Device and method for achieving reaction and filtration concentration
By integrating the reaction and filtration and concentration process in one reactor, complex space and control problems caused by equipment independence in the prior art are solved, reducing the number of equipment and footprint, and improving the efficiency of the process flow.
Patent Information
- Application Number
- CN202010521981.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2020-06-10
- Publication Date
- 2025-04-15
- Estimated Expiration
- 2040-06-10
AI Technical Summary
In the prior art, reaction equipment and filtration and concentration equipment are usually independent, resulting in a large number of equipment, a large area of land, and complex process flow control.
By integrating the reaction and filtration concentration process in one reactor, solid-liquid separation is performed using a reactor containing filter elements, reducing the number of equipment and optimizing space utilization.
It has achieved a reduction in the number of equipment and a reduction in the footprint, and simplified process flow control and improved filtration and concentration efficiency.
Smart Images

Figure CN112535891B_ABST
Abstract
Description
Technical Field
[0001] The relevant part of the specification of the present invention relates to a filter of a system for realizing reaction and filtration and concentration, specifically to a method for causing physical and / or chemical reactions in reaction raw materials and filtering and concentrating the reaction products, especially to a method for causing raw materials for preparing a ternary material precursor to react and filtering and concentrating the ternary material precursor, and to an apparatus and method for realizing reaction and filtration and concentration. Background Art
[0002] In a process that requires the reaction raw materials to react first to obtain a reaction product, and then the reaction product is filtered and concentrated, the reaction equipment used for the reaction and the filtering and concentrating equipment used for filtering and concentrating are usually two independent and different equipment. For example, in a preparation process of a lithium-ion battery ternary material precursor, a reactor and a centrifuge are connected to each other. During operation, a mixed salt solution of a certain concentration composed of nickel salt (such as nickel sulfate), cobalt salt (such as cobalt sulfate), manganese salt (such as manganese sulfate) and water and a sodium hydroxide solution of a certain concentration enter the reactor respectively and a salt-alkali neutralization reaction occurs in the reactor to generate a ternary material precursor crystal nucleus. After the reaction is completed, the slurry in the reactor is then transported to the centrifuge for filtering and concentration. Obviously, since the reactor and the centrifuge are two independent and different equipment, the number of these equipment to be configured is large and the floor space is also large. In addition, it also increases the difficulty of process flow control. Summary of the invention
[0003] The purpose of the present invention is to provide a method for preparing a positive electrode material precursor for realizing reaction and filtration and concentration, so as to solve the technical problems of a large number of equipment and a large equipment footprint caused by the fact that the reaction equipment used for reaction and the filtration and concentration equipment used for filtration and concentration are two independent and different equipment.
[0004] In order to solve the above technical problems, according to one aspect of the present invention, a method for preparing a positive electrode material precursor is provided, comprising:
[0005] Providing a raw material containing a metal salt solution for preparing a positive electrode material precursor to the reactor; promoting the raw material to react to generate the positive electrode material precursor, and continuing to provide the reactor with the metal salt solution to ensure that the positive electrode material precursor grows to a set requirement during the growth of the positive electrode material precursor;
[0006] The solution in the reactor is filtered for solid-liquid separation through a filter element located in the reactor so as to maintain the amount of liquid in the reactor within the range required for the reaction; when the cathode material precursor grows to the set requirement, it is discharged.
[0007] By adopting the method for preparing a positive electrode material precursor, the reaction, filtration and concentration of the raw materials are concentrated in a reactor in a container, so that the number of equipment for preparing the positive electrode material precursor is reduced, the equipment occupies a smaller area, and there is no need to circulate the raw materials in multiple reactors or containers. A certain amount of solution can be directly separated into solid and liquid through a filter.
[0008] Furthermore, the preparation method includes at least one set of process units to prepare the positive electrode material precursor; the set of process units includes:
[0009] Adding raw materials including a metal salt solution for preparing a cathode material precursor into a reactor;
[0010] When the liquid level in the reactor drops to the first position, continue to add the raw material into the reactor;
[0011] When the liquid level in the reactor rises to the second position, the solution in the reactor is subjected to the solid-liquid separation through the filtering element.
[0012] When it is necessary to prepare by multiple groups of the process units, the multiple groups of the process units are carried out continuously or intermittently.
[0013] Furthermore, there may be another operation mode, including the following operations:
[0014] Continuously or intermittently feeding a raw material containing a metal salt solution for preparing a positive electrode material precursor into the reactor;
[0015] At the same time, the solution in the reactor is subjected to the solid-liquid separation through the filtering element, so that the liquid level in the reactor is maintained within a preset range.
[0016] Furthermore, after the extracted solution is output from the clean liquid output port of the filter, gas-liquid separation is performed on it.
[0017] As another aspect of the present invention, the present invention further provides a positive electrode material precursor, wherein the positive electrode material precursor is a concentrated reaction product prepared by the above-mentioned method for preparing the positive electrode material precursor.
[0018] Specifically, the cathode material precursor is a ternary cathode material precursor.
[0019] As another aspect of the present invention, the present invention also provides a system for preparing a positive electrode material precursor, comprising:
[0020] A filtering reaction device, comprising a filter and a housing provided with a reaction raw material input port and a reaction product concentrate output port, wherein the filter is arranged in or partially arranged in the housing through an installation port on the top of the housing;
[0021] The gas-liquid separation device comprises a housing provided with a material input end, a gas material output end and a liquid material output end; the liquid material input end is connected with the clean liquid output end of the filter;
[0022] The power device comprises a pump body connected to the gas-liquid separation device; or the power device comprises a pump body connected to the gas-liquid separation device and a filter.
[0023] Furthermore, the gas-liquid separation device is mainly composed of at least two gas-liquid separators connected in series, and the gas-liquid separator includes a material input port, a liquid output port and a gas output port; the gas output port of the gas-liquid separator located at the front end is connected to the material input port of the gas-liquid separator located at the rear end.
[0024] Furthermore, the gas-liquid separation device is mainly composed of at least two parallel gas-liquid separators, and the gas-liquid separators include a material input port, a liquid output port and a gas output port; the material input ports of at least two of the gas-liquid separators are connected to the clean liquid output port of the filter.
[0025] Furthermore, the power device includes a circulating water tank, which is provided with a gas inlet connected to a gas output port, and the circulating water tank is provided with a condensing device for condensing the input gas; the liquid outlet located at the bottom of the circulating water tank is connected to the liquid inlet located at the upper part of the circulating water tank through a pump body; the pump body is connected to the gas output port of the gas-liquid separation device for extracting gas.
[0026] On another aspect of the present invention, a device for realizing reaction and filtration and concentration is also provided to solve the technical problem of a large number of equipment and a large equipment footprint caused by the fact that the reaction equipment used for reaction and the filtration and concentration equipment used for filtration and concentration are two independent and different equipment.
[0027] The device for realizing reaction and filtration concentration specifically comprises: a reactor, comprising a shell provided with a reaction raw material input port and a reaction product concentrate output port, the shell having a shell top, and a filter mounting port being provided on the shell top; a filter, comprising a clean liquid output channel component installed on the filter mounting port, and a clean liquid delivery channel component and a filter element group loaded downwardly into the reactor from the filter mounting port; wherein the filter element group is suspended at the lower end of the clean liquid delivery channel component and is placed as a whole or in large part below the liquid level of the to-be-filtered material in the reactor after the reactor reaction is completed, and the clean liquid output port of the filter element group at the upper end of the filter element group is connected to the clean liquid output channel component through the clean liquid delivery channel component to form a clean liquid output flow path.
