Continuous manufacturing device and preparation method of modified sodium vanadium fluorophosphate

By designing a continuous manufacturing device for modified sodium vanadium fluorophosphate, and using a metering pipe and metering pump to control the concentration and feed rate of the mixed solution, the problems of discontinuous production and inconsistent concentration of Na3V(2-x)Nix(PO4)3F3 material in the prior art have been solved, and efficient and stable material preparation has been achieved.

CN121944978APending Publication Date: 2026-05-01GUIZHOU UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
GUIZHOU UNIV
Filing Date
2026-02-28
Publication Date
2026-05-01

AI Technical Summary

Technical Problem

In existing technologies, the preparation of mixed solutions of NH4VO3, NH4H2PO4 and C6H8O7 is mostly done manually, requiring strict adherence to the mixing sequence. This results in significant batch-to-batch variations, affecting subsequent processes and causing discontinuous production and inconsistent concentrations of Na3V(2-x)Nix(PO4)3F3 material.

Method used

A continuous manufacturing apparatus for modified sodium vanadium fluorophosphate was designed, comprising a frame, a main reaction vessel, a dispersed phase reaction vessel, and a continuous phase reaction vessel. The concentration of the mixed solution, the feed rate, and the reaction temperature are controlled by a metering pipe and a metering pump to achieve continuous production of Na3V(2-x)Nix(PO4)3F3.

Benefits of technology

Continuous production of Na3V(2-x)Nix(PO4)3F3 material was achieved, avoiding production waste caused by incorrect mixing sequence, ensuring product concentration consistency, and improving production efficiency and product quality.

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Abstract

The invention discloses a continuous manufacturing device and a preparation method of modified sodium vanadium fluorophosphate, and relates to the field of continuous preparation of modified sodium vanadium fluorophosphate, and the continuous manufacturing device comprises a frame which is provided with a first support, a second support and a third support, and the supports are used for fixing corresponding reaction tanks; the total reaction tank is mounted on the first bracket; the dispersed phase reaction tank is mounted on the second bracket; the continuous phase reaction tank is mounted on the third bracket; one quantitative conveying pipe is communicated with the total reaction tank and the dispersed phase reaction tank, and the other quantitative conveying pipe is communicated with the total reaction tank and the continuous phase reaction tank; according to the device, continuous production of Na3V (2-x) Nix (PO4) 3F3 can be realized through cooperative work of multiple tank bodies.
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Description

Continuous manufacturing apparatus and preparation method for modified sodium vanadium fluorophosphate Technical Field

[0001] This invention relates to the field of continuous preparation of modified sodium vanadium fluorophosphate, specifically a continuous manufacturing apparatus and preparation method for modified sodium vanadium fluorophosphate. Background Technology

[0002] Na3V (2-x) Ni x (PO4)3F3@C cathode material is used in the button cell process of sodium-ion batteries. It has high operating voltage, good rate performance, excellent structural stability and long cycle life. At the same time, the low conductivity problem is solved by carbon coating. It is a very promising sodium battery cathode material.

[0003] By reacting a mixed solution of NH4VO3, NH4H2PO4, and C6H8O7 with a certain proportion of a mixed solution of Ni(CH3COO)2 and NaF, and controlling the reactant concentration, feed rate, and reaction temperature (80 ℃), Na3V can be achieved. (2-x) Ni x The continuous production of (PO4)3F3 (precursor) involves calcining the synthesized precursor at 650 °C for 8 h to obtain Na3V. (2-x) Ni x (PO4)3F3@C cathode material.

[0004] Currently, the preparation of mixed solutions of NH4VO3, NH4H2PO4 and C6H8O7 is mostly done manually. The mixing order must be strictly followed during the preparation process, and the solution must be prepared and used immediately. Moreover, the concentration of manually prepared solutions varies greatly from batch to batch, which directly affects subsequent processes. Summary of the Invention

[0005] To address the above problems, the present invention provides the following technical solution: a continuous manufacturing apparatus for modified sodium vanadium fluorophosphate, comprising:

[0006] The frame is provided with a first support, a second support and a third support, all of which are used to fix the corresponding reaction vessel;

[0007] The main reaction vessel is mounted on the first support;

[0008] A dispersed phase reaction vessel, which is mounted on the second support;

[0009] A continuous phase reaction vessel, which is mounted on the third support;

[0010] Two quantitative delivery pipes, one of which connects the total reaction vessel and the dispersed phase reaction vessel, and the other connects the total reaction vessel and the continuous phase reaction vessel.

