CN115432747A - Method and equipment for reducing magnetic foreign matters of ternary precursor - Google Patents

Method and equipment for reducing magnetic foreign matters of ternary precursor Download PDF

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Publication number
CN115432747A
CN115432747A CN202211206740.1A CN202211206740A CN115432747A CN 115432747 A CN115432747 A CN 115432747A CN 202211206740 A CN202211206740 A CN 202211206740A CN 115432747 A CN115432747 A CN 115432747A
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permanent magnet
ternary
magnet iron
solution
iron removal
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董柯静
王登登
刘郁
许开华
任云强
吴雨晴
周林
黄家龙
余尚清
周毅
孙越
邓凯
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Green Aike Jingmen New Energy Materials Co ltd
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Green Aike Jingmen New Energy Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00Compounds of nickel
    • C01G53/006Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03CMAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00Magnetic separation
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M2004/026Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028Positive electrodes

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Abstract

The invention discloses a method and equipment for reducing a ternary precursor magnetic foreign matter, wherein the method comprises the following steps: respectively carrying out first permanent magnet iron removal on a main raw material and an auxiliary solution required by the ternary liquid, preparing the main raw material into the ternary liquid according to the preparation requirement, and then carrying out second permanent magnet iron removal; mixing the obtained ternary solution with the required auxiliary solution, performing precipitation reaction, filter pressing and washing, performing third permanent magnet iron removal to obtain a mixed solution, and mixing the required auxiliary solution with the mixed solution to obtain a slurry solution; and (4) carrying out fourth permanent magnet iron removal on the slurry solution, dehydrating, drying and then screening to obtain a ternary precursor. By adopting the invention, the magnetic foreign matter removal of the whole process is realized, the product quality is improved, and the energy consumption is reduced.

