Grading, lifting and fixing integrated device for precursor synthesis

Abstract

The utility model discloses a grading and solid extraction integrated device for precursor synthesis, and belongs to the technical field of solid extraction of lithium ion battery slurry. The utility model is provided with a grading lifting and fixing device which is provided with a box body; at least two separation membranes are sequentially arranged in the box body and are used for dividing an inner cavity of the box body into a first-stage filtering cavity, a second-stage filtering cavity and a clear liquid cavity, the first-stage filtering cavity is provided with a liquid inlet and a liquid outlet and is used for being communicated with a first reaction kettle so as to convey slurry and collect precursor particles isolated in the first-stage filtering cavity, and the second-stage filtering cavity is communicated with a second reaction kettle; the secondary filter cavity is provided with a reflux inlet so as to be communicated with a second reaction kettle to collect precursor particles isolated in the secondary filter cavity, and the device has the beneficial effects of realizing grading of crystal nucleus granularity while lifting and fixing, and improving the production efficiency.

Description

Technical Field

[0001] This utility model relates to the field of lithium-ion battery slurry consolidation technology, and in particular to an integrated device for grading and consolidation of precursors for synthesis. Background Technology

[0002] Lithium-ion batteries, as a new type of green rechargeable battery, are widely used in mobile electronic devices, power tools, electric vehicles, and other fields. The cathode material of lithium-ion batteries is one of the key factors restricting the development of batteries towards higher energy density. Among them, ternary materials have attracted much attention due to their high energy density, relatively low cost, and excellent cycle performance. However, the structure and performance of these materials depend on the physical properties of the precursors and the preparation technology.

[0003] Currently, co-precipitation is the mainstream method for preparing ternary precursors. By adjusting parameters such as solution concentration, pH value, stirring speed, and reaction time, materials with different particle sizes, morphologies, and densities can be prepared. However, fluctuations in flow rate, temperature, pH, and atmosphere are inevitable during precursor production, leading to the generation of excessively small particles, fine powder, broken spheres, and excessively large particles. These abnormal materials can adversely affect subsequent material sintering and the final battery electrical performance. Therefore, there is an urgent need for a simple and efficient device that can adjust the solid content of the reaction solution in real time during the reaction process, while controlling the particle size distribution of the precursor, avoiding the generation of abnormal particles, improving the stability and consistency of the precursor products, thereby improving the quality of the cathode material precursor and ultimately enhancing the overall performance of lithium-ion batteries.

[0004] Regarding the issue of reducing the particle size distribution range of precursors, existing technologies already exist. For example, Chinese patent CN112191212A discloses a reactor for preparing lithium-ion battery cathode material precursors, including a shell, a stirring device, a first inlet pipe, an outlet pipe, a feed pipe, and a filter plate. The filter plate divides the shell into a reaction zone and a classification zone. During the reaction, precursors of the desired particle size are separated and continue to grow. Filter plates with different pore sizes prepare precursors of different particle sizes, which are then mixed in proportion, making the particle size and particle size distribution of the lithium-ion battery cathode material precursors controllable. However, this patent still requires improvement to the structure of the filter plate to better facilitate the separation and collection of small precursor particles, reducing the loss and waste of small particles.

[0005] Chinese patent CN215232468U discloses a simple device for consolidating ternary precursor slurry, comprising an upper chamber, a lower chamber, and a filter cartridge assembly. The upper chamber includes a consolidation tank, a discharge port, and a pressure balancing port. The filter cartridge assembly is located within the consolidation tank and is inclined. The inclined filter cartridge assembly effectively slows down the rising speed of solid matter and obstructs its movement. When the solid matter's ascent is hindered, it is more likely to settle downwards under its own gravity, significantly reducing the amount of solid matter reaching the discharge port, thereby improving the consolidation effect and efficiency. However, this patent still faces the challenge of optimizing the number and position of the filter cartridges to further improve the consolidation effect.

[0006] To address the aforementioned problems, this invention proposes a simple grain grading and consolidation device that simultaneously consolidates the grains and grades the nucleus size, thereby reducing the particle size distribution range of the precursor and improving production efficiency. Utility Model Content

[0007] The purpose of this invention is to overcome the defects of the existing technology and provide an integrated device for grading and consolidation of precursors for synthesis, which solves the problems of wide particle size distribution, high content of fine and large particles, and low production efficiency in the existing technology.