[0011] Furthermore, as a preferred embodiment, the upper end of the dispersed phase reaction vessel is provided with a Ni(CHCOO)2 inlet pipe communicating with the inner cavity and a NaF inlet pipe symmetrically arranged with the Ni(CHCOO)2 inlet pipe.

[0012] Furthermore, as a preferred embodiment, the quantitative delivery pipe is equipped with a metering pump.

[0013] Further, preferably, the continuous phase reaction vessel includes:

[0014] Outer can;

[0015] A temperature-controlled container is disposed inside the outer container, and a heat flow pipe is provided at the lower end of the temperature-controlled container;

[0016] The first reaction vessel is located inside the temperature control vessel. The upper end of the first reaction vessel is provided with an NH4VO3 material pipe and a first liquid supply pipe, and the NH4VO3 material pipe and the first liquid supply pipe are arranged symmetrically. The lower inner wall of the first reaction vessel is provided with a first fixing buckle.

[0017] The second reaction vessel is located between the temperature control vessel and the outer vessel. Multiple spiral tubes are arranged in a circumferential array at the bottom of the second reaction vessel. The other end of each spiral tube is connected to the first reaction vessel. The spiral tubes are encircled around the second reaction vessel. An NH4H2PO4 feed pipe and a second liquid supply pipe are provided at the upper end of the second reaction vessel. The NH4H2PO4 feed pipe and the second liquid supply pipe are arranged symmetrically.

[0018] The third reaction vessel is located inside the first reaction vessel. The upper end of the third reaction vessel is provided with a C6H8O7 material pipe and a third liquid supply pipe. The C6H8O7 material pipe and the third liquid supply pipe are arranged symmetrically. The lower inner wall of the third reaction vessel is provided with a second fixing buckle.

[0019] The batching components are disposed between the third reaction vessel and the second reaction vessel;

[0020] The first base plate is fixedly mounted on the second fixing buckle;

[0021] The second base plate is fixedly mounted on the first fixing buckle.

[0022] Further, preferably, the batching component includes:

[0023] The inclined bottom tube has an annular flange on the outer wall of its straight section.

[0024] A movable ring is provided at the lower end of the inclined bottom tube. Multiple reciprocating rods are provided between the movable ring and the annular flange, and the reciprocating rods are covered with an isolation membrane.

[0025] An elastic ring is disposed between the inclined bottom tube and the movable ring.

[0026] Further, as a preferred embodiment, the first base plate includes:

[0027] The upper cover plate has multiple flanges A arranged in a circumferential array on its outer wall, and a first pin is provided at the lower end of each flange A.

[0028] A sieve, which is slidably disposed within the upper cover plate;

[0029] The lower cover plate has multiple flanges B arranged in a circumferential array on its outer wall. A second pin is provided at the upper end of each flange B. The lower cover plate has through holes that coincide with the mesh openings of the screen.

[0030] Multiple guide plates, one end of which is provided with a gradient hole as a movable end, the movable end being sleeved around the first pin, and the other end of which is provided with a round hole as a fixed end, the fixed end being sleeved around the second pin;

[0031] Multiple springs are disposed between the movable end of the guide plate and the flange A;

[0032] The gap between flange A and flange B is provided with an elastic contraction member and a universal reset rod.

[0033] Furthermore, as a preferred embodiment, the first base plate and the second base plate divide the first reaction vessel into a pre-dissolving chamber, a first reaction chamber, and a second reaction chamber.