[0028] According to some embodiments of the present invention, the clean liquid delivery channel component is mainly composed of a first cylindrical structure, and the central axis of the first cylindrical structure is arranged roughly along the vertical direction; a first cylindrical structure lower end plate is arranged at the lower port of the first cylindrical structure, the filter element group is installed on the lower end plate of the first cylindrical structure and the clean liquid output port of the filter element group is connected to the internal space of the first cylindrical structure; a first cylindrical structure upper end plate is arranged at the upper port of the first cylindrical structure, and the clean liquid output channel component is installed on the upper end plate of the first cylindrical structure and is connected to the internal space of the first cylindrical structure.
[0029] According to some embodiments of the present invention, the upper port of the first cylindrical structure extends upward to the vicinity of the filter installation port so that the upper end plate of the first cylindrical structure is located above the filter installation port.
[0030] According to some embodiments of the present invention, the upper end plate of the first cylindrical structure serves as a flange and is connected to the flange on the filter mounting port or to the flange on the clean liquid output channel component or to both the flange on the filter mounting port and the flange on the clean liquid output channel component through a bolted connector.
[0031] According to some embodiments of the present invention, the upper end plate of the first cylindrical structure is clamped between the flange on the filter mounting port and the flange on the clean liquid output channel component, and the upper end plate of the first cylindrical structure, the flange on the filter mounting port and the flange on the clean liquid output channel component are connected by the same set of bolt connectors.
[0032] According to some embodiments of the present invention, the upper end plate of the first cylindrical structure is a certain distance lower than the filter installation port; the first cylindrical structure and the filter element group below the first cylindrical structure are hoisted below the clean liquid output channel component through a clean liquid delivery pull tube connected to the upper end plate of the first cylindrical structure, and the clean liquid delivery pull tube connects the clean liquid output channel component and the internal space of the first cylindrical structure.
[0033] According to some embodiments of the present invention, the length of the clean liquid delivery draw tube enables the first cylindrical structure to be placed as a whole below the liquid level of the to-be-filtered material in the reactor when the reaction in the reactor is completed.
[0034] According to some embodiments of the present invention, a cover plate is installed on the filter mounting port, and the upper end of the clean liquid delivery pull tube is installed on the cover plate; the outer edge of the cover plate is clamped between the flange on the filter mounting port and the flange on the clean liquid output channel component connected together by bolt connectors, or the outer edge of the cover plate is directly connected as a flange to the flange on the filter mounting port through bolt connectors.
[0035] According to some embodiments of the present invention, if the outer edge of the cover plate is directly connected to the flange on the filter mounting port via a bolt connector as a flange, the clean liquid output channel component includes a pipe joint arranged at the upper end of the clean liquid delivery pull tube.
[0036] According to some embodiments of the present invention, a second cylindrical structure extending downward is further provided at the lower end of the first cylindrical structure, the filter element group is located in the second cylindrical structure, and the second cylindrical structure is provided with a through hole for the filtered material to enter between the second cylindrical structure and the filter element group.
[0037] According to some embodiments of the present invention, a filter element limiting plate is further provided on the inner side of the second cylindrical structure, and filter element limiting holes are distributed on the filter element limiting plate, and each filter element limiting hole is respectively matched with a corresponding filter element in the filter element group.
[0038] According to some embodiments of the present invention, the clean liquid output channel component includes a head located on the filter installation port and a pipe joint arranged on the head, and the head is installed on the filter installation port through a flange at the lower end of the head.
[0039] According to some embodiments of the present invention, a stirring mechanism is further provided in the reactor, and the filter element group is located above the stirring mechanism.
[0040] According to some embodiments of the present invention, the reactor is a reactor for preparing a ternary material precursor, and the reaction raw material input port is used to input raw materials for preparing the ternary material precursor into the reactor, and the reaction product concentrate output port is used to output the concentrated ternary material precursor from the reactor.
[0041] The device for achieving reaction and filtration concentration can also adopt another structure, wherein the filter comprises a clean liquid output channel component extending from the housing and a filter element group installed downwardly into the reactor from the filter installation port;
[0042] The filter element group is suspended at the lower end of the clean liquid output channel component and is placed in its entirety or in large part below the liquid level of the to-be-filtered substance in the reactor after the reaction in the reactor is completed.
[0043] According to some embodiments of the present invention, a cover body is disposed in the housing, and the clean liquid output channel component is connected to the filter element group through holes distributed on the cover body.
[0044] According to some embodiments of the present invention, a transversely arranged ring plate is provided in the housing, and the outer side of the ring plate is fixedly connected to the middle section of the clean liquid output channel component, forming a structure in which the clean liquid output channel component is annularly distributed outside the ring plate.
[0045] According to some embodiments of the present invention, a fixing plate is provided in the outer shell, and the fixing plate is connected to the lower end of the filter element group; the filter element group is composed of a plurality of circumferentially arranged filter element units, and the fixing plate is provided with holes corresponding to the lower ends of the filter element units and used to limit the filter element units, and the lower ends of the filter element units of the filter element group are fixed by bolts passing through the holes.
[0046] According to some embodiments of the present invention, the reactor is a reactor for preparing a ternary material precursor, and the reaction raw material input port is used to input raw materials for preparing the ternary material precursor into the reactor, and the reaction product concentrate output port is used to output the concentrated ternary material precursor from the reactor.
[0047] The device for realizing reaction and filtration concentration of the present invention integrates the reactor and the filter into the same device. The filter is installed from the filter installation port on the top of the reactor shell, that is, the clean liquid output channel component of the filter is installed on the filter installation port, and the clean liquid delivery channel component (in another structure, only the clean liquid output channel component) and the filter element group below the clean liquid output channel component are installed into the reactor from the filter installation port downward, thereby, the filter can be conveniently installed and removed from the reactor, especially the filter can be installed on the existing reactor in an ideal way to realize the rapid modification of the existing reactor.
[0048] In addition, since the filter element group of the filter is suspended at the lower end of the clean liquid delivery channel component and is placed as a whole or mostly below the liquid level of the filter material in the reactor after the reactor reaction is completed, the filter element group is in contact with more of the upper layer of the filter material with lower solid content in the filter material, which helps to improve the filtration and concentration efficiency.
[0049] The method for realizing reaction and filtration concentration uses the above-mentioned device for realizing reaction and filtration concentration, so as to obtain the concentrated reaction product through the reaction product concentrate output port.
[0050] The present invention also provides a method for modifying a reactor for realizing reaction and filtration and concentration. The method modifies an existing reactor and a reaction kettle to form a reactor for reaction, filtration and concentration. The modification method includes the following operations:
[0051] Prepare the filter to be placed in the reactor;
[0052] Ensure that the reactor for achieving reaction and filtration concentration is provided with an opening leading to the interior of the reactor;
[0053] extending a filter into the reactor through the opening;
[0054] The filter was fixed on the reactor.
[0055] The method can be used to install a filter on an existing reactor in an ideal manner, thereby realizing rapid modification of the existing reactor.
[0056] Furthermore, when the reactor is originally provided with an opening, the filter is inserted into the reactor through the opening; wherein, the opening of the reactor is expanded or shrunk according to the size of the filter.
[0057] Furthermore, when the shrinkage is performed, a mounting component is processed according to the size of the filter, the mounting component is provided with a hole matching the size of the filter, and the mounting component is set on the opening of the reactor by welding, bonding or flange.
[0058] Furthermore, the size of the mounting component is adapted to the opening on the reactor.
[0059] Furthermore, flange holes are arranged in an annular direction around the opening of the reactor, and after the filter is inserted into the reactor, the part of the filter used for fixing on the reactor is installed on the reactor through the flange.
[0060] Furthermore, a corresponding filter mounting seat with a pipeline structure is installed on the opening of the reactor, and the filter is extended into the reactor through the filter mounting seat and fixed on the reactor.
[0061] Furthermore, a flange is arranged on the opening of the filter mounting seat of the reactor, and after the filter is inserted into the reactor, the filter is fixed in the reactor through the flange.
[0062] Furthermore, a connecting piece is arranged on the filter, and the upper channel of the filter passes through the connecting piece and extends out. After the filter is extended into the reactor, the connecting piece blocks the opening.