[0008] To achieve the above objectives, this utility model provides the following technical solution:

[0009] The present invention discloses an integrated grading and consolidation device for precursor synthesis, comprising:

[0010] A graded lifting device, which has a housing;

[0011] At least two separation membranes are sequentially arranged inside the housing to divide the inner cavity of the housing into a primary filtration chamber, a secondary filtration chamber, and a clear liquid chamber.

[0012] The primary filtration chamber has an inlet and an outlet for connecting with the first reactor to transport slurry and collect precursor particles isolated in the primary filtration chamber. The secondary filtration chamber has a reflux port for connecting with the second reactor to collect precursor particles isolated in the secondary filtration chamber.

[0013] Furthermore, at least two of the separation membranes are arranged at an angle from top to bottom.

[0014] Furthermore, the separation membrane includes a first-stage separation membrane and a second-stage separation membrane disposed below the first-stage separation membrane, wherein the pore size of the first-stage separation membrane is larger than the pore size of the second-stage separation membrane.

[0015] Furthermore, the bottom end of the first-stage separation membrane is connected to the side wall of the housing, and the other end extends upward at an angle. Above the first-stage separation membrane is the first-stage filtration chamber, and below it is the second-stage filtration chamber.

[0016] Furthermore, the bottom end of the secondary separation membrane is connected to the bottom wall of the housing, the other end extends upward at an angle, and the top is connected to the side wall adjacent to the bottom wall of the housing. The secondary separation membrane is located above the secondary filtration chamber and below the clear liquid chamber.

[0017] Furthermore, the housing has a discharge port corresponding to the clear liquid chamber, and the discharge port is connected to the supernatant collection tank.

[0018] Furthermore, the side wall of the enclosure is provided with an observation window.

[0019] Furthermore, the graded lifting device also includes a top cover, which is closed on the top of the box body.

[0020] Furthermore, the upper cover is provided with a pressure balancing port, and the pressure balancing port is connected to a pressure balancing device.

[0021] In the above technical solution, the integrated grading and consolidation device for precursor synthesis provided by this utility model has the following advantages compared with the prior art:

[0022] 1. By using two consecutive stages of separation membranes with different pore sizes, the particle size of the crystal nuclei is classified while consolidation is achieved, effectively reducing the particle size distribution range of the precursor and reducing the content of fine and large particles, thereby improving material performance and consistency. In addition, by adjusting the pore size of the separation membrane, the required precursor particle size range can be flexibly controlled to meet the needs of different products.

[0023] 2. The device has a simple structure and is easy to operate, requiring no complex control system, resulting in high production efficiency and low investment cost. Secondly, the device adopts a continuous production process, requiring little floor space and having a simple process, which is conducive to achieving automated production. In addition, the device can effectively reduce the loss and waste of fine particles, improve the utilization rate of raw materials, and reduce production costs. Attached Figure Description

[0024] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in this utility model. For those skilled in the art, other drawings can be obtained based on these drawings.

[0025] Figure 1This is a schematic diagram of the integrated grading and consolidation device for precursor synthesis disclosed in this utility model.

[0026] Explanation of reference numerals in the attached figures:

[0027] 101. Container body; 102. Observation window; 103. Top cover; 104. Pressure balancing device; 110. First reaction vessel; 111. Liquid inlet; 112. First-stage separation membrane; 113. Liquid outlet; 120. Second reaction vessel; 121. Reflux port; 122. Second-stage separation membrane; 130. Supernatant collection tank; 131. Discharge port. Detailed Implementation

[0028] To enable those skilled in the art to better understand the technical solution of this utility model, the present utility model will be further described in detail below with reference to the accompanying drawings.

[0029] See Figure 1 As shown;

[0030] The utility model is an integrated device for grading and consolidation in precursor synthesis, comprising: a first reaction vessel 110, a second reaction vessel 120, and a grading and consolidation device connected to the first reaction vessel 110 and the second reaction vessel 120 respectively.

[0031] The graded consolidation device includes: a housing 101, an inlet 111, an outlet 113, a reflux port 121, a clearing port 131, a top cover 103, an observation window 102, and a pressure balancing device 104.

