CN112535892A - Filter of system for realizing reaction and filtration concentration - Google Patents

Filter of system for realizing reaction and filtration concentration Download PDF

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Publication number
CN112535892A
CN112535892A CN202010522361.8A CN202010522361A CN112535892A CN 112535892 A CN112535892 A CN 112535892A CN 202010522361 A CN202010522361 A CN 202010522361A CN 112535892 A CN112535892 A CN 112535892A
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China
Prior art keywords
filter
filter element
reactor
cylinder structure
reaction
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CN202010522361.8A
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Chinese (zh)
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CN112535892B (en
Inventor
何志
李仲恺
何珂桥
刘超
何劲松
杨光耀
赵聪
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Sichuan Scsdn Technology Co ltd
Chengdu Stareng Environmental Protection Equipment Co ltd
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Sichuan Scsdn Technology Co ltd
Chengdu Stareng Environmental Protection Equipment Co ltd
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Priority to CN202010522361.8A priority Critical patent/CN112535892B/en
Publication of CN112535892A publication Critical patent/CN112535892A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/50—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition
    • B01D29/52—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition in parallel connection
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/88—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor having feed or discharge devices
    • B01D29/92—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor having feed or discharge devices for discharging filtrate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/96—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor in which the filtering elements are moved between filtering operations; Particular measures for removing or replacing the filtering elements; Transport systems for filters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention discloses a filter of a system for realizing reaction and filtration concentration, which is arranged in a reactor shell of the system for realizing reaction and filtration concentration, wherein the reactor shell is provided with a filter mounting port, the filter is mounted with the reactor shell through the filter mounting port, and the filter comprises: the upper end of the purified liquid output channel part extends out of the reactor and is used for outputting purified liquid; the filter element group is used for carrying out solid-liquid separation on the raw material of the metal salt solution in the reactor; the filter element group is suspended at the lower end of the purified liquid conveying channel part and is wholly or mostly arranged below the liquid level of the substance to be filtered in the reactor after the reaction of the reactor is finished. Through adopting this system's that realizes the reaction and filter concentration filter, help improving and filter concentration efficiency.

Description

Filter of system for realizing reaction and filtration concentration
Technical Field
The invention relates to a filter of a system for realizing reaction and filtration concentration, in particular to a method for carrying out physical and/or chemical reaction on reaction raw materials and carrying out filtration concentration on reaction products, in particular to a method for carrying out reaction on raw materials for preparing a ternary material precursor and carrying out filtration concentration on the ternary material precursor, and relates to a filter of a system for realizing reaction and filtration concentration.
Background
In a process flow in which a reaction raw material is reacted to obtain a reaction product and then the reaction product is filtered and concentrated, two different apparatuses independent of each other are generally used between a reaction apparatus for reaction and a filtering and concentrating apparatus for filtering and concentrating. For example, in a preparation process of a ternary material precursor of a lithium ion battery, a reaction kettle and a centrifuge are connected with each other, when the preparation process is in operation, a mixed salt solution with a certain concentration and a sodium hydroxide solution with a certain concentration, which are prepared from nickel salt (such as nickel sulfate), cobalt salt (such as cobalt sulfate), manganese salt (such as manganese sulfate) and water, respectively enter the reaction kettle, and undergo a saline-alkali neutralization reaction in the reaction kettle to generate a ternary material precursor crystal nucleus, and after the reaction is completed, slurry in the reaction kettle is conveyed to the centrifuge for filtration and concentration. Obviously, because the reaction kettle and the centrifuge belong to two different devices independent of each other, the devices need to be configured in a large number and occupy a large area, and in addition, the difficulty of process flow control is increased.
Disclosure of Invention
The invention provides a preparation method of a precursor of a cathode material for realizing reaction and filtration concentration, which aims to solve the technical problems of more equipment and larger equipment floor area caused by two different pieces of equipment which are independent from each other between reaction equipment for reaction and filtration concentration equipment for filtration concentration.
In order to solve the above technical problems, according to an aspect of the present invention, there is provided a method for preparing a precursor of a positive electrode material, including:
supplying a raw material containing a metal salt solution for preparing a precursor of a positive electrode material to a reactor; promoting the raw materials to react to generate a precursor of the anode material, and continuously providing the metal salt solution for ensuring that the precursor of the anode material grows to the set requirement for the reactor in the growth process of the precursor of the anode material;
carrying out solid-liquid separation and filtration on the solution in the reactor through a filter element positioned in the reactor so as to maintain the amount of liquid in the reactor in a range required by the reaction; and discharging the precursor of the cathode material after the precursor grows to the set requirement.
By adopting the preparation method of the precursor of the cathode material, the reaction, the filtration and the concentration of the raw materials are concentrated in the reactor in one container, so that the quantity of equipment for preparing the precursor of the cathode material is less, the occupied area of the equipment is smaller, the raw materials do not need to circularly flow in a plurality of reactors or containers, and a certain amount of solution can be directly subjected to solid-liquid separation through the filter.
Further, the preparation method comprises the steps that at least one group of process units are used for preparing the positive electrode material precursor; the group of process units comprises:
charging a raw material containing a metal salt solution for preparing a precursor of a positive electrode material into a reactor;
when the liquid level in the reactor is lowered to a first position, continuously feeding the raw materials into the reactor;
when the liquid level in the reactor rises to the second position, the above-mentioned solid-liquid separation of the solution in the reactor is carried out by means of the filter element.
When the preparation is required to be carried out through a plurality of groups of the process units, the plurality of groups of the process units are carried out continuously or at intervals.
Further, there may be another mode of operation, including the following operations:
continuously or intermittently feeding a raw material containing a metal salt solution for preparing a precursor of the positive electrode material into the reactor;
meanwhile, the solution in the reactor is subjected to solid-liquid separation through the filter element, so that the height of the liquid level in the reactor is kept within a preset range value.
Further, the extracted solution is outputted from a clean liquid output port of the filter, and then subjected to gas-liquid separation.
As another aspect of the present invention, the present invention also provides a precursor of a positive electrode material, wherein the precursor of the positive electrode material is a reaction product concentrate prepared by the preparation method of the precursor of the positive electrode material.
Specifically, the precursor of the cathode material is a ternary precursor of the cathode material.
As another aspect of the present invention, the present invention also provides a system for preparing a precursor of a positive electrode material, including:
the filtering reaction device comprises a filter and a shell provided with a reaction raw material input port and a reaction product concentrate output port, wherein the filter is arranged in the shell or partially arranged in the shell through a mounting port on the top of the shell;
the gas-liquid separation device comprises a shell provided with an incoming material input end, a gas material output end and a liquid material output end; the liquid material input end is communicated with a purified liquid output port of the filter;
the power device comprises a pump body communicated with the gas-liquid separation device; alternatively, the power plant includes a pump body in communication with the gas-liquid separation device and the filter.
Further, the gas-liquid separation device mainly comprises at least two gas-liquid separators connected in series, and each gas-liquid separator comprises a material inlet, a liquid outlet and a gas outlet; and a gas output port of the gas-liquid separator positioned at the front end is communicated with an incoming material input port of the gas-liquid separator positioned at the rear end.
Further, the gas-liquid separation device mainly comprises at least two gas-liquid separators connected in parallel, and each gas-liquid separator comprises a material inlet, a liquid outlet and a gas outlet; and the incoming material input ports of at least two gas-liquid separators are communicated with the clean liquid output port of the filter.
Furthermore, the power device comprises a circulating water tank, a gas material inlet communicated with a gas material outlet is arranged on the circulating water tank, and a condensing device used for condensing input gas materials is arranged on the circulating water tank; the liquid material outlet positioned at the bottom of the circulating water tank is communicated with the liquid material inlet positioned at the upper part of the circulating water tank through the pump body; the pump body is connected with a gas material output port of the gas-liquid separation device and used for extracting gas materials.
In another aspect of the invention, a device for realizing reaction and filtration concentration is further provided, so as to solve the technical problems of a large number of devices and a large occupied area of the devices due to the fact that the reaction device for reaction and the filtration concentration device for filtration concentration belong to two different devices which are independent of each other.