[0063] Furthermore, the method further comprises the following steps:
[0064] preparing a cover, which is a hollow structure with an open lower end;
[0065] A hole is opened on the cover so that a pipe on the filter can pass through;
[0066] After the filter has been inserted into the reactor, the connector can be clamped between the cover and the shell of the reactor.
[0067] Furthermore, the method specifically includes the step of fixing the cover, the connector and the housing by bolts that pass through the cover and the housing in sequence; or clamping the connector between the cover and the housing by bolts that pass through the cover and the housing in sequence.
[0068] The present invention also provides a filter for a system for realizing reaction and filtration concentration, wherein the filter is used to be arranged in a reactor housing of the system for realizing reaction and filtration concentration, and the reactor housing is provided with a filter mounting port, and the filter is mounted on the reactor housing through the filter mounting port, and the filter comprises:
[0069] A clean liquid output channel component, the upper end of which extends out of the reactor and is used to output the clean liquid;
[0070] A filter element group is used to separate the solid and liquid of the raw materials of the metal salt solution in the reactor;
[0071] The filter element group is suspended and installed at the lower end of the clean liquid conveying channel component and is placed in its entirety or in large part below the liquid level of the to-be-filtered substance in the reactor after the reaction in the reactor is completed.
[0072] Furthermore, the clean liquid output port of the filter element group at the upper end of the filter element group is connected to the clean liquid output channel component by setting a clean liquid delivery channel component to form a clean liquid output flow path;
[0073] The clean liquid delivery channel component is mainly composed of a first cylindrical structure, and the central axis of the first cylindrical structure is substantially arranged along the vertical direction; wherein,
[0074] A first cylindrical structure lower end plate is provided at the lower port of the first cylindrical structure, the filter element group is installed on the first cylindrical structure lower end plate, and the filter element group clean liquid output port is connected to the internal space of the first cylindrical structure;
[0075] An upper end plate of the first cylindrical structure is arranged at the upper port of the first cylindrical structure, and the clean liquid output channel component is mounted on the upper end plate of the first cylindrical structure and communicates with the inner space of the first cylindrical structure.
[0076] Furthermore, the upper end plate of the first cylindrical structure is connected as a flange to the flange on the filter mounting port through a bolt connector; or, the upper end plate of the first cylindrical structure is connected as a flange to the flange on the clean liquid output channel component through a bolt connector; or, the upper end plate of the first cylindrical structure is clamped between the flange on the clean liquid output channel component and the flange on the filter mounting port through a bolt connector and connected through a bolt connector; or, the upper end plate of the first cylindrical structure is arranged between the flange on the clean liquid output channel component and the flange on the filter mounting port, and the flange on the clean liquid output channel component and the flange on the filter mounting port are connected through a bolt connector to clamp the upper end plate of the first cylindrical structure.
[0077] Furthermore, the upper end plate of the first cylindrical structure is a certain distance lower than the filter installation port; then, the first cylindrical structure and the filter element group below the first cylindrical structure are hoisted below the clean liquid output channel component through a clean liquid delivery pull tube connected to the upper end plate of the first cylindrical structure, and the clean liquid delivery pull tube connects the clean liquid output channel component and the internal space of the first cylindrical structure.
[0078] Furthermore, the length of the clean liquid delivery draw tube can enable the first cylindrical structure as a whole to be placed below the liquid level of the to-be-filtered material in the reactor when the reaction in the reactor is completed.
[0079] Furthermore, a cover plate is installed on the filter installation port, and the upper end of the clean liquid delivery pull tube is installed on the cover plate; the outer edge of the cover plate is clamped between the flange on the filter installation port and the flange on the clean liquid output channel component connected together by bolt connectors, or the outer edge of the cover plate is directly used as a flange and connected to the flange on the filter installation port through bolt connectors;
[0080] If the outer edge of the cover plate is directly connected as a flange to the flange on the filter installation port through a bolt connector, the clean liquid output channel component includes a pipe joint arranged at the upper end of the clean liquid delivery pull pipe.
[0081] Furthermore, a second cylindrical structure extending downward is further provided at the lower end of the first cylindrical structure, the filter element group is located in the second cylindrical structure, and the second cylindrical structure is provided with a through hole for the filtered material to enter between the second cylindrical structure and the filter element group;
[0082] A filter element limiting plate is also provided on the inner side of the second cylinder structure, and filter element limiting holes are distributed on the filter element limiting plate, and each filter element limiting hole is matched with a corresponding filter element in the filter element group.
[0083] Furthermore, the filter comprises a clean liquid output channel component extending from the shell and a filter element group installed downward into the reactor from the filter installation port; wherein the filter element group is suspended at the lower end of the clean liquid output channel component and is placed as a whole or in large part below the liquid level of the to-be-filtered substance in the reactor after the reactor reaction is completed.
[0084] Furthermore, the clean liquid output channel component is directly connected to the filter element in the filter element group.
[0085] Furthermore, a filter element connector is provided at the upper end of the filter element in the filter element group, and the filter element connector is threadedly connected to the clean liquid output channel component.
[0086] By adopting the filter of the system for realizing reaction and filtration and concentration, the reaction, filtration and concentration of the raw materials are all concentrated in a reactor in a container, the number of equipment used is less, and the equipment occupies a smaller area. The core group is suspended at the lower end of the clean liquid conveying channel component and is placed in its entirety or in large part below the liquid level of the to-be-filtered material in the reactor after the reactor reaction is completed. The filter core group is in contact with more of the upper layer of the to-be-filtered material with lower solid content in the to-be-filtered material, which helps to improve the filtration and concentration efficiency.
[0087] The present invention also provides a filter that can be preferably arranged in a reactor to realize a reaction and filtration concentration system. The filter is used to be arranged in a reactor with an agitator through a filter installation port on the reactor. The filter includes a filter element assembly arranged in the reactor, and the filter element in the filter element assembly is a filter element of an inorganic porous material with a hollow cylindrical structure. The inorganic porous material here is, for example, SiC, FeAl, TiAl, NiAl, TiSiC, Ti, etc. The porosity of the filter element here is 15-40%.
[0088] Specifically, the radial crushing strength of the filter element is greater than 185 MPa.
[0089] Specifically, the wall thickness of the filter element is 5 to 15 mm.
[0090] Specifically, the force on the filter element is calculated based on the cantilever beam, and the moment that the maximum force-bearing surface of the filter element can withstand is 147.4 to 188.3 Nm.
[0091] Specifically, the outer diameter of the filter element is 45-55 mm.
[0092] Specifically, the distance between the filter element and the stirrer in the reactor is 0.05-1.5 m.
[0093] Specifically, the filter element is a filter element made of sintered inorganic porous material.
[0094] Specifically, the filter element is a metal porous material filter element.
[0095] Specifically, the filter element is a cylindrical filter element formed by folding a porous metal material.
[0096] Specifically, a sealing cover for sealing the opening at the lower end of the filter element is provided at the lower end of the filter element.
[0097] Specifically, the filter further includes a filter element limiting plate for limiting the filter element.
[0098] Specifically, the filtration area of the filter element is 0.03 to 0.25.
[0099] The filter element in the filter of the system for realizing reaction and filtering concentration can be well arranged in the reactor and can operate more reliably and safely in the reactor.
