor probe (6) and the particle morphology analyzer probe (7) are respectively 15°-35°.

4. The ferric phosphate synthesis reactor according to claim 1, characterized in that: It also includes a temperature monitoring component, which is a thermocouple (11). The thermocouple (11) is obliquely plugged into the side wall near the bottom of the reactor body (1). The thermocouple probe extends into the reactor body (1). The thermocouple is connected to an air guide component that controls the introduction of hot air and cold air into the heating coil (3) through controller 2.

5. The ferric phosphate synthesis reactor according to claim 4, characterized in that: The air guide assembly comprises a refrigerator (12), a heater (13), a cold air conduit (14), a hot air conduit (15), a second valve (16) and a third valve (17); the output end of the refrigerator (12) is connected to a first air inlet of the heating coil (3) via the cold air conduit (14) equipped with the second valve (16); the heating machine (13) is connected to a second air inlet of the heating coil (3) via the hot air conduit (15) equipped with the third valve (17); the second valve (16) and the third valve (17) are electrically connected to the thermocouple (11) via the second controller.

6. The ferric phosphate synthesis reactor according to claim 1, characterized in that: The inner wall of the reaction kettle body (1) is provided with a raised ring (18) for spreading the raw materials. The raised ring (18) is provided with a cone structure, and the sharp end of the raised ring (18) is provided towards an end away from the inner wall of the reaction kettle body (1).

7. The ferric phosphate synthesis reactor according to claim 1, characterized in that: The bottom of the reactor body (1) is arranged in an arc-shaped structure, and the lowest end of the arc-shaped structure of the reactor body (1) is connected to the discharge port (5).

8. The ferric phosphate synthesis reactor according to claim 1, characterized in that: The four material troughs (8) are respectively material trough A, material trough B, material trough C and material trough D. Material trough A, material trough B and material trough C are used to hold powdered raw materials, and material trough D is used to hold liquid raw materials.

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