[0032] The housing 101 includes at least two separation membranes, a first-stage separation membrane 112 and a second-stage separation membrane 122. The number of separation membranes corresponds to the number of reaction vessels. The first-stage separation membrane 112 and the second-stage separation membrane 122 are arranged at an angle and, from top to bottom, divide the inner cavity of the housing 101 into a primary filtration chamber, a secondary filtration chamber and a clear liquid chamber.

[0033] The primary filtration chamber is provided with an inlet 111 and an outlet 113, which are connected to the first reactor 110. The slurry in the first reactor 110 enters the primary filtration chamber through the inlet 111 and can flow back into the first reactor 110 through the outlet 113. The secondary filtration chamber is provided with a return port 121, which is connected to the second reactor 120.

[0034] The pore size of the first-stage separation membrane 112 is larger than that of the second-stage separation membrane 122. The bottom end of the first-stage separation membrane 112 is connected to the side wall of the housing 101, and the other end extends upward at an angle. The upper part of the first-stage separation membrane 112 is the first-stage filtration chamber, and the lower part is the second-stage filtration chamber. The bottom end of the second-stage separation membrane 122 is connected to the bottom wall of the housing 101, and the other end extends upward at an angle. The top end is connected to the side wall adjacent to the bottom wall of the housing 101, so that the upper part of the second-stage separation membrane 122 is the second-stage filtration chamber, and the lower part is the clear liquid chamber. The housing 101 has a clear liquid outlet 131 corresponding to the clear liquid chamber. The clear liquid outlet 131 is connected to the supernatant collection tank 130. The side wall of the housing 101 has an observation window 102. The top of the housing 101 is covered with a top cover 103. The top cover 103 has a pressure balance port. The pressure balance port is connected to a pressure balance device 104. The pressure balance device 104 can be a reaction vessel that can provide gas pressure or other gas pressure regulating device that can adjust the pressure in the prior art.

[0035] In use, the slurry in the first reactor 110 is pumped into the classifier and solidifier. First, it passes through the first-stage separation membrane 112 with a slightly larger pore size. The slurry that does not pass through the first-stage separation membrane 112 enters the first reactor 110 through the outlet 113. The slurry that passes through the first-stage separation membrane 112 then enters the second-stage separation membrane 122. The second-stage separation membrane 122 has a slightly smaller pore size. The slurry that does not pass through the second-stage separation membrane 122 flows back to the second reactor 120 through the return port 121. The clear liquid that passes through the second-stage separation membrane 122 is discharged from the clear liquid outlet 131 into the supernatant collection tank 130.

[0036] In a specific embodiment, Example 1:

[0037] The first-stage separation membrane 112 has a pore size of 3 μm, and the second-stage separation membrane 122 has a pore size of 0.5 μm.

[0038] The upper inlet 111 of the housing 101 is connected to the outlet of the first reactor 110, and the outlet 113 is connected to the inlet of the first reactor 110. A reflux port 121 is provided at the lower part of the housing 101 corresponding to the secondary filtration chamber, and the reflux port 121 is connected to the second reactor 120. A clearing port 131 is provided at the lower part of the housing 101 corresponding to the clearing chamber, and the clearing port 131 is connected to the supernatant collection tank 130.

[0039] During operation, the slurry in the first reaction vessel 110 is pumped into the housing 101 of the classifier through the inlet 111. The slurry first passes through the first-stage separation membrane 112 with a larger pore size. Large particles and some medium-sized particles are blocked in the primary filtration chamber on the first-stage separation membrane 112. The slurry then enters the first reaction vessel 110 through the outlet 113. The slurry containing small particles and some medium-sized particles that has passed through the first-stage separation membrane 112 then enters the secondary filtration chamber formed by the second-stage separation membrane 122 and the first-stage separation membrane 112.

[0040] The second-stage separation membrane 122 has a smaller pore size, which can block small particles. The slurry containing small particles that does not pass through the second-stage separation membrane 122 is returned to the second reaction vessel 120 through the reflux port 121. The clear liquid that passes through the second-stage separation membrane 122 and enters the clear liquid chamber is discharged from the clear liquid outlet 131 to the supernatant collection tank 130.

[0041] In addition, the chamber 101 is equipped with a pressure balancing device 104, which adjusts the pressure inside the chamber 101 to 0.05-0.15MPa so that the slurry can pass smoothly through the separation membrane. An observation window 102 is provided on the side of the chamber 101, through which the condition inside the classifier can be observed in real time, and the pressure of the pressure balancing device 104 can be adjusted as needed.