[0100] The present invention is further described below in conjunction with the accompanying drawings and specific embodiments. Additional aspects and advantages of the present invention will be partially given in the following description, partially become apparent from the following description, or be learned through the practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS
[0101] The drawings constituting a part of the present invention are used to assist in understanding the present invention. The contents provided in the drawings and their related descriptions in the present invention can be used to explain the present invention, but do not constitute improper limitations on the present invention. In the drawings:
[0102] Figure 1 It is a schematic structural diagram of an embodiment of a device for realizing reaction and filtration concentration of the present invention;
[0103] Figure 2 It is a schematic structural diagram of an embodiment of a device for realizing reaction and filtration concentration of the present invention;
[0104] Figure 3 It is a schematic structural diagram of an embodiment of a device for realizing reaction and filtration concentration of the present invention;
[0105] Figure 4 It is a schematic diagram of the structure of another filter in the device for realizing reaction and filtration concentration of the present invention;
[0106] Figure 5 for Figure 4 A local enlarged schematic diagram of the middle A;
[0107] Figure 6 It is a top view schematic diagram of a cover body in another filter in the device for realizing reaction and filtration concentration of the present invention;
[0108] Figure 7 It is a bottom view schematic diagram of a fixed plate in another filter in the device for realizing reaction and filtration concentration of the present invention;
[0109] Figure 8 It is a schematic diagram of a ring plate in another filter in the device for realizing reaction and filtration concentration of the present invention;
[0110] Fig. 9 A schematic structural diagram of a system for preparing a cathode material precursor of the present invention;
[0111] Fig.10 is a schematic diagram of the filter element;
[0112] Fig.11 for Fig.10Schematic diagram of filter material cross section and connecting pipe cross section of the middle filter element;
[0113] The figure is marked as follows: filtering reaction device 1, clean liquid output port 11, gas-liquid separation device 2, incoming material input port 2a, liquid output port 2b, gas output port 2c, power device 3, circulating water tank 31, gas material inlet 31a, liquid material outlet 31b, liquid material inlet 31c, condensing device 32, pump body 33, reactor 100, shell 110, shell top 111, filter installation port 112, filter 200, clean liquid output channel component 210, head 211 , pipe joint 212, pipe joint 213, clean liquid delivery channel component 220, first cylinder structure 221, first cylinder structure lower end plate 222, first cylinder structure upper end plate 223, bolt connector 224, clean liquid delivery pull tube 225, cover plate 226, filter element group 230, filter element 231, second cylinder structure 240, filter element limiting plate 241, clean liquid output pipe 300, cover body 310, ring plate 320, fixing plate 330, filter element unit 340. DETAILED DESCRIPTION
[0114] This embodiment adopts a method for preparing a positive electrode material precursor, comprising:
[0115] Providing a raw material containing a metal salt solution for preparing a positive electrode material precursor to the reactor 100; promoting the raw material to react to generate a positive electrode material precursor, and continuing to provide the reactor 100 with the metal salt solution to ensure that the positive electrode material precursor grows to a set requirement during the growth of the positive electrode material precursor;
[0116] The solution in the reactor 100 is filtered for solid-liquid separation by a filter element in the reactor 100 so as to maintain the amount of liquid in the reactor 100 within the range required for the reaction; when the positive electrode material precursor grows to the set requirement, it is discharged. After the extracted solution is output from the clean liquid output port 11 of the filter, it is subjected to gas-liquid separation.
[0117] By adopting the present method for preparing a cathode material precursor, the reaction, filtration and concentration of the raw materials are concentrated in a container reactor 100, so that the number of equipment for preparing the cathode material precursor is reduced, the equipment occupies a smaller area, and there is no need to circulate the raw materials in multiple reactors 100 or containers. A certain amount of solution can be directly separated into solid and liquid through a filter.
[0118] The preparation method includes at least one set of process units to prepare the positive electrode material precursor; the set of process units includes:
[0119] Adding a raw material including a metal salt solution for preparing a positive electrode material precursor into the reactor 100;
[0120] When the liquid level in the reactor 100 drops to the first position, the raw material continues to be added into the reactor 100;
[0121] When the liquid level in the reactor 100 rises to the second position, the solid-liquid separation is performed on the solution in the reactor 100 through the filtering element.
[0122] When it is necessary to prepare by multiple groups of the process units, the multiple groups of the process units are carried out continuously or intermittently.
[0123] In this way, control can be performed according to actual needs, such as the size of the crystals formed in the reactor 100 and the overall amount. That is, an automatic program can be set, a liquid level meter can be set, etc. When the first position or the second position is reached, the suction action (through the filter) and the feeding action are started respectively, so that there is no excess and it is easy to circulate through other pipelines and other containers, thereby reducing the number of equipment used.
[0124] There is also another operation mode, including the following operations:
[0125] The raw material containing the metal salt solution for preparing the positive electrode material precursor is continuously or intermittently added to the reactor 100; at the same time, the solution in the reactor 100 is subjected to the solid-liquid separation by the filtering element, so that the liquid level in the reactor 100 is maintained within a preset range. Such dynamic feeding and filtering actions can keep the reactor 100 in an efficient operating state.
[0126] Here, a positive electrode material precursor is obtained, and the positive electrode material precursor is a concentrated product of a reaction product prepared by the above-mentioned method for preparing a positive electrode material precursor. The positive electrode material precursor is a ternary positive electrode material precursor.
[0127] like Fig. 9 The method for preparing a cathode material precursor adopts a cathode material precursor preparation system, comprising:
[0128] The filtering reaction device 1 comprises a filter 200 and a reactor shell 110 provided with a reaction raw material input port and a reaction product concentrate output port. The filter is arranged in or partially arranged in the shell through a mounting port on the top of the shell. The outer layer of the filtering reaction device 1 may be provided with a jacket layer.
[0129] The gas-liquid separation device 2 comprises a gas-liquid separation housing provided with a material input end, a gas output end and a liquid material output end; the liquid material input end is connected to the clean liquid output port 11 of the filter;
[0130] The power device 3 includes a pump body 33 connected to the gas-liquid separation device 2; or, the power device 3 includes a pump body 33 connected to the gas-liquid separation device 2 and a filter.
[0131] By adopting the positive electrode material precursor preparation system, reaction, filtration and concentration can be completed with only one reactor 100, and the positive electrode material precursor is prepared with fewer devices and less space.
[0132] The gas-liquid separation device 2 here can be arranged in two ways.
[0133] One is: the gas-liquid separation device 2 is mainly composed of at least a series of gas-liquid separators, the gas-liquid separators comprising a material input port 2a, a liquid output port 2b and a gas output port 2c; the gas output port 2c of the gas-liquid separator at the front end is connected to the material input port 2a of the gas-liquid separator at the rear end. By using two gas-liquid separators in series, two-stage gas-liquid separation can be conveniently achieved, making the gas-liquid separation more complete and accurate.
[0134] Another is: the gas-liquid separation device 2 is mainly composed of two parallel gas-liquid separators, the gas-liquid separators include a material input port 2a, a liquid output port 2b and a gas output port 2c; the material input ports 2a of the two gas-liquid separators are both connected to the clean liquid output port 11 of the filter. When using such a parallel connection, one can be set as a backup.
[0135] The power device 3 includes a circulating water tank 31, which is provided with a gas material inlet 31a connected to the gas output port 2c, and a condensing device 32 for condensing the input gas material is provided on the circulating water tank 31; the liquid material outlet 31b at the bottom of the circulating water tank 31 is connected to the liquid material inlet 31c at the upper part of the circulating water tank 31 through a pump body 33; the pump body 33 is connected to the gas output port 2c of the gas-liquid separation device 2 for extracting gas material. The condensing device 32 can be a water-cooled pipe jacket condensation.
[0136] In this embodiment, a device for realizing reaction and filtration and concentration is used as a reactor.
[0137] Figure 1 FIG. 1 is a schematic diagram of a structure of an embodiment of a device for realizing reaction and filtration concentration according to the present invention. Figure 1As shown, the device for realizing reaction and filtration concentration includes a reactor 100 and a filter 200, wherein the reactor 100 includes a reactor shell 110 provided with a reaction raw material input port (not shown in the figure) and a reaction product concentrate output port (not shown in the figure), wherein the reactor shell 110 has a shell top 111, wherein the shell top 111 is provided with a filter mounting port 112, wherein the filter 200 includes a clean liquid output channel component 110 installed on the filter mounting port 112, and a clean liquid delivery channel component 220 and a filter element group 230 loaded downwardly into the reactor 100 from the filter mounting port 112, wherein the filter element group 230 is suspended and installed at the lower end of the clean liquid delivery channel component 220 and is placed as a whole or in large part below the liquid level of the to-be-filtered substance in the reactor 100 after the reaction of the reactor 100 is completed, and wherein the clean liquid output port (not numbered in the figure) of the filter element group at the upper end of the filter element group 230 is connected to the clean liquid output channel component 110 through the clean liquid delivery channel component 220 to form a clean liquid output flow path.