[0034] A continuous preparation method for modified sodium vanadium fluorophosphate includes the following steps:

[0035] S1. Water at 60-80℃ is injected into the temperature-controlled tank through a hot flow pipe to provide a uniform temperature environment for the dissolution and reaction of NH4VO3, NH4H2PO4 and C6H8O7;

[0036] S2. Prepare C6H8O7 solution in the third reaction vessel, NH4VO3 solution in the pre-dissolution chamber of the first reaction vessel, and NH4H2PO4 solution in the second reaction vessel; prepare a mixed solution of Ni(CH3COO)2 and NaF in the dispersed phase reaction vessel 2;

[0037] S3.C6H8O7 solution is mixed with NH4VO3 solution passing through batch assembly in the first reaction chamber of the first reaction vessel through the first bottom plate to generate a mixed solution of NH4VO3 and C6H8O7.

[0038] S4. The mixed solution of NH4VO3 and C6H8O7 through the second bottom plate reacts with the NH4H2PO4 solution in the second reaction chamber of the first reaction vessel to generate a mixed solution of NH4VO3, NH4H2PO4 and C6H8O7.

[0039] S5. A quantitative delivery pipe transports the prepared mixed solution of NH4VO3, NH4H2PO4, and C6H8O7, along with a mixed solution of Ni(CH3COO)2 and NaF, into the main reaction tank. The process conditions, including the concentration of the two mixed solutions, the feed rate, and the reaction temperature of 80 ℃, are controlled to produce Na3V. (2-x) Nix(PO4)3F3.

[0040] Compared with the prior art, the present invention provides a continuous manufacturing apparatus and preparation method for modified sodium vanadium fluorophosphate, which has the following beneficial effects:

[0041] This device can achieve Na3V if the mixing sequence is strictly followed. (2-x) Ni x The continuous production of (PO4)3F3 effectively avoids production waste caused by incorrect mixing sequence, and the Na3V prepared by this device... (2-x) Ni x (PO4)3F3 does not exhibit concentration differences between batches. Attached Figure Description

[0042] Figure 1 is a three-dimensional structural schematic diagram of a continuous manufacturing apparatus for modified sodium vanadium fluorophosphate;

[0043] Figure 2 is a schematic diagram of the continuous phase reaction vessel in a continuous manufacturing apparatus for modified sodium vanadium fluorophosphate.

[0044] Figure 3 is a schematic diagram of the structure of the first bottom plate in the continuous phase reaction vessel;

[0045] Figure 4. Partial structural diagram of the first base plate;

[0046] Figure 5 is a schematic diagram of the batch assembly in the continuous phase reactor;

[0047] Figure 6 shows the changes in the working status of the batch components;

[0048] Figure 7 is a flowchart of a continuous preparation method for modified sodium vanadium fluorophosphate.

[0049] In the diagram: 1. Main reaction vessel;

[0050] 2. Dispersed phase reaction vessel; 21. Ni(CH3COO)2 inlet pipe; 22. NaF inlet pipe;

[0051] 3. Continuous phase reaction vessel; 31. Outer vessel; 32. Temperature control vessel; 321. Hot flow tube; 33. First reaction vessel; 331. NH4VO3 feed pipe; 332. First liquid supply pipe; 333. First fixing buckle; 34. Second reaction vessel; 341. NH4H2PO4 feed pipe; 342. Second liquid supply pipe; 343. Spiral tube; 35. Batch assembly; 351. Inclined bottom tube; 352. Elastic ring; 353. Movable ring; 354. Separating membrane; 35 5. Shaker; 36. Third reaction vessel; 361. C6H8O7 feed pipe; 362. Third liquid supply pipe; 363. Second fixing buckle; 37. First base plate; 371. Upper cover plate; 372. Lower cover plate; 373. Elastic shrinking component; 374. Universal return rod; 375. Spring; 376. Guide plate; 3761. Gradient hole; 3762. Round hole; 377. Sieve plate; 378. First pin; 379. Second pin; 38. Second base plate;

[0052] 4. Precursor fluid pipe;

[0053] 5. Frame; 51. First support; 52. Second support; 53. Third support. Detailed Implementation

[0054] The terms "first," "second," etc., used in the specification, claims, and accompanying drawings of this application are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such terms are interchangeable where appropriate; this is merely a distinguishing method used to describe objects with the same attributes in the embodiments of this application. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusion, so that a process, method, system, product, or apparatus that comprises a series of elements is not necessarily limited to those elements but may include other elements not explicitly listed or inherent to those processes, methods, products, or apparatuses.