[0042] Example 2:

[0043] This embodiment is basically the same as the first embodiment above, except that the pore size of the first-stage separation membrane 112 is 4 μm and the pore size of the second-stage separation membrane 122 is 0.8 μm.

[0044] During operation, the slurry in the first reactor 110 is pumped into the housing 101 of the classifier through the inlet 111. The slurry first passes through the first-stage separation membrane 112 with a larger aperture, where large particles are blocked. The slurry that does not pass through the first-stage separation membrane 112 contains large particles and some medium-sized particles, and enters the first reactor 110 through the outlet 113. The slurry that passes through the first-stage separation membrane 112 contains small particles and then enters the second-stage separation membrane 122.

[0045] The second-stage separation membrane 122 has a smaller pore size, which can block small particles from passing through. The slurry containing small particles that does not pass through the second-stage separation membrane 122 is returned to the second reactor 120 through the reflux port 121. The clear liquid that passes through the second-stage separation membrane 122 is discharged from the clear outlet 131.

[0046] The pressure inside the tank 101 is adjusted to 0.08-0.12 MPa by the pressure balancing device 104, allowing the slurry to pass smoothly through the separation membrane. The situation inside the classifier is observed in real time through the observation window 102, and the pressure of the pressure balancing device 104 is adjusted as needed.

[0047] Example 3:

[0048] This embodiment is basically the same as Embodiment 1 above, except that the pore size of the first-stage separation membrane 112 is 2.5 μm and the pore size of the second-stage separation membrane 122 is 0.3 μm.

[0049] During operation, the slurry in the first reactor 110 is pumped into the stager housing 101 through the inlet 111. The slurry first passes through the first-stage separation membrane 112 with a larger aperture, where large particles are blocked. The slurry that does not pass through the first-stage separation membrane 112 contains large particles and enters the first reactor 110 through the outlet 113. The slurry that passes through the first-stage separation membrane 112 contains smaller particles and then enters the second-stage separation membrane 122.

[0050] The second-stage separation membrane 122 has a smaller pore size, which can block small particles from passing through. The slurry containing small particles that does not pass through the second-stage separation membrane 122 is returned to the second reactor 120 through the reflux port 121. The clear liquid that passes through the second-stage separation membrane 122 is discharged from the clear outlet 131.

[0051] The pressure inside the tank 101 is adjusted to 0.1-0.2 MPa by the pressure balancing device 104, allowing the slurry to pass smoothly through the separation membrane. The situation inside the classifier is observed in real time through the observation window 102, and the pressure of the pressure balancing device 104 is adjusted as needed.

[0052] In the above technical solution, the integrated device for grading and consolidation of precursor synthesis provided by this utility model includes the following steps for grading and consolidation of precursor synthesis nuclei:

[0053] Step 1: Pump the slurry in the first reaction vessel 110 into the classifier and solidifier;

[0054] Step 2: The slurry first passes through the first-stage separation membrane 112 with a slightly larger pore size. The slurry that does not pass through the first-stage separation membrane 112 enters the first reaction vessel 110 through the liquid outlet 113. The slurry that passes through the first-stage separation membrane 112 then enters the second-stage separation membrane 122.

[0055] Step 3: Determine if the pore size of the second-stage separation membrane 122 is appropriate. If yes, return to step 1; otherwise, proceed to step 4.

[0056] Step 4: The second-stage separation membrane 122 has a slightly smaller pore size. The slurry that does not pass through the second-stage separation membrane 122 is returned to the second reaction vessel 120 through the reflux port 121, while the clear liquid that passes through the second-stage separation membrane 122 is discharged from the clear outlet 131.

[0057] Step 1 includes:

[0058] Step 1.1: Pump the slurry in the first reaction vessel 110 into the box 101 of the classifier through the inlet 111;

[0059] Step 1.2: A first-stage separation membrane 112 and a second-stage separation membrane 122 are provided inside the housing 101. The pore size of the first-stage separation membrane 112 is larger than that of the second-stage separation membrane 122.

[0060] Step 1.3: Adjust the pressure inside the tank 101 using the pressure balancing device 104 so that the slurry can pass smoothly through the separation membrane.

[0061] Step 2 includes:

[0062] Step 2.1: The slurry first passes through the first-stage separation membrane 112 with a larger pore size. Large particles and some medium-sized particles are blocked on the first-stage separation membrane 112.