[0138] According to the above-mentioned device for realizing reaction and filtration concentration, the "reaction raw material input port" refers to: the input port on the reactor 100 for receiving the reaction raw material, and the reaction raw material undergoes physical and / or chemical reactions in the reactor 100 to obtain the reaction product. The "reaction product concentrate output port" refers to: the output port on the reactor 100 for discharging the reaction product concentrate, and the reaction product concentrate is the substance after the aforementioned reaction product is concentrated in the reactor 100. The "liquid level to be filtered" refers to: the liquid level position in the reactor 100 before the aforementioned reaction raw material undergoes physical and / or chemical reactions in the reactor 100 to obtain the reaction product before being filtered by the filter element group 230. The "filter element group clean liquid output port" refers to: the output port on the filter element group 230 for outputting the filtered liquid (clean liquid). The "clean liquid delivery channel component" refers to a component or structure for delivering the clean liquid from the aforementioned filter element group clean liquid output port to the clean liquid output channel component. The "clean liquid output channel component" refers to a component or structure for outputting the clean liquid from the filter 200 to the outside.
[0139] According to the above-mentioned device for realizing reaction and filtration concentration, its main feature is that the reactor 100 and the filter 200 are integrated into the same device. Among them, the filter 200 is installed from the filter installation port 112 on the shell top 111 of the reactor shell 110 of the reactor 100, the clean liquid output channel component 110 of the filter 200 is installed on the filter installation port 112, and the clean liquid delivery channel component 220 and the filter element group 230 below the clean liquid output channel component 110 are installed downward into the reactor 100 from the filter installation port 112. Therefore, the filter 200 can be easily installed and removed from the reactor 100, especially the filter 200 can be installed on the existing reactor 100 to realize the rapid modification of the existing reactor 100. In view of the situation that the reaction equipment used for reaction and the filtering and concentrating equipment used for filtering and concentrating are two different independent equipments in the past, as long as the reaction equipment belongs to the above-mentioned reactor 100 (such as a reactor), the above-mentioned filter 200 can usually be installed on the reaction equipment, so as to realize the above-mentioned device for realizing reaction and filtering and concentrating, thereby reducing the number of equipment and the equipment footprint. Since the filter element group 230 of the filter 200 is suspended and installed at the lower end of the clean liquid delivery channel component 220 and is placed in its entirety or in large part below the liquid level of the to-be-filtered material in the reactor 100 after the reaction of the reactor 100 is completed, the filter element group 230 is more in contact with the upper layer of the to-be-filtered material with a lower solid content in the to-be-filtered material, which helps to improve the filtering and concentrating efficiency.
[0140] According to the above-mentioned device for realizing reaction and filtration concentration, its working process is: 1) reaction process: the reaction raw materials enter the reactor 100 from the reaction raw material input port and undergo physical and / or chemical reactions in the reactor 100 to obtain reaction products; 2) filtration concentration process: after the reaction process, by starting the filter 200 (mainly including the operation of forming a filtration pressure difference on both sides of the filtration surface formed by the filter element group 230, this operation is usually achieved by means of a pump connected to the clean liquid output channel component 110), the reaction product is separated into solid and liquid, and the clean liquid separated from the solid and liquid is output through the clean liquid delivery channel component 220 and the clean liquid output channel component 110, thereby leaving the reaction product concentrate in the reactor 100; 3) reaction product concentrate discharge process: the reaction product concentrate is discharged from the reactor 100 through the reaction product concentrate output port.
[0141] The reaction process and the filtration and concentration process here can be carried out alternately or simultaneously and can be adjusted according to actual needs.
[0142] According to the above-mentioned device for realizing reaction and filtration concentration, its clean liquid delivery channel component 220 specifically involves the following structure: the clean liquid delivery channel component 220 is mainly composed of the first cylindrical structure 111, the central axis of the first cylindrical structure 111 is arranged roughly along the vertical direction, and the first cylindrical structure 111 is provided with a first cylindrical structure lower end plate 222 at the lower port, the filter element group 230 is installed on the first cylindrical structure lower end plate 222 and the clean liquid output port of the filter element group is connected to the internal space of the first cylindrical structure 111; the first cylindrical structure 211 is provided with a first cylindrical structure upper end plate 223 at the upper port, and the upper port of the first cylindrical structure 211 extends upward to the vicinity of the filter installation port 112 so that the first cylindrical structure upper end plate 223 is located at the filter installation port. Above the mounting port 112, the upper end plate 223 of the first cylindrical structure also serves as a flange and is connected to the flange 113 on the filter mounting port 112 and the flange 114 on the clean liquid output channel component 110 through bolt connectors 224. Specifically, the upper end plate 223 of the first cylindrical structure is clamped between the flange 113 on the filter mounting port 112 and the flange 114 on the clean liquid output channel component 110, and the upper end plate 223 of the first cylindrical structure, the flange 113 on the filter mounting port 112 and the flange 114 on the clean liquid output channel component 110 are connected through the same set of bolt connectors 224, so that the clean liquid output channel component 110 is installed on the upper end plate 223 of the first cylindrical structure and is connected to the internal space of the first cylindrical structure 211.
[0143] According to the clean liquid delivery channel component 220 of the above-mentioned device for realizing reaction and filtration concentration, since the lower end plate 222 of the first cylindrical structure is provided at the lower port of the first cylindrical structure 211 and the filter element group 230 is installed on the lower end plate 222 of the first cylindrical structure, and the upper end plate 223 of the first cylindrical structure 211 extends upward to the vicinity of the filter installation port 112 so that the upper end plate 223 of the first cylindrical structure is located above the filter installation port 112 and the upper end plate 223 of the first cylindrical structure is used as a flange to be connected to the flange 113 on the filter installation port 112 and the flange 114 on the clean liquid output channel component 110 through the bolt connector 224. In this way, the first cylindrical structure 211 as a whole plays the role of connecting the filter element group 230 and the clean liquid output channel component 110, and through the first cylindrical structure 211, the filtering part of the filter element group 230 is placed more below the liquid level of the to-be-filtered material in the reactor 100 after the reaction of the reactor 100 is completed, thereby ensuring the effective use area of the filter element group 230.
[0144] According to the above-mentioned device for realizing reaction and filtration concentration, the clean liquid output channel component 110 specifically includes a head 111 located on the filter mounting port 112 and a pipe joint 112 arranged on the head 111. The head 111 is installed on the filter mounting port 112 through a flange at the lower end of the head 111 (flange 114 on the clean liquid output channel component 110).
[0145] According to the above-mentioned device for realizing reaction and filtration concentration, the lower end of the first cylinder structure 211 is also provided with a second cylinder structure 240 extending downward, the filter element group 230 is located in the second cylinder structure 240, and the second cylinder structure 240 is provided with a through hole for the filtered material to enter the second cylinder structure and the filter element group; in addition, the inner side of the second cylinder structure 240 is also provided with a filter element limiting plate 241, and the filter element limiting plate 241 is distributed with filter element limiting holes, and each filter element limiting hole is respectively matched with the corresponding filter element 231 in the filter element group 230.
[0146] The second cylindrical structure 240 can accommodate the filter element group 230, so as to protect the filter element group 230; since a filter element limiting plate 241 is also provided on the inner side of the second cylindrical structure 240, filter element limiting holes are distributed on the filter element limiting plate 241, and each filter element limiting hole is respectively matched with the corresponding filter element 231 in the filter element group 230, therefore, the filter element limiting plate 241 can position the corresponding filter element 231 in the filter element group 230 to prevent the filter element 231 from moving.