This a device for realizing reaction and concentrated with filtering specifically includes: a reactor comprising a housing having a reactant feedstock input port and a reaction product concentrate output port, said housing having a housing top with a filter mounting port disposed thereon; a filter comprising a net liquid output passage member installed on the filter installation port, and a net liquid delivery passage member and a filter element group which are installed into the reactor from the filter installation port downward; the filter element group is arranged at the lower end of the purified liquid conveying channel part in a suspending mode and is wholly or mostly arranged below the liquid level of a substance to be filtered in the reactor after the reaction of the reactor is completed, and the purified liquid outlet of the filter element group at the upper end of the filter element group is connected with the purified liquid outlet channel part through the purified liquid conveying channel part to form a purified liquid outlet flow path.
According to some embodiments of the present invention, the net liquid conveying passage member is mainly composed of a first cylinder structure, and a central axis of the first cylinder structure is substantially arranged along a vertical direction; a first cylinder structure lower end plate is arranged at the lower port of the first cylinder structure, the filter element group is arranged on the first cylinder structure lower end plate, and a filter element group clean liquid output port is communicated with the inner space of the first cylinder structure; the upper port of the first cylinder structure is provided with a first cylinder structure upper end plate, and the purified liquid output channel component is installed on the first cylinder structure upper end plate and is communicated with the inner space of the first cylinder structure.
According to some embodiments of the invention, the upper port of the first tubular structure extends upwardly to a position proximate the filter mounting opening such that the first tubular structure upper end plate is positioned above the filter mounting opening.
According to some embodiments of the present invention, the first tubular structure upper end plate is connected as a flange to a flange on the filter mounting port or to a flange on the clean liquid outlet passage member or to both a flange on the filter mounting port and a flange on the clean liquid outlet passage member by means of a bolt connection.
According to some embodiments of the present invention, the first tubular structure upper end plate is clamped between the flange on the filter mounting opening and the flange on the purified liquid outlet channel member, and the first tubular structure upper end plate, the flange on the filter mounting opening and the flange on the purified liquid outlet channel member are connected by a same set of bolt connectors.
According to some embodiments of the invention, the first cylinder structure upper end plate is lower than the filter mounting opening by a certain distance; the filter element group below the first cylinder structure and the first cylinder structure is hoisted below the clean liquid output passage component through a clean liquid conveying pull pipe connected to the upper end plate of the first cylinder structure, and the clean liquid conveying pull pipe conducts the clean liquid output passage component and the inner space of the first cylinder structure.
According to some embodiments of the present invention, the length of the net liquid conveying pull pipe is such that the first cylinder structure is integrally disposed below the liquid level of the substance to be filtered in the reactor when the reaction in the reactor is completed.
According to some embodiments of the present invention, a cover plate is installed on the filter installation opening, and the upper end of the clean liquid conveying pull pipe is installed on the cover plate; the outer edge of the cover plate is clamped between a flange plate on the filter mounting port and a flange plate on the purified liquid output channel part which are connected together through a bolt connecting piece, or the outer edge of the cover plate is directly used as a flange plate and is connected with the flange plate on the filter mounting port through the bolt connecting piece.
According to some embodiments of the present invention, if the outer edge of the cover plate is directly connected as a flange to a flange on the filter mounting opening by a bolt connection, the clean liquid discharge passage member includes a pipe joint provided at an upper end of the clean liquid feed stay pipe.
According to some embodiments of the present invention, the lower end of the first cylinder structure is further provided with a second cylinder structure extending downward, the filter element group is located in the second cylinder structure, and the second cylinder structure is provided with a through hole for allowing the substance to be filtered to enter between the second cylinder structure and the filter element group.
According to some embodiments of the present invention, the inner side of the second cylinder structure is further provided with a filter element limiting plate, 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.
According to some embodiments of the present invention, the purified liquid output channel member includes a sealing head located on the filter mounting opening and a pipe joint disposed on the sealing head, and the sealing head is mounted on the filter mounting opening through a flange at a lower end of the sealing head.
According to some embodiments of the present invention, a stirring mechanism is further disposed in the reactor, and the filter element group is located above the stirring mechanism.
According to some embodiments of the present invention, the reactor is a reactor for preparing a ternary material precursor, the reaction raw material input port is used for inputting a raw material for preparing the ternary material precursor into the reactor, and the reaction product concentrate output port is used for outputting the concentrated ternary material precursor from the reactor.
The device for realizing the reaction, the filtration and the concentration can also adopt another structure, and the filter comprises a purified liquid output channel part extending out of the shell and a filter element group which is downwards arranged into the reactor from a filter mounting port;
the filter element group is suspended at the lower end of the purified liquid output channel part and is wholly or mostly arranged below the liquid level of a substance to be filtered in the reactor after the reaction of the reactor is finished.
According to some embodiments of the present invention, a cover is disposed in the housing, and the clean liquid outlet channel is connected to the filter element assembly through holes distributed on the cover.
According to some embodiments of the present invention, a transversely disposed ring plate is disposed in the housing, and an outer side of the ring plate is fixedly connected to a middle section of the purified liquid output passage member, so as to form a structure in which the purified liquid output passage member is annularly distributed on an outer side of the ring plate.
According to some embodiments of the present invention, a fixing plate is disposed in the housing, and the fixing plate is connected to the lower end of the filter element assembly; the filter element group is composed of a plurality of filter element units which are arranged in the circumferential direction, the fixing plate is provided with holes which correspond to the lower ends of the filter element units and are used for limiting the filter element units, and the lower ends of the filter element units of the filter element group are fixed through bolts penetrating through the holes.
According to some embodiments of the present invention, the reactor is a reactor for preparing a ternary material precursor, the reaction raw material input port is used for inputting a raw material for preparing the ternary material precursor into the reactor, and the reaction product concentrate output port is used for outputting the concentrated ternary material precursor from the reactor.
The device for realizing the reaction and the filtration concentration integrates the reactor and the filter into the same equipment. Wherein the filter is installed from a filter installation opening on the top of the reactor shell, namely, a net liquid output channel part of the filter is installed on the filter installation opening, and a net liquid conveying channel part (only the net liquid output channel part in another structure) and a filter element group below the net liquid output channel part are downwards installed into the reactor from the filter installation opening, so that the filter can be conveniently installed and disassembled on the reactor, and particularly, the filter can be additionally installed on the existing reactor in an ideal mode, thereby realizing the quick modification of the existing reactor.
In addition, because the filter element group of the filter is arranged at the lower end of the clean liquid conveying channel part in a suspending way and is wholly or mostly arranged below the liquid level of the object to be filtered in the reactor after the reaction of the reactor is finished, the filter element group is more contacted with the object to be filtered at the upper layer with lower solid content in the object to be filtered, and the efficiency of filtering and concentrating is favorably improved.
The method for realizing the reaction and the filtration concentration uses the device for realizing the reaction and the filtration concentration, so that the concentrated reaction product is obtained through the reaction product concentrate output port.
The invention also provides a reactor refitting method for realizing reaction and filtration concentration, which is used for refitting the existing reactor and reaction kettle to form the reactor for reaction, filtration and concentration, and comprises the following operations:
preparing a filter to be placed in a reactor;
the reactor ensuring the reaction and the filtration concentration is provided with an opening leading to the inside of the reactor;
extending a filter into said reactor through said opening;
the filter was fixed to the reactor.
The method can be used for adding a filter on the existing reactor in an ideal mode, and realizes the quick modification of the existing reactor.
Further, 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 reamed or shrunk depending on the size of the filter.
Further, when the hole is reduced, a mounting member is processed according to the size of the filter, the mounting member is provided with a hole corresponding to the size of the filter, and the mounting member is arranged on the opening of the reactor by welding, bonding or flange according to the size of the mounting member.
Further, the size of the mounting member is adapted to the opening in the reactor.
Further, a flange hole arranged in an annular direction is formed in the periphery of the opening of the reactor, and after the filter is inserted into the reactor, a portion of the filter to be fixed to the reactor is mounted on the reactor through the flange.
Furthermore, a corresponding filter mounting seat with a pipeline structure is mounted on the opening of the reactor, and the filter is inserted into the reactor through the filter mounting seat and is fixed on the reactor.