[0063] Step 2.2: The slurry that does not pass through the first-stage separation membrane 112 contains large particles and some medium particles, and enters the first reaction vessel 110 through the liquid outlet 113;

[0064] Step 2.3: The slurry containing small particles and some medium particles passes through the first-stage separation membrane 112 and then enters the second-stage separation membrane 122.

[0065] Step 4 includes:

[0066] Step 4.1: The second-stage separation membrane 122 has a smaller pore size, which can block small particles from passing through;

[0067] Step 4.2: The slurry containing small particles that did not pass through the second-stage separation membrane 122 is returned to the second reactor 120 through the reflux port 121;

[0068] Step 4.3: The supernatant that has passed through the second-stage separation membrane 122 is discharged from the outlet 131 into the supernatant collection tank 130.

[0069] Step 4.4: By adjusting the pore size of the first-stage separation membrane 112 and the second-stage separation membrane 122, the particle size range of the precursor crystal nuclei can be controlled and separation can be performed.

[0070] Step 4.5: Observe the situation inside the graded consolidator in real time through the observation window 102, and adjust the pressure of the pressure balancing device 104 as needed.

[0071] This invention provides an integrated grading and consolidation device for precursor synthesis. By using two consecutive stages of separation membranes with different pore sizes, it achieves grading of crystal nuclei size while consolidating the precursors, thereby reducing the particle size distribution range of the precursors and improving production efficiency.

[0072] The foregoing description only illustrates certain exemplary embodiments of the present invention. Undoubtedly, those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the above drawings and descriptions are illustrative in nature and should not be construed as limiting the scope of protection of the claims of the present invention.

Claims

1. An integrated device for graded and consolidated synthesis of precursors, comprising: A graded lifting device having a housing (101); The housing (101) is provided with at least two separation membranes in sequence inside, which are used to divide the inner cavity of the housing (101) into a primary filtration chamber, a secondary filtration chamber and a clear liquid chamber, characterized in that: The primary filtration chamber is provided with an inlet (111) and an outlet (113) for communication with the first reactor (110) to transport slurry and collect precursor particles isolated in the primary filtration chamber. The secondary filtration chamber is provided with a reflux port (121) for communication with the second reactor (120) to collect precursor particles isolated in the secondary filtration chamber.

2. The integrated grading and consolidation device for precursor synthesis according to claim 1, characterized in that: At least two of the separation membranes are arranged at an angle from top to bottom.

3. The integrated grading and consolidation device for precursor synthesis according to claim 2, characterized in that: The separation membrane includes a first-stage separation membrane (112) and a second-stage separation membrane (122) placed below the first-stage separation membrane (112). The pore size of the first-stage separation membrane (112) is larger than that of the second-stage separation membrane (122).

4. The integrated grading and consolidation device for precursor synthesis according to claim 3, characterized in that: The bottom end of the first-stage separation membrane (112) is connected to the side wall of the housing (101), and the other end extends upward at an angle. The first-stage filtration chamber is located above the first-stage separation membrane (112), and the second-stage filtration chamber is located below it.

5. The integrated grading and consolidation device for precursor synthesis according to claim 3, characterized in that: The bottom end of the secondary separation membrane (122) is connected to the bottom wall of the box (101), the other end extends upward at an angle, and the top is connected to the side wall adjacent to the bottom wall of the box (101). The secondary separation membrane (122) is located above the secondary filtration chamber and below the clear liquid chamber.

6. The integrated grading and consolidation device for precursor synthesis according to claim 1, characterized in that: The housing (101) has a discharge port (131) corresponding to the clear liquid chamber, and the discharge port (131) is connected to the supernatant collection tank (130).

7. The integrated grading and consolidation apparatus for precursor synthesis according to any one of claims 1-6, characterized in that: The side wall of the enclosure (101) is provided with an observation window (102).

8. The integrated grading and consolidation apparatus for precursor synthesis according to any one of claims 1-6, characterized in that: The graded lifting device also includes a top cover (103), which is placed on the top of the box (101).

9. The integrated grading and consolidation apparatus for precursor synthesis according to claim 8, characterized in that: The upper cover (103) is provided with a pressure balancing port, and the pressure balancing port is connected to a pressure balancing device (104).

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