[0147] Figure 2 FIG. 1 is a schematic diagram of a structure of an embodiment of a device for realizing reaction and filtration concentration according to the present invention. Figure 2 As shown, the device for realizing reaction and filtration concentration includes a reactor 100 and a filter 200, wherein the reactor 100 includes a reactor shell 110 provided with a reaction raw material input port (not shown in the figure) and a reaction product concentrate output port (not shown in the figure), wherein the reactor shell 110 has a shell top 111, wherein the shell top 111 is provided with a filter mounting port 112, wherein the filter 200 includes a clean liquid output channel component 110 installed on the filter mounting port 112, and a clean liquid delivery channel component 220 and a filter element group 230 loaded downwardly into the reactor 100 from the filter mounting port 112, wherein the filter element group 230 is suspended and installed at the lower end of the clean liquid delivery channel component 220 and is placed as a whole or in large part below the liquid level of the to-be-filtered substance in the reactor 100 after the reaction of the reactor 100 is completed, and wherein the clean liquid output port (not numbered in the figure) of the filter element group at the upper end of the filter element group 230 is connected to the clean liquid output channel component 110 through the clean liquid delivery channel component 220 to form a clean liquid output flow path.
[0148] According to the above-mentioned device for realizing reaction and filtration concentration, the clean liquid delivery channel component 220 is mainly composed of a first cylindrical structure 211, the central axis of the first cylindrical structure 211 is arranged roughly in the vertical direction, and a first cylindrical structure lower end plate 222 is arranged at the lower port of the first cylindrical structure 211, and the filter element group 230 is installed on the first cylindrical structure lower end plate 222 and the clean liquid output port of the filter element group is connected to the internal space of the first cylindrical structure 211; a first cylindrical structure upper end plate 223 is arranged at the upper port of the first cylindrical structure 211, and the first cylindrical structure upper end plate 223 is lower than the filter installation port 112 by a certain distance, and the first cylindrical structure 211 and the filter element group 230 below the first cylindrical structure 211 are hoisted below the clean liquid output channel component 110 through a clean liquid delivery pull pipe 225 connected to the first cylindrical structure upper end plate 223. The clean liquid delivery pull pipe 225 can deliver the clean liquid to the filter element group 230. The liquid output channel component 110 is connected to the internal space of the first cylinder structure 211, and the length of the clean liquid delivery pull tube 225 can make the first cylinder structure 211 as a whole be placed below the liquid level of the to-be-filtered material in the reactor 100 when the reaction of the reactor 100 is completed; a cover plate 226 is installed on the filter installation port 112, and the upper end of the clean liquid delivery pull tube 225 is installed on the cover plate 226, and the outer edge of the cover plate 226 is clamped between the flange 113 on the filter installation port 112 and the flange 114 on the clean liquid output channel component 110 connected together by bolt connectors 224; and the clean liquid output channel component 110 includes a head 111 located on the filter installation port 112 and a pipe joint 112 arranged on the head 111, and the head 111 is installed on the filter installation port 112 through the flange at the lower end of the head 111 (the flange 114 on the clean liquid output channel component 110).
[0149] Since the first cylinder structure 211 and the filter element group 230 below the first cylinder structure 211 are hoisted below the clean liquid output channel component 110 through the clean liquid delivery pull tube 225 connected to the upper end plate 223 of the first cylinder structure, the setting of the clean liquid delivery pull tube 225 compresses the internal volume of the first cylinder structure 211, and the diameter of the clean liquid delivery pull tube 225 itself is small. Therefore, the overall capacity of the clean liquid delivery channel component 220 of this structure is small, and more clean liquid can be output.
[0150] According to the above-mentioned device for realizing reaction and filtration concentration, the lower end of the first cylinder structure 211 is also provided with a second cylinder structure 240 extending downward, the filter element group 230 is located in the second cylinder structure 240, and the second cylinder structure 240 is provided with a through hole for the filtered material to enter the second cylinder structure and the filter element group; in addition, the inner side of the second cylinder structure 240 is also provided with a filter element limiting plate 241, and the filter element limiting plate 241 is distributed with filter element limiting holes, and each filter element limiting hole is respectively matched with the corresponding filter element 231 in the filter element group 230.
[0151] Figure 3 FIG. 1 is a schematic diagram of a structure of an embodiment of a device for realizing reaction and filtration concentration according to the present invention. Figure 3 As shown, the clean liquid delivery channel component 220 of the device for realizing reaction and filtration concentration specifically involves the following structure: the clean liquid delivery channel component 220 is mainly composed of a first cylindrical structure 211, the central axis of the first cylindrical structure 211 is arranged roughly along the vertical direction, and a first cylindrical structure lower end plate 222 is arranged at the lower port of the first cylindrical structure 211, and the filter element group 230 is installed on the first cylindrical structure lower end plate 222 and the clean liquid output port of the filter element group is connected to the internal space of the first cylindrical structure 211; a first cylindrical structure upper end plate 223 is arranged at the upper port of the first cylindrical structure 211, and the first cylindrical structure upper end plate 223 is lower than the filter installation port 112 by a certain distance, and the first cylindrical structure 211 and the filter element group 230 below the first cylindrical structure 211 are connected to the filter element group 230 at the lower end plate 222 of the first cylindrical structure. The clean liquid delivery pull tube 225 on the upper end plate 223 of the first cylindrical structure is hoisted below the clean liquid output channel component 110, and the clean liquid delivery pull tube 225 connects the clean liquid output channel component 110 and the internal space of the first cylindrical structure 211. The length of the clean liquid delivery pull tube 225 can place the first cylindrical structure 211 as a whole below the liquid level of the to-be-filtered material in the reactor 100 when the reaction of the reactor 100 is completed; a cover plate 226 is installed on the filter mounting port 112, and the upper end of the clean liquid delivery pull tube 225 is installed on the cover plate 226, and the outer edge of the cover plate 226 is directly connected to the flange 113 on the filter mounting port 112 as a flange through a bolt connector 224; the clean liquid output channel component 110 includes a pipe joint 113 arranged at the upper end of the clean liquid delivery pull tube 225.
[0152] like Figure 4-8In this embodiment, the filter 200 in the reactor 100 can be directly replaced with another filter structure, which omits the first barrel and the second barrel, and the filter element directly passes through the outside of the reactor through a continuous pipeline. The filter includes a clean liquid output channel component extending from the reactor housing 110 and a filter element group installed downwardly into the reactor 100 from the filter installation port 112. The clean liquid output channel component is set as a clean liquid output pipe 300 connecting the filter element and the outside of the reactor 100; wherein the filter element group is suspended at the lower end of the clean liquid output pipe 300 and is placed in its entirety or in large part below the liquid level of the to-be-filtered substance in the reactor 100 after the reaction of the reactor 100 is completed. That is, in this structure, the continuous clean liquid output pipe 300 is directly connected to the filter element group, and the filter element group is directly built into the reactor 100.
[0153] The reactor housing 110 is provided with a cover 310, and the clean liquid output pipe 300 is connected to the filter element group through the holes distributed on the cover 310, and the cover 310 here is a flange. The cover 310 here can be regarded as the same component as the cover plate in the above-mentioned other structure, that is, the function is to enable the filter to be stably installed on the reactor housing 110 of the reactor 100. The fixing method of the cover 310 here can also adopt the fixed connection method of the above-mentioned cover plate, that is, the outer edge of the above-mentioned cover plate can be clamped between the flange on the filter installation port 112 and another flange, or the outer edge of the cover 310 on the filter installation port 112 is directly used as a flange and connected to the flange on the filter installation port 112 through a bolt connector. Here, a transversely arranged ring plate 320 is provided in the reactor housing 110, and the outer side of the ring plate 320 is fixedly connected to the middle section of the clean liquid output pipe 300, forming a structure in which the clean liquid output pipe 300 is annularly distributed on the outer side of the ring plate 320. The ring plate 320 here can be welded so that its outer side is fixed to the clean liquid output pipe 300 here, and the clean liquid output pipe 300 is arranged in a circular direction outside the ring plate 320. After the ring plate 320 is arranged, the clean liquid output pipe 300 is prevented from shaking, which is equivalent to bundling multiple clean liquid output pipes 300 together, so that the clean liquid output pipe 300 can be relatively stable.