Furthermore, a flange is arranged on an opening of the filter mounting seat of the reactor, and the filter is fixed in the reactor through the flange after extending into the reactor.
Furthermore, a connecting piece is arranged on the filter, an upper channel of the filter penetrates through the connecting piece and extends out, and after the filter is extended into the reactor, the connecting piece is used for plugging the opening.
Further, the method specifically comprises the following steps:
preparing a sealing cover which is a hollow structure with an opening at the lower end;
the sealing cover is provided with an opening for the pipeline on the filter to pass through;
after the filter has been inserted into the reactor, the above-mentioned connecting piece can be clamped between the cover and the outer shell of the reactor.
Further, the method specifically comprises the step of fixing the three by bolts which sequentially penetrate through the sealing cover, the connecting piece and the shell; alternatively, the connecting member is held between the cover and the housing by bolts which pass through the cover and the housing in this order.
The present invention also provides a filter for a system for performing a reaction and a filtration concentration, the filter being configured to be installed in a reactor housing of the system for performing a reaction and a filtration concentration, the reactor housing being provided with a filter installation opening, the filter being installed in the reactor housing through the filter installation opening, the filter comprising:
the upper end of the purified liquid output channel part extends out of the reactor and is used for outputting purified liquid;
the filter element group is used for carrying out solid-liquid separation on the raw material of the metal salt solution in the reactor;
the filter element group is suspended at the lower end of the purified liquid conveying channel part and is wholly or mostly arranged below the liquid level of the substance to be filtered in the reactor after the reaction of the reactor is finished.
Furthermore, a purified liquid outlet of the filter element group at the upper end of the filter element group is connected with the purified liquid output channel part through a purified liquid conveying channel part to form a purified liquid output flow path;
the clean liquid conveying channel component mainly comprises a first cylinder structure, and the central axis of the first cylinder structure is arranged along the vertical direction approximately; wherein,
a first cylinder structure lower end plate is arranged at the lower port of the first cylinder structure, the filter element group is arranged on the first cylinder structure lower end plate, and a filter element group clean liquid output port is communicated with the inner space of the first cylinder structure;
the upper port of the first cylinder structure is provided with a first cylinder structure upper end plate, and the purified liquid output channel component is installed on the first cylinder structure upper end plate and is communicated with the inner space of the first cylinder structure.
Furthermore, the upper end plate of the first cylinder structure is used as a flange plate and is connected with the flange plate on the filter mounting opening through a bolt connecting piece; or the upper end plate of the first cylinder structure is used as a flange plate and is connected with the flange plate on the purified liquid output channel part through a bolt connecting piece; or the upper end plate of the first cylinder structure is used as a flange plate and is clamped between the flange plate on the purified liquid output channel part and the flange plate on the filter mounting opening through a bolt connecting piece and is connected through the bolt connecting piece; or the upper end plate of the first cylinder structure is arranged between the flange on the purified liquid output channel part and the flange on the filter mounting opening, and the flange on the purified liquid output channel part and the flange on the filter mounting opening are connected through a bolt connecting piece and then clamp the upper end plate of the first cylinder structure.
Further, the upper end plate of the first cylinder structure is lower than the filter mounting opening by a certain distance; then, the filter element group below the first cylinder structure and the first cylinder structure is hoisted below the purified liquid output channel part through a purified liquid conveying pull pipe connected to an upper end plate of the first cylinder structure, and the purified liquid conveying pull pipe conducts the purified liquid output channel part and the inner space of the first cylinder structure.
Furthermore, the length of the clean liquid conveying pull pipe can enable the first cylinder structure to be integrally placed below the liquid level of the substance to be filtered in the reactor when the reaction of the reactor is finished.
Further, a cover plate is arranged on the filter mounting opening, and the upper end of the clean liquid conveying pull pipe is arranged on the cover plate; the outer edge of the cover plate is clamped between a flange on the filter mounting port and a flange on the purified liquid output channel part which are connected together through a bolt connecting piece, or the outer edge of the cover plate is directly used as a flange to be connected with the flange on the filter mounting port through the bolt connecting piece;
if the outer edge of the cover plate is directly used as a flange plate and is connected with the flange plate on the filter mounting opening through a bolt connecting piece, the purified liquid output channel part comprises a pipeline joint arranged at the upper end of the purified liquid conveying pull pipe.
Furthermore, the lower end of the first cylinder structure is also provided with a second cylinder structure extending downwards, the filter element group is positioned in the second cylinder structure, and the second cylinder structure is provided with a through hole for the substance to be filtered to enter between the second cylinder structure and the filter element group;
the inner side of the second cylinder structure is also provided with a filter element limiting plate, filter element limiting holes are distributed on the filter element limiting plate, and the filter element limiting holes are respectively matched with corresponding filter elements in the filter element group.
Further, the filter comprises a purified liquid output channel component extending out of the shell and a filter element group which is downwards arranged into the reactor from a filter mounting port; the filter element group is suspended at the lower end of the purified liquid output channel part and is wholly or partially arranged below the liquid level of a substance to be filtered in the reactor after the reaction of the reactor is finished.
Further, the purified liquid output channel part is directly connected with the filter elements in the filter element group.
Furthermore, the upper end of the filter element in the filter element group is provided with a filter element joint which is in threaded connection with the purified liquid output channel component.
Through adopting this filter of realizing reaction and concentrated system of filtering, the reaction of raw materials, filter and concentrate and go on in concentrating on a container in the reactor, the equipment quantity that uses is still less, equipment area is less, core group is unsettled to be installed at the lower extreme of net liquid transfer passage part and by whole or most arrange reactor reaction completion in treat under the filter liquid level, filter core group more with above-mentioned treat that the lower upper strata of solid content waits to filter the contact in the filter, help improving and filter concentration efficiency.
The invention also provides a filter of the system for realizing reaction, filtration and concentration, which can be better arranged in the reactor, the filter is arranged in the reactor with the stirrer through a filter mounting port on the reactor, the filter comprises a filter element assembly arranged in the reactor, and the filter element in the filter element assembly is a hollow filter element made of inorganic porous materials with a cylindrical structure. The inorganic porous material herein is, for example, SiC, FeAl, TiAl, NiAl, TiSiC, Ti or the like. The porosity of the filter element here is 15-40%.
Specifically, the radial crushing strength of the filter element is more than 185 MPa.
Specifically, the wall thickness of the filter element is 5-15 mm.
Specifically, the stress of the filter element is calculated according to the cantilever beam, and the moment born by the maximum stress surface of the filter element is 147.4-188.3 N.m.
Specifically, the outer diameter of the filter element is 45-55 mm.
Specifically, the distance between the filter element and the stirrer in the reactor is 0.05-1.5 m.
Specifically, the filter element is a sintered inorganic porous material.
Specifically, the filter element is a metal porous material filter element.
Specifically, the filter element is a cylindrical filter element formed by folding a metal porous material.
Specifically, the lower end of the filter element is provided with a sealing cover for sealing the lower end opening of the filter element.
Specifically, the filter further comprises a filter element limiting plate for limiting the filter element.
Specifically, the filtering area of the filtering element is 0.03-0.25.
The filter element in the filter of the system for realizing reaction and filtration concentration can be better arranged in the reactor, and the operation in the reactor is more reliable and safer.