[0055] Example: Referring to Figures 1-7, in this embodiment of the invention, a continuous manufacturing apparatus for modified sodium vanadium fluorophosphate is provided, comprising:

[0056] The frame 5 is provided with a first support 51, a second support 52 and a third support 53, all of which are used to fix the corresponding reaction vessel.

[0057] The main reaction vessel 1 is mounted on the first support 51. The main reaction vessel 1 is a reaction vessel for a mixed solution of NH4VO3, NH4H2PO4 and C6H8O7 and a mixed solution of Ni(CH3COO)2 and NaF.

[0058] Dispersed phase reaction vessel 2, which is mounted on the second support 52, is a production vessel for a mixed solution of Ni(CH3COO)2 and NaF;

[0059] The continuous phase reaction vessel 3 is mounted on the third support 53. The continuous phase reaction vessel 3 is a production vessel for a mixed solution of NH4VO3, NH4H2PO4 and C6H8O7.

[0060] Two quantitative delivery pipes 4, one of which connects the total reaction vessel 1 and the dispersed phase reaction vessel 2, and the other connects the total reaction vessel 1 and the continuous phase reaction vessel 3.

[0061] In the preparation of Na3V using this device (2-x) Ni x When (PO4)3F3 is prepared, the required mixed solution of NH4VO3, NH4H2PO4, and C6H8O7 is prepared in the continuous phase reaction vessel 3 and then introduced into the main reaction vessel 1 through the continuous phase inlet via the quantitative conveying pipe 4. The mixed solution of Ni(CH3COO)2 and NaF is prepared in the dispersed phase reaction vessel 2 and then introduced into the main reaction vessel 1 through the dispersed phase inlet via the quantitative conveying pipe 4. The concentrations of the two mixed solutions, the feed rate, and the reaction temperature (80 ℃) are controlled to achieve Na3V (2-x) Continuous production of Nix(PO4)3F3.

[0062] Furthermore, the upper end of the dispersed phase reaction vessel 2 is provided with a Ni(CH3COO)2 inlet pipe communicating with the inner cavity and a NaF inlet pipe 22 symmetrically arranged with the Ni(CH3COO)2 inlet pipe.

[0063] In the specific preparation process, the pre-dissolved Ni(CH3COO)2 solution and NaF solution are introduced into the dispersed phase reaction vessel 2 through the corresponding inlet pipe, and the mixing reaction is completed in the dispersed phase reaction vessel 2.

[0064] It should be noted that the quantitative delivery pipe 4 is equipped with a metering pump to control the dosage of the solution poured into the total reaction tank 1.

[0065] In this embodiment, please refer to Figure 2. The continuous phase reaction vessel 3 includes:

[0066] The outer tank 31 is used to support and protect the internal structure of the continuous phase reaction vessel 3;

[0067] Temperature control tank 32 is fixedly installed inside the outer tank 31. A heat flow pipe 321 is provided at the lower end of the temperature control tank 32. The heat flow pipe 321 controls the reaction temperature in the continuous phase reaction tank 3 by controlling the temperature of the circulating liquid introduced into the temperature control tank 32.

[0068] The first reaction vessel 33 is disposed inside the temperature control vessel 32. The upper end of the first reaction vessel 33 is provided with an NH4VO3 material pipe 331 and a first liquid supply pipe 332, and the NH4VO3 material pipe 331 and the first liquid supply pipe 332 are symmetrically arranged. The lower end of the inner wall of the first reaction vessel 33 is provided with a first fixing buckle 333.

[0069] The second reaction vessel 34 is disposed between the temperature control vessel 32 and the outer vessel 31, and multiple spiral tubes 343 are arranged in a circumferential array at the bottom end of the second reaction vessel 34. The other end of the spiral tubes 343 is connected to the first reaction vessel 33. The spiral tubes 343 are wrapped around the periphery of the second reaction vessel 34. The pipeline connecting the spiral tubes 343 and the first reaction vessel 33 is Z-shaped, and the Z-shaped pipeline is disposed inside the temperature control vessel 32.