[0154] A fixing plate 330 is provided in the reactor housing 110, and the fixing plate 330 is connected to the lower end of the filter element group; the filter element group is composed of a plurality of filter element units 340 arranged in an annular direction, and a hole corresponding to the lower end of the filter element unit 340 is provided on the fixing plate 330 for limiting the filter element unit 340, and the lower end of the filter element unit 340 of the filter element group is fixed by a bolt passing through the hole. A reinforcing rib, such as a cross-shaped bracket, can be provided in the middle of the fixing plate 330. The fixing plate 330 here is set in a disc shape, and the holes here can be long strip holes extending and arranged along the circumference of the fixing plate 330 to improve the flexibility of installation. A joint can be provided at the upper end of the filter element unit 340, and the joint is threadedly connected to the clean liquid output pipe 300.
[0155] According to the above-mentioned device for realizing reaction and filtration concentration, the reactor 100 is a reactor 100 for preparing a ternary material precursor, and the reaction raw material input port is used to input the raw materials for preparing the ternary material precursor into the reactor 100, and the reaction product concentrate output port is used to output the concentrated ternary material precursor from the reactor 100.
[0156] The above-mentioned device for realizing reaction and filtration concentration can adopt a modification method, in which the existing reactor 100 and the reactor are modified to form a reactor 100 for reaction filtration concentration. The modification method includes the following operations: preparing the filter to be placed in the reactor 100; ensuring that the reactor 100 for realizing reaction and filtration concentration is provided with an opening leading to the inside of the reactor 100; extending the filter into the reactor 100 through the opening; and fixing the filter on the reactor 100. Through this method, the filter can be added to the existing reactor 100 in an ideal way, so as to realize the rapid modification of the existing reactor 100. The reactor (reactor) maintains normal pressure or slightly positive pressure, the filter element is connected to the vacuum system through the vacuum tank, and the vacuum pump establishes negative pressure, thereby forming a pressure difference between the outside and inside of the filter element, so that the liquid phase passes through the filter element to form a filtrate, and the solid phase is trapped in the reactor to achieve the purpose of material concentration.
[0157] When the reactor 100 is originally provided with an opening, the filter is inserted into the reactor 100 through the opening; wherein, the opening of the reactor 100 is expanded or shrunk according to the size of the filter. When shrinking the hole, a mounting component is processed according to the size of the filter, the mounting component has a hole matching the size of the filter, and the mounting component is set on the opening of the reactor 100 by welding, bonding or flange. The size of the mounting component is adapted to the opening on the reactor 100.
[0158] In one modification method, flange holes arranged in a ring are opened around the opening of the reactor 100, and after the filter is inserted into the reactor 100, the part of the filter used for fixing on the reactor 100 is installed on the reactor 100 through the flange.
[0159] Another modification method is to install a corresponding filter mounting seat with a pipeline structure on the opening of the reactor 100 , extend the filter into the reactor 100 through the filter mounting seat, and fix the filter on the reactor 100 .
[0160] Another modification method is to set a flange on the opening of the filter mounting seat of the reactor 100, and after the filter is inserted into the reactor 100, the filter is fixed in the reactor 100 through the flange.
[0161] In the above three modification methods, a connector can be set on the filter, and the channel formed by the clean liquid output channel component and the clean liquid delivery channel component (in the structure without the clean liquid delivery channel component, the channel here only refers to the clean liquid output pipe 300) passes through the connector and extends out. After the filter is extended into the reactor 100, the connector is used to block the opening.
[0162] The cover can be added during the modification, which specifically includes the following steps:
[0163] preparing a cover, which is a hollow structure with an open lower end;
[0164] A hole is opened on the cover so that a pipe on the filter can pass through;
[0165] After the filter has been inserted into the reactor 100 , the connector can be clamped between the cover and the reactor housing 110 of the reactor 100 .
[0166] The cover, the connector and the reactor shell 110 are fixed by bolts passing through the cover, the connector and the reactor shell 110 in sequence; or, the connector is clamped between the cover and the reactor shell 110 by bolts passing through the cover and the reactor shell 110 in sequence.
[0167] In this embodiment, a filter is used to realize the system of reaction and filtration concentration, which can be well arranged in the reactor and can operate relatively stably and reliably.
[0168] Reference Figures 1 to 4The present invention also provides a filter that can be preferably arranged in a reactor to realize a reaction and filtration concentration system. The filter is used to be arranged in a reactor with a stirrer through a filter installation port on the reactor. The filter includes a filter element assembly arranged in the reactor. The filter element in the filter element assembly (the filter element is a filter element 231 or a filter element unit 340) is a filter element of an inorganic porous material with a hollow cylindrical structure. The radial crushing strength of the filter element is 185 to 340 Mpa.
[0169] Preferably, the wall thickness of the filter element is 5 to 15 mm. According to the cantilever beam calculation of the filter element force, the moment that the maximum force-bearing surface of the filter element can withstand is 147.4 to 188.3 Nm. Preferably, the outer diameter of the filter element is 45 to 55 mm. The filter element is a metal porous material filter element.
[0170] One arrangement of the filter element here is to use a cylindrical filter element formed by folding a metal porous material. That is, the metal porous material is digitally folded to form pleats and then surrounded by a cylindrical structure. Specifically, a cover is provided at the lower end of the filter element to block the lower end opening of the filter element.
[0171] Another configuration is to directly use a formed, hollow, columnar metal porous material filter element.
[0172] A filter element limiting plate 241 is provided at an appropriate position on the filter to prevent vibration of the filter element group.
[0173] The distance between the filter element and the stirrer in the reactor is 0.05-1.5 m.
[0174] The filtration area of the filter element is 0.03 to 0.25.
[0175] The following is explained using a strength test of the filter elements in the filter element group.
[0176] In the reactor, since this embodiment uses inclined paddles, the paddles are at an angle of 30 degrees to the horizontal plane. During the stirring process, the paddles are acted upon by the fluid to generate lift and drag. The fluid moves due to the reaction force of the lift and drag, flowing in radial, axial and circumferential directions, forming a complex flow pattern.
[0177] The lift component causes the fluid to flow downward along the axis of the impeller, and after moving away from the impeller blades or reaching the bottom of the container, it turns back to form a circular flow component upward along the axis of the impeller.
[0178] The resistance component causes the fluid to generate a velocity component in the tangential direction of the blade movement direction. Under the influence of the cylinder wall, a part of the component rises or falls along the cylinder wall to form a radial flow component, and the other part moves with the paddle blade to form an annular flow component.
[0179] The three directions of fluid motion generated by stirring exert forces on the filter element stationary in the container. This force can also be decomposed into three directions for examination. Among the three directions, the axial flow component is parallel to the filter element. The projected area of the filter element on the section perpendicular to the flow direction is very small. Compared with the other two directions, the axial force can be ignored.
[0180] For the circumferential and radial flow components, their directions are perpendicular to the axis of the filter element. Since the circumferential and radial components are generated by the reaction forces of lift and resistance respectively, and the premise for the fluid to generate lift and resistance on the blade is in the direction of blade movement, the flow velocity of the fluid in the radial and circumferential directions relative to the filter element is less than the linear velocity of the blade edge, and the force on the filter element is less than the fluid resistance generated by the fluid flowing at the linear velocity of the blade edge. According to the torque distribution characteristics of the cantilever structure, the closer the part is to the fixed end, the greater its torque. Combined with the structural characteristics of the filter element, the filter element has two weak parts: one is the part where the filter material is connected to the joint, which is the place where the filter material cross section is subjected to the largest torque, and the material strength is the lowest near the weld; the other is the place where the pipe is connected to the external thread joint. Although the material strength is much higher than that of the filter element, due to the turning of the thread, its cross-sectional area and cross-sectional diameter are very small, which is also a weak part.