The invention is further described with reference to the following figures and detailed description. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to assist in understanding the invention, and are included to explain the invention and their equivalents in the description and should not be taken to limit the invention to the proper form disclosed herein. In the drawings:
FIG. 1 is a schematic structural diagram of an embodiment of an apparatus for carrying out reaction and filtration concentration according to the present invention;
FIG. 2 is a schematic structural diagram of an embodiment of the apparatus for carrying out the reaction and filtration concentration according to the present invention;
FIG. 3 is a schematic structural diagram of an embodiment of the apparatus for carrying out the reaction and filtration concentration according to the present invention;
FIG. 4 is a schematic diagram of another filter of the apparatus for carrying out the reaction and filtration concentration according to the present invention;
FIG. 5 is an enlarged view of a portion of FIG. 4 at A;
FIG. 6 is a schematic top view of a cover of another filter of the apparatus for performing reaction and filtration concentration according to the present invention;
FIG. 7 is a schematic bottom view of a fixed plate of another filter of the apparatus for performing reaction and filtration concentration according to the present invention;
FIG. 8 is a schematic view of another filter middle ring plate in the apparatus for carrying out the reaction and filtration concentration according to the present invention;
fig. 9 is a schematic structural view of a system for producing a precursor of a positive electrode material according to the present invention;
FIG. 10 is a schematic view of a filter cartridge;
FIG. 11 is a schematic cross-sectional view of the filter material and a schematic cross-sectional view of the adapter of the filter cartridge of FIG. 10;
labeled as: a filtration reaction device 1, a purified liquid output port 11, a gas-liquid separation device 2, a supplied material input port 2a, a liquid output port 2b, a gas output port 2c, a power device 3, a circulating water tank 31, a gas material input port 31a, a liquid material output port 31b, a liquid material input port 31c, a condensing device 32, a pump body 33, a reactor 100, a shell 110, a shell top 111, a filter mounting port 112, a filter 200, a purified liquid output channel part 210, the filter comprises a sealing head 211, a pipe joint 212, a pipe joint 213, a purified liquid conveying channel component 220, a first cylinder structure 221, a first cylinder structure lower end plate 222, a first cylinder structure upper end plate 223, a bolt connector 224, a purified liquid conveying pull pipe 225, a cover plate 226, a filter element group 230, a filter element 231, a second cylinder structure 240, a filter element limiting plate 241, a purified liquid output pipe 300, a cover body 310, a ring plate 320, a fixing plate 330 and a filter element unit 340.
Detailed Description
The embodiment adopts a method for preparing a precursor of a positive electrode material, which comprises the following steps:
supplying a raw material containing a metal salt solution for preparing a precursor of a cathode material to the reactor 100; the raw materials are promoted to react to generate a precursor of the anode material, and the metal salt solution for ensuring the growth of the precursor of the anode material to the set requirement is continuously provided for the reactor 100 in the growth process of the precursor of the anode material;
performing solid-liquid separation filtration on the solution in the reactor 100 through a filter element located in the reactor 100 so as to maintain the amount of the liquid in the reactor 100 in a range required for the reaction; and discharging the precursor of the cathode material after the precursor grows to the set requirement. The extracted solution is outputted from the purified liquid output port 11 of the filter, and then subjected to gas-liquid separation.
By adopting the preparation method of the precursor of the cathode material, the reaction, filtration and concentration of the raw materials are concentrated in the reactor 100 in one container, so that the quantity of equipment for preparing the precursor of the cathode material is less, the occupied area of the equipment is smaller, the raw materials do not need to circularly flow in a plurality of reactors 100 or containers, and a certain amount of solution can be directly subjected to solid-liquid separation through a filter.
The preparation method comprises preparing the precursor of the cathode material by at least one group of process units; the group of process units comprises:
charging a raw material containing a metal salt solution for preparing a precursor of a positive electrode material into the reactor 100;
when the liquid level in the reactor 100 drops to the first position, the raw materials are continuously fed into the reactor 100;
when the liquid level in the reactor 100 rises to the second position, the above-mentioned solid-liquid separation of the solution in the reactor 100 is performed by the filter element.
When the preparation is required to be carried out through a plurality of groups of the process units, the plurality of groups of the process units are carried out continuously or at intervals.
Thus, according to actual needs, such as the requirement of the size of crystals formed in the reactor 100 and the whole amount, an automatic program can be set, a liquid level meter and the like are arranged, when the first position or the second position is reached, the suction action (through a filter) and the feeding action are respectively started, so that no surplus liquid is easy to circulate with other containers through other pipelines, and the number of used equipment is reduced.
There may also be another mode of operation, including the following:
continuously or intermittently feeding a raw material containing a metal salt solution for preparing a precursor of the positive electrode material to the reactor 100; meanwhile, the solution in the reactor 100 is subjected to the solid-liquid separation through the filter element, so that the height of the liquid level in the reactor 100 is kept within a preset range value. This dynamic feeding and filtering allows the reactor 100 to operate efficiently.
The precursor of the cathode material is obtained, and the precursor of the cathode material is the reaction product concentrate prepared by the preparation method of the precursor of the cathode material. The precursor of the anode material is a precursor of a ternary anode material.
As shown in fig. 9, the method for preparing a precursor of a positive electrode material uses a system for preparing a precursor of a positive electrode material, and includes:
a filtration reaction apparatus 1 comprising a filter 200 and a reactor housing 110 provided with a reaction raw material input port and a reaction product concentrate output port, the filter being disposed or partially disposed in the housing through a mounting port on the top of the housing; the outer layer of the filtering reaction device 1 can be provided with a jacket layer;
the gas-liquid separation device 2 comprises a gas-liquid separation shell provided with a material input end, a gas output end and a liquid material output end; the liquid material input end is communicated with a purified liquid output port 11 of the filter;
a power unit 3 including a pump body 33 communicating with the gas-liquid separation device 2; alternatively, the power unit 3 includes a pump body 33 communicating with the gas-liquid separator 2 and the filter.
By adopting the preparation system of the precursor of the anode material, the reaction, the filtration and the concentration can be completed only by one reactor 100, and the preparation of the precursor of the anode material has the advantages of less used equipment and small occupied area.
The gas-liquid separation device 2 herein may be provided in two arrangements.
One is as follows: the gas-liquid separation device 2 mainly comprises at least gas-liquid separators connected in series, and each gas-liquid separator comprises a supplied material inlet 2a, a liquid outlet 2b and a gas outlet 2 c; the gas outlet 2c of the gas-liquid separator at the front end communicates with the incoming material inlet 2a of the gas-liquid separator at the rear end. Two gas-liquid separators which are connected in series are adopted, so that two-stage gas-liquid separation can be conveniently realized, and the gas-liquid separation is more sufficient and accurate.
The other is as follows: the gas-liquid separation device 2 mainly comprises two gas-liquid separators which are connected in parallel, wherein each gas-liquid separator comprises a material inlet 2a, a liquid outlet 2b and a gas outlet 2 c; the incoming material input ports 2a of the two gas-liquid separators are communicated with the clean liquid output port 11 of the filter. By adopting the parallel connection mode, one of the two can be used as a standby device when in use.
The power device 3 comprises a circulating water tank 31, the circulating water tank 31 is provided with a gas inlet 31a communicated with the gas outlet 2c, and the circulating water tank 31 is provided with a condensing device 32 for condensing the input gas; a liquid outlet 31b at the bottom of the circulating water tank 31 is communicated with a liquid inlet 31c at the upper part of the circulating water tank 31 through a pump 33; the pump body 33 is connected to the gas outlet 2c of the gas-liquid separator 2 and used for pumping gas. The condensing means 32 may be a water-cooled tube jacket.
In this embodiment, a device for carrying out the reaction and the filtration and concentration is used as the reactor.
FIG. 1 is a schematic structural diagram of an embodiment of the apparatus for carrying out the reaction and the concentration by filtration according to the present invention. As shown in FIG. 1, the apparatus for performing reaction and filtration concentration comprises a reactor 100 and a filter 200, wherein the reactor 100 comprises a reactor shell 110 having a reaction raw material inlet (not shown) and a reaction product concentrate outlet (not shown), the reactor shell 110 has a shell top 111, the shell top 111 is provided with a filter mounting port 112, the filter 200 comprises a net liquid outlet passage member 110 mounted on the filter mounting port 112, and a net liquid outlet passage member 220 and a filter element group 230 which are downwardly mounted into the reactor 100 from the filter mounting port 112, the filter element group 230 is suspended at the lower end of the net liquid outlet passage member 220 and is wholly or mostly disposed below the liquid level of the filtered material in the reactor 100 after the reaction in the reactor 100 is completed, and the net liquid outlet (not numbered) of the filter element group 230 at the upper end passes through the net liquid outlet passage member 220 and the net liquid outlet passage member 220 The outlet passage member 110 is connected to and forms a net liquid output flow path.