[0070] The upper end of the second reaction vessel 34 is provided with an NH4H2PO4 feed pipe 341 and a second liquid supply pipe 342, and the NH4H2PO4 feed pipe 341 and the second liquid supply pipe 342 are arranged symmetrically. The second reaction vessel 34 is used to prepare NH4H2PO4 solution.

[0071] It should be noted that NH4H2PO4 is readily soluble in water, and its solubility increases dramatically with increasing temperature. When the NH4H2PO4 solution prepared in the second reaction vessel 34 is introduced into the first reaction vessel 33 along the spiral tube 343, the solubility of residual NH4H2PO4 in the NH4H2PO4 solution increases as it flows through the Z-shaped pipeline, which can effectively prevent the spiral tube 343 from becoming clogged due to insufficient dissolution of NH4H2PO4 particles.

[0072] The third reaction vessel 36 is disposed inside the first reaction vessel 33. The upper end of the third reaction vessel 36 is provided with a C6H8O7 material pipe 361 and a third liquid supply pipe 362. The C6H8O7 material pipe 361 and the third liquid supply pipe 362 are symmetrically arranged. The lower end of the inner wall of the third reaction vessel 36 is provided with a second fixing buckle 363. The third reaction vessel 36 is used to prepare C6H8O7 solution.

[0073] The batching component 35 is disposed between the third reaction vessel 36 and the second reaction vessel 34;

[0074] The first base plate 37 is fixedly mounted on the second fixing buckle 363;

[0075] The second base plate 38 is fixedly mounted on the first fixing buckle 333, and a locking component is provided between the second base plate 38 and the first fixing buckle 333.

[0076] It should be noted that the first base plate 27 and the second base plate 28 have the same structure.

[0077] The first base plate 37 and the second base plate 38 divide the first reaction vessel into a pre-dissolution chamber, a first reaction chamber, and a second reaction chamber; the liquid supply pipes are all used to introduce deionized water to dissolve the corresponding raw materials.

[0078] The preparation of a mixed solution of NH4VO3, NH4H2PO4, and C6H8O7 using this apparatus can be divided into the following stages:

[0079] During the preparation stage, water at 60-80°C is added to the temperature control tank 32 through the heat pipe 321 to provide a uniform temperature environment for the dissolution and reaction of NH4VO3, NH4H2PO4 and C6H8O7, thereby improving production efficiency.

[0080] In the pre-dissolution stage, C6H8O7 is introduced into the third reaction tank 36 through the C6H8O7 feed pipe 361 according to a preset ratio and mixed with deionized water introduced through the third liquid supply pipe 362. A C6H8O7 solution is generated under the catalysis of the temperature-controlled tank 32. Similarly, NH4VO3 is introduced into the pre-dissolution chamber of the first reaction tank 33 through the NH4VO3 feed pipe 331 and mixed with deionized water introduced through the first liquid supply pipe 332. An NH4VO3 solution is generated under the catalysis of the temperature-controlled tank 32. Finally, NH4H2PO4 is introduced into the second reaction tank 34 through the NH4H2PO4 feed pipe 341 and mixed with deionized water introduced through the second liquid supply pipe 342. An NH4H2PO4 solution is generated under the catalysis of the temperature-controlled tank 32.

[0081] In the first reaction stage, when the amount of pre-dissolved C6H8O7 solution generated reaches the threshold of the first bottom plate 37, the bottom C6H8O7 solution in the third reaction tank 36 will flow into the first reaction chamber of the first reaction tank 33 through the first bottom plate 37; when the amount of pre-dissolved NH4VO3 solution generated reaches the threshold, the first liquid level sensor 334 is triggered; when the amount of C6H8O7 solution stored in the first reaction chamber reaches the threshold, the second liquid level sensor 335 is triggered, the batching component 35 is started, and the NH4VO3 solution in the pre-dissolved chamber is added in batches to the first reaction chamber to mix with the C6H8O7 solution;

[0082] In other words, the first base plate 37 is not closed until the amount of pre-dissolved C6H8O7 solution generated reaches the first threshold; the batching component 35 will only start when both the first liquid level sensor 334 and the second liquid level sensor 335 are triggered.