[0181] For details on the filter element stress, see Fig.10 In the figure, the length of the force arm is the distance from the geometric center of the filter element to the force-bearing surface. The length of the force arm on the weak surface of the filter element is 248mm, and the length of the force arm on the weak surface of the connecting pipe is 255mm.
[0182] Substitute the fluid resistance value and calculate the maximum moment caused by stirring at each weak point:
[0183] Thick filter element M 厚max =261.1N×0.248m=84.28Nm
[0184] Thin filter element M 薄max =261.1N×0.248m=84.28Nm
[0185] Take over M 接max =261.1N×0.255m=81.97Nm
[0186] For example, the actual outer diameter of the thick filter element is 47mm, and the wall thickness is not less than 5mm; the actual outer diameter of the thin filter element is 50mm, and the wall thickness is not less than 3mm; the theoretical size of the connecting pipe section is as follows Fig.10 , taking into account the dimensional tolerance, the actual outer diameter is calculated as 90% of the theoretical outer diameter.
[0187] The tubular filter element can be regarded as a hollow cylinder, and its cross-sectional coefficient is calculated as follows:
[0188]
[0189] in:
[0190] Wz Section modulus
[0191] D is the outer diameter of the cylinder;
[0192] α is the ratio of the inner diameter to the outer diameter of a hollow cylinder.
[0193] Calculate the weak point from this: W 厚 =6.28×10 -6 , W 薄 =4.91×10 -6 , W 接 =6.61×10 -7 .
[0194] According to the filter element crush test data, the minimum compressive strength of the filter element is 185Mpa. The test data are as follows:
[0195] Table 1 Filter element crush test data
[0196]
[0197] According to relevant literature on the strength of sintered titanium aluminum filter elements, the tensile strength of titanium aluminum filter elements is related to the material particle size and pressing pressure. The smaller the particle size, the greater the pressing pressure and the higher the filter element strength.
[0198] The tensile strength of the filter element is much smaller than the crushing strength of the filter element, so the filter element will first break from the tensile side when subjected to bending moment. The tensile strength of the filter element of this embodiment is greater than 30Mpa, and 30Mpa is conservatively calculated as the maximum stress that the filter element material of this embodiment can withstand.
[0199] The relationship between the filter element cross-sectional stress and moment:
[0200] σ max =M max / W z
[0201] in:
[0202] σmax is the maximum stress that the filter element can withstand;
[0203] M max is the maximum moment that the filter element cross section can withstand;
[0204] Wz filter element cross-sectional coefficient.
[0205] Calculate the force of the filter element according to the cantilever beam. The moment that the thick filter element filter material can withstand on the maximum force surface is:
[0206] M 厚 =W 厚 ×σ 厚
[0207] =6.28×10 -6 ×30Mpa
[0208] =188.3Nm
[0209] The torque that the maximum force-bearing surface of the thin filter element can withstand is:
[0210] M 薄 =W 薄 ×σ 薄
[0211] =4.91×10 -6 ×30Mpa
[0212] =147.4Nm
[0213] The torque that the maximum force-bearing surface of the filter element can withstand is (316L tensile strength 500Mpa):
[0214] M 接 =W 接 ×σ 接
[0215] =6.61×10 -7 ×500Mpa
[0216] =330.7Nm
[0217] Compare the maximum torque that the weak part of the filter element can withstand and the maximum torque that can be generated by stirring:
[0218] Thick filter element: M 厚 =188.3Nm>M 厚max =81.97Nm
[0219] Thin filter element: M 薄 =147.4Nm>M 薄max =81.97Nm
[0220] Take over: M 接 =330.7Nm>M 接max =84.28Nm
[0221] It can be seen that the maximum torque that the thick filter element and the thin filter element can withstand at the weak point of the filter element is much greater than the maximum torque that can be generated by stirring. The filter element can be reliably arranged in the reactor.
[0222] The above is a description of the relevant contents of the present invention. A person skilled in the art will be able to implement the present invention based on these descriptions. Based on the above contents of the present invention, all other preferred implementations and embodiments obtained by a person skilled in the art without making creative work shall fall within the scope of protection of the present invention.
Claims
1. A device for achieving reaction and filtration concentration, characterized in that: The reactor comprises a shell provided with a reaction raw material input port and a reaction product concentrate output port, and the shell is provided with a jacket layer; The reactor is a reactor for preparing a ternary material precursor, the reaction raw material input port is used to input raw materials for preparing the ternary material precursor into the reactor, and the reaction product concentrate output port is used to output the concentrated ternary material precursor from the reactor; Wherein, the housing is provided with a filter installation opening, and the reactor is provided with a filter through the filter installation opening so that the filter is arranged in the reactor; The filter comprises a clean liquid output channel component mounted on the filter installation port, and a clean liquid delivery channel component and a filter element group installed downwardly into the reactor from the filter installation port; The filter element group is suspended and installed at the lower end of the clean liquid delivery channel component and is placed as a whole below the liquid level of the to-be-filtered substance in the reactor after the reactor reaction is completed, and The clean liquid output port of the filter element group at the upper end of the filter element group is connected to the clean liquid output channel component through the clean liquid delivery channel component to form a clean liquid output flow path; The clean liquid delivery channel component is mainly composed of a first cylindrical structure, the central axis of the first cylindrical structure is substantially arranged along the vertical direction, the first cylindrical structure includes a first cylindrical structure upper end plate and a first cylindrical structure lower end plate, and a first cylindrical structure inner cavity is formed between the first cylindrical structure upper end plate and the first cylindrical structure lower end plate; A second cylindrical structure extending downward is provided at the lower end of the first cylindrical structure, the filter element group is located in the second cylindrical structure, and the second cylindrical structure is provided with a through hole for the filtered material to enter between the second cylindrical structure and the filter element group, and a filter element limiting plate is also provided on the inner side of the second cylindrical structure, and filter element limiting holes are distributed on the filter element limiting plate, and each filter element limiting hole is respectively matched with a corresponding filter element in the filter element group; The upper end plate of the first cylindrical structure is lower than the filter installation port by a certain distance, and the first cylindrical structure and the filter element group below the first cylindrical structure are hoisted below the clean liquid output channel component through a clean liquid delivery pull tube connected to the upper end plate of the first cylindrical structure, and the clean liquid delivery pull tube conducts the clean liquid output channel component and the internal space of the first cylindrical structure; In addition, the clean liquid output channel component includes pipeline joints respectively arranged on the upper ends of each clean liquid delivery pull tube.
2. The device for achieving reaction and filtration concentration according to claim 1, characterized in that: A cover plate is installed on the filter mounting port, and the upper end of the clean liquid delivery pull tube is installed on the cover plate; the outer edge of the cover plate is clamped between the flange on the filter mounting port and the flange on the clean liquid output channel component connected together by bolt connectors, or the outer edge of the cover plate is directly used as a flange and connected to the flange on the filter mounting port through bolt connectors.
3. The device for achieving reaction and filtration concentration as claimed in claim 2, characterized in that: If the outer edge of the cover plate is directly connected as a flange to the flange on the filter installation port through a bolt connector, the clean liquid output channel component includes a pipe joint arranged at the upper end of the clean liquid delivery pull pipe.
4. A method for achieving reaction and filtration concentration, characterized in that: The device for realizing reaction and filtration concentration as described in any one of claims 1 to 3 is used to obtain the concentrated ternary material precursor through the reaction product concentrate output port.
Citation Information
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