The device for realizing reaction and filtering concentration according to the above, wherein the "reaction raw material input port" means: an input port on reactor 100 is configured to receive a reactant material that reacts physically and/or chemically in reactor 100 to produce a reaction product. By "reaction product concentrate outlet" is meant: an outlet on the reactor 100 for discharging a reaction product concentrate, which is the reaction product after the concentration process in the reactor 100. The liquid level of the substance to be filtered refers to: the aforementioned reaction raw materials are physically and/or chemically reacted in the reactor 100 to obtain a liquid level position of the reaction product in the reactor 100 before being filtered by the filter element group 230. The 'filter element group clean liquid output port' refers to: the filter element group 230 is provided with an output port for outputting filtered liquid (clean liquid). The "purified liquid conveying channel component" refers to a component or structure for conveying purified liquid from the purified liquid output port of the filter element group to the purified liquid output channel component. The "net liquid output passage member" means a member or structure for outputting net liquid from the filter 200 to the outside.
The apparatus for performing the reaction and the concentration by filtration as described above is mainly characterized in that the reactor 100 and the filter 200 are integrated into the same device. Wherein the filter 200 is installed from the filter installation port 112 on the case top 111 of the reactor case 110 of the reactor 100, the net liquid outlet passage member 110 of the filter 200 is installed on the filter installation port 112, and the net liquid transfer passage member 220 and the filter element group 230 below the net liquid outlet passage member 110 are downwardly installed into the reactor 100 from the filter installation port 112. Therefore, the filter 200 can be conveniently installed and disassembled on the reactor 100, and particularly, the filter 200 can be additionally installed on the existing reactor 100, so that the existing reactor 100 can be quickly modified. In the case where the reaction apparatus and the filtration and concentration apparatus for filtration and concentration are different from each other in the past, if the reaction apparatus is the reactor 100 (e.g., a reaction vessel), the filter 200 may be additionally installed in the reaction apparatus, so that the apparatus for reaction and filtration and concentration can be realized, thereby reducing the number of apparatuses and the floor space of the apparatus. Since the filter element assembly 230 of the filter 200 is suspended at the lower end of the clean liquid conveying channel part 220 and is wholly or mostly placed below the liquid level of the substance to be filtered in the reactor 100 after the reaction in the reactor 100 is completed, the filter element assembly 230 is more contacted with the substance to be filtered at the upper layer with lower solid content in the substance to be filtered, which is helpful for improving the filtration and concentration efficiency.
According to the device for realizing reaction, filtration and concentration, the working process is as follows: 1) the reaction process is as follows: the reaction raw materials enter the reactor 100 from the reaction raw material input port and perform physical and/or chemical reaction in the reactor 100 to obtain a reaction product; 2) and (3) filtering and concentrating: after the reaction process, by activating the filter 200 (mainly including an operation of forming a filtering pressure difference on both sides of the filtering surface formed by the filter element group 230, which is generally performed by a pump connected to the net liquid output channel part 110), the reaction product is subjected to solid-liquid separation, and the net liquid separated by the solid-liquid separation is output through the net liquid transfer channel part 220 and the net liquid output channel part 110, thereby leaving a reaction product concentrate in the reactor 100; 3) reaction product concentrate discharge process: the reaction product concentrate exits the reactor 100 through a reaction product concentrate outlet.
The reaction process and the filtration and concentration process can be carried out alternately or simultaneously, and can be adjusted according to actual requirements.
According to the above device for implementing reaction and filtering concentration, the clean liquid conveying channel part 220 specifically relates to the following structure: the purified liquid conveying channel component 220 is mainly composed of a first cylinder structure 111, the central axis of the first cylinder structure 111 is arranged along the vertical direction, a first cylinder structure lower end plate 222 is arranged at the lower port of the first cylinder structure 111, the filter element group 230 is arranged on the first cylinder structure lower end plate 222, and the purified liquid outlet of the filter element group is communicated with the inner space of the first cylinder structure 111; a first cylinder structure upper end plate 223 is disposed at the upper end opening of the first cylinder structure 211, the upper end opening of the first cylinder structure 211 extends upward to the vicinity of the filter mounting opening 112 so that the first cylinder structure upper end plate 223 is located above the filter mounting opening 112, the first cylinder structure upper end plate 223 is also connected to the flange 113 on the filter mounting opening 112 and the flange 114 on the purified liquid outlet passage member 110 through a bolt connector 224 as a flange, specifically, the first cylinder structure upper end plate 223 is clamped between the flange 113 on the filter mounting opening 112 and the flange 114 on the purified liquid outlet passage member 110, and the first cylinder structure upper end plate 223, the flange 113 on the filter mounting opening 112 and the flange 114 on the purified liquid outlet passage member 110 are connected through the same bolt connector 224, so that the net liquid outlet passage member 110 is installed on the first cylinder structure upper end plate 223 and communicates with the inner space of the first cylinder structure 211.
According to the net liquid transporting passage part 220 of the apparatus for performing reaction and filtration concentration, since the lower port of the first cylinder structure 211 is provided with the first cylinder structure lower end plate 222 and the filter element group 230 is mounted on the first cylinder structure lower end plate 222, and the upper port of the first cylinder structure 211 extends upward to the vicinity of the filter mounting port 112 so that the first cylinder structure upper end plate 223 is positioned above the filter mounting port 112 and the first cylinder structure upper end plate 223 is used as a flange plate to be simultaneously connected with the flange plate 113 on the filter mounting port 112 and the flange plate 114 on the net liquid output passage part 110 through the bolt connection 224, the first cylinder structure 211 as a whole functions to connect the filter element group 230 with the net liquid output passage part 110, and the part of the filter element group 230 functioning as a filtration function is more placed below the liquid level of the object to be filtered in the reactor 100 after the reaction of the reactor 100 is completed through the first cylinder structure 211, ensuring an effective use area of the filter element group 230.
According to the above-mentioned device for performing reaction and filtering concentration, the purified liquid outlet channel member 110 specifically includes a sealing head 111 located on the filter mounting opening 112 and a pipe joint 112 disposed on the sealing head 111, and the sealing head 111 is mounted on the filter mounting opening 112 through a flange at the lower end of the sealing head 111 (a flange 114 on the purified liquid outlet channel member 110).
According to the device for implementing the reaction and the filtration concentration, the lower end of the first cylinder structure 211 is further provided with a second cylinder structure 240 extending downwards, the filter element group 230 is located in the second cylinder structure 240, and the second cylinder structure 240 is provided with through holes for the substance to be filtered to enter between the second cylinder structure and the filter element group; in addition, the inner side of the second cylinder 240 is further provided with a filter element limiting plate 241, 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.
The second cylinder structure 240 may accommodate the filter element assembly 230, so as to protect the filter element assembly 230; because the inner side of the second cylinder structure 240 is further provided with a filter element limiting plate 241, 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.
FIG. 2 is a schematic structural diagram of an embodiment of the apparatus for carrying out the reaction and filtration concentration according to the present invention. As shown in FIG. 2, the apparatus for performing reaction and filtration concentration comprises a reactor 100 and a filter 200, wherein the reactor 100 comprises a reactor shell 110 having a reaction raw material inlet (not shown) and a reaction product concentrate outlet (not shown), the reactor shell 110 has a shell top 111, the shell top 111 is provided with a filter mounting port 112, the filter 200 comprises a net liquid outlet passage member 110 mounted on the filter mounting port 112, and a net liquid outlet passage member 220 and a filter element group 230 which are downwardly mounted into the reactor 100 from the filter mounting port 112, the filter element group 230 is suspended at the lower end of the net liquid outlet passage member 220 and is wholly or mostly disposed below the liquid level of the filtered material in the reactor 100 after the reaction in the reactor 100 is completed, and the net liquid outlet (not numbered) of the filter element group 230 at the upper end passes through the net liquid outlet passage member 220 and the net liquid outlet passage member 220 The outlet passage member 110 is connected to and forms a net liquid output flow path.