[0083] In the second reaction stage, when the mixed solution of NH4VO3 and C6H8O7 in the first reaction chamber turns blue-green or dark blue after the reaction, the color sensor 336 is triggered, the locking component is released, and the second base plate 38 becomes active. When the amount of the mixed solution of NH4VO3 and C6H8O7 in the first reaction chamber reaches the threshold of the second base plate 38, the second base plate 38 becomes open, allowing the solution to enter the second reaction chamber.

[0084] In other words, the second base plate 38 will only be turned on when the color sensor 336 is triggered and the amount of the mixed solution of NH4VO3 and C6H8O7 reaches a threshold.

[0085] In the third reaction stage, the NH4H2PO4 solution in the second reaction vessel 24 is introduced into the second reaction chamber along the spiral tube 343 and mixed with the mixed solution of NH4VO3 and C6H8O7 to generate a mixed solution of NH4VO3, NH4H2PO4 and C6H8O7.

[0086] Further, referring to Figures 5 and 6, the batching component 35 includes:

[0087] The inclined bottom tube 351 has an annular flange on the outer wall of its straight tube section.

[0088] A movable ring 353 is disposed at the lower end of the inclined bottom tube 351. Multiple reciprocating rods 355 are disposed between the movable ring 353 and the annular flange, and the reciprocating rods 355 are covered with an isolation membrane 354 to protect the reciprocating rods 355.

[0089] An elastic ring 352 is disposed between the inclined bottom tube 351 and the movable ring 353.

[0090] In the specific implementation process, when the batching component 35 is started, the reciprocating rod 355 extends and retracts, driving the movable ring 353 to rise and fall. One rise and one fall constitutes one batch. The time interval of the extension and retraction of the reciprocating rod 355 can be changed according to the needs to achieve control of the NH4VO3 solution addition efficiency.

[0091] Further, referring to Figure 3, the first base plate 37 includes:

[0092] The upper cover plate 371 has multiple flanges A arranged in a circumferential array on its outer wall, and a first pin 378 is provided at the lower end of the flanges A.

[0093] The screen 377 is slidably disposed within the upper cover plate 371;

[0094] The lower cover plate 372 has multiple flanges B arranged in a circumferential array on its outer wall. A second pin 379 is provided at the upper end of the flange B. The lower cover plate has through holes that overlap with the sieve holes of the screen 377. The lower cover plate 372 is fixedly mounted on the first fixing buckle 333.

[0095] Multiple guide plates 376, one end of which is provided with a gradient hole 3761 as a movable end, the movable end being sleeved around the first pin 378, and the other end is provided with a round hole 3762 as a fixed end, the fixed end being sleeved around the second pin 379;

[0096] Multiple springs 375 are disposed between the movable end of the guide plate 376 and the flange A;

[0097] An elastic contraction member 373 and a universal reset rod 374 are provided in the gap between flange A and flange B.

[0098] It should be noted that the screen 377 is always attached to the lower cover plate 372. In the initial state, the screen holes of the screen 377 and the through holes of the lower cover plate 372 are misaligned and overlapped.

[0099] In the specific implementation process, the first base plate 37 has the following two states:

[0100] In the semi-open state, when the pre-dissolved amount of C6H8O7 solution reaches the first threshold of the upper cover plate 371, the upper cover plate 371 is pressed down, the first pin 378 is pressed down to the first step, the elastic shrink member 373 shrinks and pulls the upper cover plate 371 to rotate, and the sieve holes of the screen 377 overlap with the through holes of the lower cover plate 372 by 1 / 2;

[0101] In the fully open / closed state, when the pre-dissolved amount of C6H8O7 solution reaches the second threshold of the upper cover plate 371, the upper cover plate 371 continues to press down, the first pin 378 is pressed down to the second step, the elastic contraction member 373 contracts again to pull the upper cover plate 371 to rotate, and the sieve holes of the screen 377 completely overlap with the through holes of the lower cover plate 372.

[0102] It should be noted that during the downward rotation of the upper cover plate 371, the universal reset rod 374 is in a standby state and will retract with the contraction of the elastic contraction member 373. After the C6H8O7 solution above the first base plate 37 is drained, the universal reset rod 374 is activated and pushed the upper cover plate 371 to rotate in the opposite direction to reset.

[0103] A continuous preparation method for modified sodium vanadium fluorophosphate, please refer to Figure 7, includes the following steps:

[0104] S1. Water at 60-80℃ is injected into the temperature control tank 32 through the heat flow pipe 321 to provide a uniform temperature environment for the dissolution and reaction of NH4VO3, NH4H2PO4 and C6H8O7;

[0105] S2. Prepare C6H8O7 solution in the third reaction vessel 36, prepare NH4VO3 solution in the pre-dissolution chamber of the first reaction vessel 33, and prepare NH4H2PO4 solution in the second reaction vessel 34; prepare a mixed solution of Ni(CH3COO)2 and NaF in the dispersed phase reaction vessel 2;

[0106] S3.C6H8O7 solution is mixed with NH4VO3 solution passing through batch assembly 35 in the first reaction chamber of first reaction vessel 33 through first bottom plate 37 to generate NH4VO3 and C6H8O7 mixed solution;

[0107] S4. The mixed solution of NH4VO3 and C6H8O7 through the second bottom plate 38 reacts with the NH4H2PO4 solution in the second reaction chamber of the first reaction vessel 33 to generate a mixed solution of NH4VO3, NH4H2PO4 and C6H8O7.

[0108] S5. Quantitative delivery pipe 4 delivers the prepared mixed solution of NH4VO3, NH4H2PO4, and C6H8O7, along with the mixed solution of Ni(CH3COO)2 and NaF, into the main reaction tank 1. The process conditions, including the concentration of the two mixed solutions, the feed rate, and the reaction temperature of 80 ℃, are controlled to produce Na3V. (2-x) Nix(PO4)3F3.

[0109] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A continuous manufacturing apparatus for modified sodium vanadium fluorophosphate, characterized in that, include: The frame (5) is provided with a first support (51), a second support (52) and a third support (53), all of which are used to fix the corresponding reaction vessels; the main reaction vessel (1) is installed on the first support (51); the dispersed phase reaction vessel (2) is installed on the second support (52); the continuous phase reaction vessel (3) is installed on the third support (53); and two quantitative delivery pipes (4), one of which connects the main reaction vessel (1) and the dispersed phase reaction vessel (2), and the other connects the main reaction vessel (1) and the continuous phase reaction vessel (3).

2. The continuous manufacturing apparatus for modified sodium vanadium fluorophosphate according to claim 1, characterized in that, The upper end of the dispersed phase reaction vessel (2) is provided with a Ni(CH) container that connects to the inner cavity. (3) COO)2 inlet pipe and the Ni(CH) (3) NaF inlet pipes (22) are symmetrically arranged with COO)2 inlet pipes.

3. The continuous manufacturing apparatus for modified sodium vanadium fluorophosphate according to claim 1, characterized in that, The metering pipe (4) is equipped with a metering pump.

4. The continuous manufacturing apparatus for modified sodium vanadium fluorophosphate according to claim 1, characterized in that, The continuous phase reaction vessel (3) includes: an outer vessel (31); a temperature control vessel (32) disposed inside the outer vessel (31), with a heat flow pipe (321) at the lower end of the temperature control vessel (32); a first reaction vessel (33) disposed inside the temperature control vessel (32), with an NH4VO3 feed pipe (331) and a first liquid supply pipe (332) at the upper end of the first reaction vessel (33), and the NH4VO3 feed pipe (331) and the first liquid supply pipe (332) being symmetrically arranged, and a first fixing buckle (333) being provided on the inner wall of the lower end of the first reaction vessel (33); and a second reaction vessel (34) disposed between the temperature control vessel (32) and the outer vessel (31), with multiple spiral tubes (343) arranged in a circumferential array at the bottom end of the second reaction vessel (34), the other end of the spiral tubes (343) being connected to the first reaction vessel (33), and the spiral tubes (343) being looped around the second reaction vessel. (34) The second reaction tank (34) is provided with an NH4H2PO4 feed pipe (341) and a second liquid supply pipe (342) at its upper end, and the NH4H2PO4 feed pipe (341) and the second liquid supply pipe (342) are arranged symmetrically; the third reaction tank (36) is provided inside the first reaction tank (33), and the third reaction tank (36) is provided with a C6H8O7 feed pipe (361) and a third liquid supply pipe (362) at its upper end, and the C6H8O7 feed pipe (361) and the third liquid supply pipe (362) are arranged symmetrically, and the lower inner wall of the third reaction tank (36) is provided with a second fixing buckle (363); the batching assembly (35) is provided between the third reaction tank (36) and the second reaction tank (34); the first bottom plate (37) is fixedly provided on the second fixing buckle (363); the second bottom plate (38) is fixedly provided on the first fixing buckle (333).