According to the above-mentioned device for implementing reaction and filtering concentration, the above-mentioned clean liquid conveying channel component 220 is mainly composed of a first cylinder structure 211, the central axis of the first cylinder structure 211 is arranged along the vertical direction, the lower port of the first cylinder structure 211 is provided with a first cylinder structure lower end plate 222, the above-mentioned filter element group 230 is installed on the first cylinder structure lower end plate 222 and the filter element clean liquid outlet is communicated with the inner space of the first cylinder structure 211; a first cylinder structure upper end plate 223 is arranged at an upper end opening of the first cylinder structure 211, the first cylinder structure upper end plate 223 is lower than the filter mounting opening 112 by a certain distance, the first cylinder structure 211 and a filter element group 230 below the first cylinder structure 211 are hung below the clean liquid output channel part 110 through a clean liquid conveying pull pipe 225 connected to the first cylinder structure upper end plate 223, the clean liquid conveying pull pipe 225 conducts the clean liquid output channel part 110 with the inner space of the first cylinder structure 211, and the length of the clean liquid conveying pull pipe 225 can enable the first cylinder structure 211 to be integrally arranged below the liquid level of a substance to be filtered in the reactor 100 when the reaction of the reactor 100 is completed; a cover plate 226 is mounted on the filter mounting port 112, the upper end of the clean liquid conveying pull pipe 225 is mounted on the cover plate 226, and the outer edge of the cover plate 226 is clamped between the flange 113 on the filter mounting port 112 and the flange 114 on the clean liquid output channel member 110 which are connected together by the bolt connector 224; the purified liquid outlet passage member 110 includes a cap 111 disposed on the filter mounting opening 112 and a pipe joint 112 disposed on the cap 111, and the cap 111 is mounted on the filter mounting opening 112 through a flange at the lower end of the cap 111 (a flange 114 on the purified liquid outlet passage member 110).
Because the filter element group 230 below the first cylinder structure 211 and the first cylinder structure 211 is hung below the clean liquid output channel part 110 through the clean liquid conveying pull pipe 225 connected to the upper end plate 223 of the first cylinder structure, the internal volume of the first cylinder structure 211 is compressed by the arrangement of the clean liquid conveying pull pipe 225, and the pipe diameter of the clean liquid conveying pull pipe 225 per se is smaller, therefore, the whole capacity of the clean liquid conveying channel part 220 of the structure is smaller, and more clean liquid can be output.
According to the device for implementing the reaction and the filtration concentration, the lower end of the first cylinder structure 211 is also provided with a second cylinder structure 240 extending downwards, 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 substance to be filtered to enter between the second cylinder structure and the filter element group; in addition, the inner side of the second cylinder structure 240 is further provided with a filter element limiting plate 241, 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.
FIG. 3 is a schematic structural diagram of an embodiment of the apparatus for carrying out the reaction and filtration concentration according to the present invention. As shown in fig. 3, the net liquid conveying channel part 220 of the device for realizing reaction and filtration concentration specifically relates to the following structure: the purified liquid conveying channel component 220 is mainly composed of a first cylinder structure 211, the central axis of the first cylinder structure 211 is arranged along the vertical direction, a first cylinder structure lower end plate 222 is arranged at the lower port of the first cylinder structure 211, the filter element group 230 is arranged on the first cylinder structure lower end plate 222, and the purified liquid outlet of the filter element group is communicated with the inner space of the first cylinder structure 211; a first cylinder structure upper end plate 223 is arranged at an upper end opening of the first cylinder structure 211, the first cylinder structure upper end plate 223 is lower than the filter mounting opening 112 by a certain distance, the first cylinder structure 211 and a filter element group 230 below the first cylinder structure 211 are hung below the clean liquid output channel part 110 through a clean liquid conveying pull pipe 225 connected to the first cylinder structure upper end plate 223, the clean liquid conveying pull pipe 225 conducts the clean liquid output channel part 110 with the inner space of the first cylinder structure 211, and the length of the clean liquid conveying pull pipe 225 can enable the first cylinder structure 211 to be integrally arranged below the liquid level of a substance to be filtered in the reactor 100 when the reaction of the reactor 100 is completed; a cover plate 226 is mounted on the filter mounting port 112, the upper end of the clean liquid conveying pull pipe 225 is mounted on the cover plate 226, and the outer edge of the cover plate 226 is directly used as a flange and is connected with the flange 113 on the filter mounting port 112 through a bolt connector 224; the clean liquid discharge passage part 110 includes a pipe joint 113 provided at an upper end of the clean liquid feeding pull pipe 225.
As shown in fig. 4 to 8, in the present embodiment, the filter 200 in the reactor 100 can be directly replaced by another filter structure, which omits the first cylinder and the second cylinder, and the filter element is directly connected to the outside of the reactor through a continuous pipe, and the filter includes a clean liquid outlet passage member protruding from the reactor shell 110 and a filter element group downwardly installed into the reactor 100 from the filter installation port 112, and the clean liquid outlet passage member is provided to communicate the filter element with the clean liquid outlet pipe 300 outside the reactor 100; wherein, the filter element group is suspended at the lower end of the purified liquid output pipe 300 and is wholly or mostly arranged below the liquid level of the substance to be filtered in the reactor 100 after the reaction of the reactor 100 is finished. That is, the continuous purified liquid output pipe 300 of the structure is directly communicated with the filter element group, and the filter element group is directly arranged in the reactor 100.
The reactor shell 110 is provided with a cover 310, and the purified liquid output pipe 300 is connected to the filter element assembly through holes distributed on the cover 310, wherein the cover 310 is a flange. The cover 310 may be regarded as the same component as the cover in the above-mentioned another structure, that is, the functions of the cover are to allow the filter to be stably mounted on the reactor housing 110 of the reactor 100. The cover 310 may be fixed by the cover plate, i.e., the outer edge of the cover plate is clamped between the flange on the filter mounting opening 112 and another flange, or the outer edge of the cover 310 on the filter mounting opening 112 is directly used as a flange and connected to the flange on the filter mounting opening 112 by a bolt. Here, a transversely arranged ring plate 320 is disposed in the reactor shell 110, and the outer side of the ring plate 320 is fixedly connected to the middle section of the purified liquid outlet pipe 300, so as to form a structure in which the purified liquid outlet pipe 300 is annularly distributed on the outer side of the ring plate 320. The ring plate 320 can be welded to fix the outer side of the net liquid outlet pipe 300, and the net liquid outlet pipe 300 is arranged on the outer side of the ring plate 320 in a circular shape. After the ring plate 320 is arranged, the purified liquid output pipe 300 is prevented from shaking, namely, a plurality of purified liquid output pipes 300 are bound together, so that the purified liquid output pipe 300 can be stable.
A fixing plate 330 is disposed in the reactor housing 110, and the fixing plate 330 is connected to the lower end of the filter element assembly; the filter element group is composed of a plurality of filter element units 340 which are arranged annularly, the fixing plate 330 is provided with holes which correspond to the lower ends of the filter element units 340 and are used for limiting the filter element units 340, and the lower ends of the filter element units 340 of the filter element group are fixed through bolts which penetrate through the holes. A reinforcing rib, such as a cross-shaped bracket, may be provided at a middle portion of the fixing plate 330. The fixing plate 330 is formed in a disk shape, and the holes may be elongated holes extending along the periphery of the fixing plate 330 to improve the flexibility of installation. The upper end of the filter element unit 340 may be provided with a joint which is screw-coupled with the purified liquid output pipe 300.
According to the apparatus for implementing the reaction and the filtering concentration, the reactor 100 is a reactor 100 for preparing the ternary material precursor, the reaction raw material input port is used for inputting a raw material for preparing the ternary material precursor into the reactor 100, and the reaction product concentrate output port is used for outputting the concentrated ternary material precursor from the reactor 100.
The above apparatus for implementing reaction and filtration concentration can adopt a modification method, which modifies the existing reactor 100 and reaction kettle to form the reactor 100 for performing reaction filtration concentration, and the modification method comprises the following operations: preparing a filter to be placed in the reactor 100; the reactor 100 ensuring the reaction and the concentration by filtration is provided with an opening to the inside of the reactor 100; extending a filter into said reactor 100 through said opening; the filter is fixed to the reactor 100. By means of the method, it is possible to add filters to an existing reactor 100 in an ideal manner, enabling rapid retrofitting of an existing reactor 100. The reactor (reaction kettle) maintains normal pressure or micro-positive pressure, the filter element is connected to a vacuum system through a vacuum tank, and negative pressure is established by a vacuum pump, so that pressure difference is formed between the outer side and the inner side of the filter element, a liquid phase penetrates through the filter element to form a filtrate, and a solid phase is intercepted in the reaction kettle to achieve the purpose of material concentration.