5. The continuous manufacturing apparatus for modified sodium vanadium fluorophosphate according to claim 4, characterized in that, The batching assembly (35) includes: a sloping bottom tube (351), the outer wall of which is provided with an annular flange; a movable ring (353), which is disposed at the lower end of the sloping bottom tube (351), and multiple reciprocating rods (355) are disposed between the movable ring (353) and the annular flange, and the reciprocating rods (355) are covered with an isolation membrane (354); and an elastic ring (352), which is disposed between the sloping bottom tube (351) and the movable ring (353).

6. The continuous manufacturing apparatus for modified sodium vanadium fluorophosphate according to claim 4, characterized in that, The first base plate (37) includes: an upper cover plate (371) with multiple flanges A arranged in a circumferential array on its outer wall, and a first pin (378) provided at the lower end of the flanges A; a screen (377) slidably disposed within the upper cover plate (371); a lower cover plate (372) with multiple flanges B arranged in a circumferential array on its outer wall, and a second pin (379) provided at the upper end of the flanges B, and the lower cover plate having through holes that overlap with the sieve holes of the screen (377); and multiple A guide plate (376) has a gradient hole (3761) at one end as a movable end, which is sleeved around the first pin (378), and a round hole (3762) at the other end as a fixed end, which is sleeved around the second pin (379); a plurality of springs (375) are disposed between the movable end of the guide plate (376) and the flange A; wherein, an elastic contraction member (373) and a universal reset rod (374) are disposed in the gap between the flange A and the flange B.

7. The continuous manufacturing apparatus for modified sodium vanadium fluorophosphate according to claim 4, characterized in that, The first base plate (37) and the second base plate (38) divide the first reaction vessel into a pre-dissolution chamber, a first reaction chamber, and a second reaction chamber.

8. A continuous preparation method for modified sodium vanadium fluorophosphate, comprising using the manufacturing apparatus as described in any one of claims 1-7, characterized in that, The steps include: S1. Water at 60-80°C is injected into the temperature-controlled container (32) through the heat pipe (321) to provide a uniform temperature environment for the dissolution and reaction of NH4VO3, NH4H2PO4 and C6H8O7; S2. Prepare C6H8O7 solution in the third reaction vessel (36), prepare NH4VO3 solution in the pre-dissolution chamber of the first reaction vessel (33), and prepare NH4H2PO4 solution in the second reaction vessel (34); prepare a mixed solution of Ni(CH3COO)2 and NaF in the dispersed phase reaction vessel 2; S3. Mix the C6H8O7 solution with the NH4VO3 solution passing through the batching component (35) in the first reaction chamber of the first reaction vessel (33) to generate a mixed solution of NH4VO3 and C6H8O7; S4. The mixed solution of NH4VO3 and C6H8O7 through the second bottom plate (38) reacts with the NH4H2PO4 solution in the second reaction chamber of the first reaction vessel (33) to generate a mixed solution of NH4VO3, NH4H2PO4 and C6H8O7. S5. The quantitative delivery pipe (4) delivers the prepared mixed solution of NH4VO3, NH4H2PO4 and C6H8O7, along with the mixed solution of Ni(CH3COO)2 and NaF, into the main reaction tank (1). The process conditions, such as the concentration of the two mixed solutions, the feed rate, and the reaction temperature of 80 ℃, are controlled to produce Na3V. (2-x) Nix(PO4)3F3.