When the reactor 100 is originally provided with an opening, a filter is inserted into the reactor 100 through the opening; wherein the opening of the reactor 100 is expanded or contracted depending on the size of the filter. In the case of the above-mentioned hole shrinkage, a mounting member having a hole corresponding to the size of the filter is formed according to the size of the filter, and the mounting member is attached to the opening of the reactor 100 by welding, bonding or flange. The mounting members are sized to fit within the openings in the reactor 100.
In a modification, a flange hole is formed in an open circumference of the reactor 100, and a portion of the filter to be fixed to the reactor 100 is flange-mounted to the reactor 100 after the filter is inserted into the reactor 100.
In another modification, a corresponding filter mounting seat of a pipe structure is installed at the opening of the reactor 100, and the filter is inserted into the reactor 100 through the filter mounting seat and fixed to the reactor 100.
In another modification, a flange is provided at an 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 by the flange.
In the above three modifications, a connector may be provided on the filter, and the passage formed by the net liquid outlet passage member and the net liquid transport passage member (in the structure without the net liquid transport passage member, the passage is referred to as the net liquid outlet pipe 300) passes through the connector and protrudes, and the connector blocks the opening after the filter is inserted into the reactor 100.
When refitting, the sealing cover can be additionally arranged, and the method specifically comprises the following steps:
preparing a sealing cover which is a hollow structure with an opening at the lower end;
the sealing cover is provided with an opening for the pipeline on the filter to pass through;
after the filter is inserted into the reactor 100, the above-mentioned coupling member can be clamped between the cover and the reactor shell 110 of the reactor 100.
Bolts sequentially penetrating through the sealing cover, the connecting piece and the reactor shell 110 are used for fixing the three; alternatively, the connection member is clamped between the cover and the reactor shell 110 using bolts sequentially passing through the cover and the reactor shell 110.
The filter of the system for realizing reaction and filtration concentration is adopted in the embodiment, can be better arranged in the reactor, and can run more stably and reliably.
Referring to fig. 1 to 4, the present invention further provides a filter of a system for performing a reaction and filtering concentration, which can be preferably disposed in a reactor, the filter being disposed in the reactor with a stirrer through a filter mounting port on the reactor, the filter including a filter element assembly disposed in the reactor, wherein a filter element (the filter element is a filter element 231 or a filter element unit 340) in the filter element assembly is a filter element of an inorganic porous material having a hollow cylindrical structure. The radial crushing strength of the filter element is 185-340 MPa.
Preferably, the thickness of the filter element is 5 to 15 mm. And calculating the stress of the filter element according to the cantilever beam, wherein the moment borne by the maximum stress surface of the filter element is 147.4-188.3 N.m. Preferably, the outer diameter of the filter element is 45-55 mm. The filter element is a metal porous material filter element.
One arrangement of the filter element is a cylindrical filter element formed by folding a metal porous material. Namely, the metal porous material is folded in a digital mode to form folds and then is enclosed into a cylindrical structure. Specifically, the lower end of the filter element is provided with a sealing cover for sealing the lower end opening of the filter element.
Yet another arrangement is to directly use a formed, hollow, cylindrical metal porous material filter element.
The filter is provided with a filter element limiting plate 241 at a proper position for preventing the vibration of the filter element group.
The distance between the filter element and the stirrer in the reactor is 0.05-1.5 m.
The filtering area of the filtering element is 0.03-0.25.
The description is given in terms of strength experiments for the filter elements in the filter element group.
In the reactor, because the inclined blades are adopted in the embodiment, the blades form an angle of 30 degrees with the horizontal plane, in the stirring process, the blades generate lift force and resistance under the action of fluid, and the fluid moves due to the reaction force of the lift force and the resistance and flows in the radial direction, the axial direction and the annular direction to form a complex flow pattern.
The lift force component enables the fluid to flow downwards along the axis of the stirring paddle, and the fluid turns back after being far away from the paddle blade or reaching the bottom of the container to form an annular flow component which is upward along the axis direction of the stirring paddle.
The resistance component enables the fluid to generate a velocity component along the tangential direction of the motion direction of the blades, a part of the component rises or falls along the cylinder wall to form a radial flow component under the approximate speed of the cylinder wall, and the other part of the component moves along with the blades to form a circumferential flow component.
The three-directional fluid motion components generated by the stirring generate acting force on the filter element which is static in the container, and the acting force can be similarly decomposed into three-directional components to be examined, wherein in the three-directional components, the axial flow component is parallel to the filter element, the projection area of the filter element on the cross section which is vertical to the flow direction is very small, and the axial acting force is negligible relative to the other two directions.
For the component of the annular flow to the radial flow, the directions of the component of the annular flow and the component of the radial flow are perpendicular to the axis of the filter element, the annular component and the radial component are respectively generated by the reaction force of the lift force and the resistance force, and the premise that the fluid generates the lift force and the resistance force on the blade is in the moving direction of the blade, so that the flow speed of the fluid relative to the filter element in the radial direction and the annular direction is smaller than the edge linear speed of the blade, and the stress of the filter element is smaller than the fluid resistance force generated by. According to cantilever structure moment distribution characteristics, apart from the part that the stiff end is closer, its moment is bigger, combines filter core structure characteristics to carry out the analysis, and the filter core has two weak positions: the joint is connected with the filter material, which is the position where the torque borne by the cross section of the filter material is the largest, and the position near a welding seam is the lowest material strength; and the other part is the connection part of the connecting pipe and the external thread joint, although the material strength is far higher than that of the filter element, the cross section area and the cross section diameter are very small due to thread turning, and the connecting pipe is also a weak part.
The stress condition of the filter element is shown in detail in figure 10, the length of the force arm is the distance from the geometric center of the filter element to the stress surface, the length of the force arm of the weak surface of the filter element cattail is 248mm, and the length of the force arm of the weak surface of the connecting pipe is 255 mm.
Substituting the fluid resistance value, and calculating the maximum torque caused by stirring at each calamus position:
thick filter element MThickness max＝261.1N×0.248m＝84.28N.m
Thin filter element MThin max＝261.1N×0.248m＝84.28N.m
Connecting pipe MIs connected to max＝261.1N×0.255m＝81.97N.m
For example, the section of the thick filter element is measured by the actual measurement of the outer diameter of 47mm, and the wall thickness is not less than 5 mm; actually measuring the outer diameter of the cattail filter element to be 50mm, and the wall thickness of the cattail filter element is not less than 3 mm; the theoretical dimension of the cross-section of the nozzle is shown in fig. 10, and the actual outer diameter is calculated as 90% of the theoretical outer diameter in consideration of the dimensional tolerance.
The tubular filter element can be regarded as a hollow cylinder, and the section coefficient of the tubular filter element is calculated according to the following formula:
Figure BDA0002532546190000181
wherein:
coefficient of area of Wz
D, the outer diameter of the cylinder;
the ratio of the inner diameter to the outer diameter of the alpha hollow cylinder.
The weak point is thus calculated: wIs thick and thick＝6.28×10-6，WThin sheet＝4.91×10-6，WIs connected with＝6.61×10-7。
According to the filter element crushing test data, the minimum compressive strength of the filter element is 185MPa, and the test data is as follows:
table 1 filter element crushing experimental data
Figure BDA0002532546190000182
According to the relevant literature of the strength of the sintered titanium-aluminum filter element, the tensile strength of the titanium-aluminum filter element is related to the granularity of materials and the pressing pressure, and the smaller the granularity is, the larger the pressing pressure is, and the higher the strength of the filter element is.
The tensile strength of the filter element is much less than the crushing strength of the filter element, so that the filter element will first break from the tensile side when subjected to a bending moment. The tensile strength of the filter element is larger than 30Mpa, and the maximum stress which can be borne by the filter element material is calculated conservatively by using 30 Mpa.
The relationship between the section stress of the filter element and the moment is as follows:
σmax＝Mmax/Wz
wherein:
the maximum stress that the sigma max filter element can bear;
the maximum moment that the cross section of the M max filter element can bear;
wz filter element section factor.
Calculate the filter core atress according to the cantilever beam, the moment that thick filter core filter media can bear at the biggest stress face is:
Mis thick and thick＝WIs thick and thick×σIs thick and thick
＝6.28×10-6×30Mpa
＝188.3N.m
The moment that the biggest stress surface of thin filter core filter media can bear is:
Mthin sheet＝WThin sheet×σThin sheet
＝4.91×10-6×30Mpa
＝147.4N.m
The moment that the biggest stress surface of filter core takeover department can bear is (316L tensile strength 500 Mpa):
Mis connected with＝WIs connected with×σIs connected with
＝6.61×10-7×500Mpa
＝330.7N.m
The maximum moment that can bear and the maximum moment that the stirring can produce are compared to the weak department of filter core:
and (3) thick filter element: mIs thick and thick＝188.3N.m＞MThickness max＝81.97N.m
Thin filter element: mThin sheet＝147.4N.m＞MThin max＝81.97N.m
Taking over: mIs connected with＝330.7N.m＞MIs connected to max＝84.28N.m
It can be seen that the maximum torque that the thick filter element and the thin filter element can bear at the weak position of the filter element is far larger than the maximum torque that can be generated by stirring, and the filter element can be reliably arranged in a reactor.
The contents of the present invention have been explained above. Those skilled in the art will be able to implement the invention based on these teachings. All other preferred embodiments and examples, which can be obtained by a person skilled in the art without inventive step based on the above description of the invention, shall fall within the scope of protection of the present invention.

Claims (10)

1. Realize the filter of reaction and the concentrated system of filtration, its characterized in that, the filter is used for setting up in the reactor shell of the concentrated system of realization reaction and filtration, is provided with the filter installing port on this reactor shell, the installation with the reactor shell is realized through this filter installing port to the filter, and this filter includes:
the upper end of the purified liquid output channel part extends out of the reactor and is used for outputting purified liquid;
the filter element group is used for carrying out solid-liquid separation on the raw material of the metal salt solution in the reactor;
the filter element group is suspended at the lower end of the purified liquid conveying channel part and is wholly or mostly arranged below the liquid level of the substance to be filtered in the reactor after the reaction of the reactor is finished.
2. The filter of a system for carrying out reactions and filtration concentrations of claim 1, wherein:
the filter element group purified liquid outlet at the upper end of the filter element group is connected with the purified liquid output channel part through a purified liquid conveying channel part to form a purified liquid output flow path;
the net liquid conveying channel component mainly comprises a first cylinder structure, and the central axis of the first cylinder structure is arranged along the vertical direction approximately; wherein,
a first cylinder structure lower end plate is arranged at the lower port of the first cylinder structure, the filter element group is arranged on the first cylinder structure lower end plate, and a filter element group clean liquid output port is communicated with the inner space of the first cylinder structure;
the upper port of the first cylinder structure is provided with a first cylinder structure upper end plate, and the purified liquid output channel component is installed on the first cylinder structure upper end plate and is communicated with the inner space of the first cylinder structure.
3. The filter of the system for carrying out reactions and filtration concentrations of claim 2, wherein:
the upper end plate of the first cylinder structure is used as a flange plate and is connected with the flange plate on the filter mounting opening through a bolt connecting piece;
or,
the upper end plate of the first cylinder structure is used as a flange plate and is connected with the flange plate on the purified liquid output channel part through a bolt connecting piece;
or,
the upper end plate of the first cylinder structure is used as a flange plate and is clamped between the flange plate on the purified liquid output channel part and the flange plate on the filter mounting port through a bolt connecting piece and is connected through the bolt connecting piece;
or,
the upper end plate of the first cylinder structure is arranged between the flange plate on the purified liquid output channel part and the flange plate on the filter mounting port, and the flange plate on the purified liquid output channel part and the flange plate on the filter mounting port are connected through the bolt connecting piece and then clamp the upper end plate of the first cylinder structure.
4. The filter of the system for carrying out reactions and filtration concentrations of claim 2, wherein: the upper end plate of the first cylinder structure is lower than the filter mounting opening by a certain distance; then, the first cylinder structure and the filter element group below the first cylinder structure are hoisted below the clean liquid output channel part through a clean liquid conveying pull pipe connected to the upper end plate of the first cylinder structure, and the clean liquid conveying pull pipe conducts the clean liquid output channel part and the inner space of the first cylinder structure.
5. The filter of a system for carrying out reactions and filtration concentrations of claim 4, wherein: the length of the clean liquid conveying pull pipe can enable the first cylinder structure to be integrally arranged below the liquid level of a substance to be filtered in the reactor when the reaction of the reactor is finished.
6. The filter of a system for carrying out reactions and filtration concentrations of claim 5, wherein: the filter mounting port is provided with a cover plate, and the upper end of the purified liquid conveying pull pipe is mounted on the cover plate; the outer edge of the cover plate is clamped between a flange on the filter mounting port and a flange on the purified liquid output channel part which are connected together through a bolt connecting piece, or the outer edge of the cover plate is directly used as a flange to be connected with the flange on the filter mounting port through the bolt connecting piece;
if the outer edge of the cover plate is directly used as a flange plate and is connected with the flange plate on the filter mounting opening through a bolt connecting piece, the purified liquid output channel part comprises a pipeline joint arranged at the upper end of the purified liquid conveying pull pipe.
7. The filter of a system for carrying out reactions and filtration concentrations of claim 5, wherein: the lower end of the first cylinder structure is also provided with a second cylinder structure extending downwards, the filter element group is positioned in the second cylinder structure, and the second cylinder structure is provided with a through hole for the object to be filtered to enter between the second cylinder structure and the filter element group;
the filter element limiting plate is arranged on the inner side of the second cylinder structure, filter element limiting holes are distributed in the filter element limiting plate, and the filter element limiting holes are matched with corresponding filter elements in the filter element group respectively.
8. The filter of a system for carrying out reactions and filtration concentrations of claim 1, wherein: the filter element group comprises a net liquid output channel part extending out of the shell and a filter element group downwards loaded into the reactor from a filter mounting port;
the filter element group is suspended at the lower end of the purified liquid output channel part and is wholly or mostly arranged below the liquid level of a substance to be filtered in the reactor after the reaction of the reactor is finished.
9. The filter of a system for performing reactions and filtration concentrations of claim 8, wherein:
the purified liquid output channel part is directly connected with the filter elements in the filter element group.
10. The filter of a system for carrying out reactions and filtration concentrations of claim 1, wherein: the upper end of the filter element in the filter element group is provided with a filter element joint, and the filter element joint is in threaded connection with the purified liquid output channel component.
CN202010522361.8A 2020-06-10 2020-06-10 System for realizing reaction and filtration concentration Active CN112535892B (en)

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CN202237798U (en) * 2011-08-11 2012-05-30 河北美邦工程科技有限公司 Separation device for catalyst in benzene partial hydrogenation reaction in production process of cyclohexanone
CN202740876U (en) * 2012-06-26 2013-02-20 浙江龙华精细化工有限公司 Built-in metal filter
CN104043385A (en) * 2014-06-09 2014-09-17 新疆美克化工股份有限公司 Reaction kettle of B3D (1,4-butynediol) reaction catalyst evaluating experiment device
CN209848879U (en) * 2019-01-25 2019-12-27 成都思达能环保设备有限公司 Reaction kettle and filtering concentration assembly
CN111298496A (en) * 2020-02-21 2020-06-19 四川思达能环保科技有限公司 Device and method for realizing reaction and filtering concentration

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Publication number Priority date Publication date Assignee Title
CN202237798U (en) * 2011-08-11 2012-05-30 河北美邦工程科技有限公司 Separation device for catalyst in benzene partial hydrogenation reaction in production process of cyclohexanone
CN202740876U (en) * 2012-06-26 2013-02-20 浙江龙华精细化工有限公司 Built-in metal filter
CN104043385A (en) * 2014-06-09 2014-09-17 新疆美克化工股份有限公司 Reaction kettle of B3D (1,4-butynediol) reaction catalyst evaluating experiment device
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112535891A (en) * 2020-06-10 2021-03-23 成都思达能环保设备有限公司 Device and method for realizing reaction and filtering concentration

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