Description

Method and equipment for reducing magnetic foreign matters of ternary precursor
Technical Field
The invention relates to the technical field of lithium ion battery materials, in particular to a method and equipment for reducing magnetic foreign matters in a precursor of a ternary lithium ion battery material.
Background
The new energy automobile is used as the development direction of the automobile industry in the future, and the power battery is used as an important component of the new energy automobile. Research shows that the high voltage and high energy density of the ternary battery are more and more concerned compared with the lithium iron phosphate battery. The ternary precursor of nickel-cobalt-aluminum and nickel-cobalt-manganese is used as the main raw material of the anode material in the lithium battery, and the foreign matter content index has decisive influence on the performance of the battery. If foreign matters exist in the metal solution and the auxiliary solution, the self-discharge and performance degradation of the battery are often caused in the manufacturing process of the battery, and even the short circuit of the battery is possibly caused, so that the safety problem is caused. Therefore, the removal of the magnetic foreign matters is particularly important in the production and preparation process of the ternary material precursor.
Chinese patent CN111018004B discloses a preparation method of a bulk phase rare earth element-doped ternary precursor and a positive electrode material thereof, which comprises the steps of crushing a sintered material, grading the particle size and removing magnetic foreign matters by a screening iron remover, wherein the method removes the magnetic foreign matters at the end of a material production process, so that the problems of introducing the magnetic foreign matters in the synthetic process of the ternary precursor and reducing the product quality exist, and the dispersion of the magnetic foreign matters can cause the pollution of a workshop and increase the cost investment.
Chinese patent CN108365214B discloses a preparation method of a high-performance small-particle-size ternary cathode material precursor, when the ternary cathode material precursor is prepared by element doping, an instrument is used for detecting and adjusting the concentration and the element content of a feed liquid and then passing through a precise filtering and demagnetizing device, the method does not remove magnetic foreign matters from raw and auxiliary materials at the front end of a material production process, if the quality of metal raw materials is different, the introduction of the magnetic foreign matters in a metal salt preparation stage cannot judge specific sources, and the total investment of time is increased; secondly, the problem that magnetic foreign matters are introduced in the subsequent process cannot be effectively solved by once iron removal in the precursor preparation process, and the method is not friendly to the health of workers.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method and equipment capable of effectively reducing the magnetic foreign matters in the precursor of the ternary lithium ion battery material.
The invention is realized by the following technical scheme.
A method for reducing a ternary precursor magnetic foreign matter comprises the following steps:
(1) Preparing a ternary liquid: respectively carrying out first permanent magnet iron removal on a main raw material and an auxiliary solution required by the ternary liquid, preparing the main raw material into the ternary liquid according to the preparation requirement, and then carrying out second permanent magnet iron removal; the auxiliary solution comprises a pure water solution, an ammonia water solution and a sodium hydroxide solution;
(2) Reaction-slurrying: mixing the ternary solution obtained in the step (1) with an ammonia water solution and a sodium hydroxide solution which are subjected to first permanent magnet iron removal treatment, carrying out precipitation reaction, filter pressing and washing to obtain a solid phase, carrying out third permanent magnet iron removal on the solid phase, mixing the solid phase with a pure water solution which is subjected to first permanent magnet iron removal treatment to obtain a slurry solution, and carrying out fourth permanent magnet iron removal on the slurry solution;
(3) Dehydration-precursor: and (3) dehydrating and drying the slurry obtained in the step (2), and then screening to obtain a ternary precursor.
And (4) further, carrying out fourth permanent magnet iron removal on the slurry liquid in the step (3), dehydrating, drying, carrying out fifth permanent magnet iron removal, screening, and finally carrying out electromagnetic iron removal to obtain the ternary precursor.
And (3) further, sampling and detecting steps are arranged after the second permanent magnet is deironized in the step (1), after the slurry liquid is prepared in the step (2), before and after screening in the step (3).
Further, the main raw materials required by the ternary liquid in the step (1) comprise nickel sulfate, cobalt sulfate and one of sodium metaaluminate and manganese sulfate.
Further, in the step (2), when the ternary liquid is a nickel-cobalt-aluminum ternary liquid, the washing process sequentially adopts a sodium hydroxide solution subjected to first permanent magnet iron removal treatment and a pure water solution for washing; when the ternary liquid is nickel-cobalt-manganese ternary liquid, the washing process adopts pure water solution subjected to first permanent magnet iron removal treatment for washing.
And further, recycling iron-removing slag generated by first permanent magnet iron removal, second permanent magnet iron removal, third permanent magnet iron removal, fifth permanent magnet iron removal and electromagnetic iron removal.
An apparatus employed by the above method, comprising: a raw material storage tank, an auxiliary solution storage tank, a ternary solution preparation tank, a reaction kettle, a filter press, a slurrying tank, a dryer and a screening machine; the discharge ports of the raw material storage tank and the auxiliary solution storage tank are connected with the feed port of the first permanent magnet iron remover; the feed inlets of the ternary liquid preparation tank, the reaction kettle, the filter press and the slurrying tank are connected with the discharge outlet of the first permanent magnet iron remover, and the ternary liquid preparation tank, the second permanent magnet iron remover, the reaction kettle, the filter press, the third permanent magnet iron remover, the slurrying tank, the fourth permanent magnet iron remover, the dryer and the sieving machine are sequentially connected.
Further, the equipment still includes fifth permanent magnetism de-ironing separator, electromagnetism de-ironing separator, the feed inlet of fifth permanent magnetism de-ironing separator is connected with the discharge gate of drying-machine, the discharge gate of fifth permanent magnetism de-ironing separator is connected with the feed inlet of screening machine, the discharge gate of screening machine is connected with the feed inlet of electromagnetism de-ironing separator.
Further, the first permanent magnet deironing device, the second permanent magnet deironing device, the third permanent magnet deironing device, the fourth permanent magnet deironing device and the fifth permanent magnet deironing device are drawer type permanent magnet deironing devices.
The invention has the beneficial technical effects that:
(1) In terms of process, the invention removes the magnetic foreign matters from the raw materials because the quality of the main raw materials and the auxiliary solution of the ternary metal is different and the magnetic foreign matters are contained in the preparation pre-stage, thereby greatly reducing the complexity of the process flow caused by overhigh content of the magnetic foreign matters in the preparation process of the ternary precursor, not only reducing the equipment cost input, but also improving the efficiency for screening the subsequent foreign matters.
(2) In the stage of preparing the ternary liquid, the ternary liquid prepared by the main raw material subjected to magnetic foreign matter removal according to the preparation requirement and the stage of precipitation-slurrying are subjected to permanent magnet iron removal again, so that the removal of the magnetic foreign matters in different processes in the stage of ternary precursor slurry is ensured, and the quality of the material is fully ensured; in addition, a sampling detection step is arranged before the next stage of process, and if data in the material is abnormal, the machine can be stopped immediately, so that the cross contamination of the material is effectively avoided.
(3) In the stage of 'dehydration-ternary precursor', a foreign matter screening device and magnetic foreign matter removing equipment, namely a fifth permanent magnet iron remover and an electromagnetic iron remover, are arranged in the stage, so that the problem of abnormal magnetic foreign matter data caused by the reason of the previous stage can be well solved, and the removal of foreign matters is fully ensured.
(4) The method has simple process, particularly ensures the full flow for removing the magnetic foreign matters, forms an independent and continuous full flow mode at each stage, can fully utilize the iron-removed slag at each stage through recovery of different processes, realizes resource circulation, and obtains the ternary precursor with higher quality.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a partial schematic flow diagram of the present invention.
FIG. 3 is a schematic diagram of the structure of the apparatus of the present invention.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
The invention provides a method for reducing a ternary precursor magnetic foreign matter, which can ensure normal operation of NCA (nickel cobalt aluminum) or NCM (nickel cobalt manganese) in a production dehydration-drying stage, can also produce an NCA or NCM ternary precursor material meeting the quality standard, and can also ensure that the problem of removing the magnetic foreign matter is solved in the stage and certain effective time is reserved; and finally, magnetic foreign matter is removed in each production stage of the production of the NCA or NCM ternary precursor material, an independent and continuous full-flow removing mode is adopted, a foreign matter removing device is arranged in each stage and is a permanent magnet iron remover or an electromagnetic iron remover, and the efficiency of removing the magnetic foreign matter is greatly improved. Therefore, the invention can not only improve the product quality, but also reduce the energy consumption.
As shown in fig. 1-2, a method for reducing a magnetic foreign substance in a ternary precursor comprises:
step 1: the ternary solution preparation tank is preposed with a unit raw material storage tank comprising nickel sulfate, cobalt sulfate and sodium metaaluminate or manganese sulfate, and the auxiliary solution comprises a pure water solution, an ammonia water solution and a sodium hydroxide solution. In the preparation stage of ternary solution: the nickel sulfate, cobalt sulfate, and sodium metaaluminate or manganese sulfate metal solutions are respectively subjected to first permanent magnet iron removal treatment, and similarly, each auxiliary solution is also respectively subjected to first permanent magnet iron removal treatment. The metal solution as the main raw material and the magnetic foreign matter in the auxiliary solution are treated. Then, according to the concentration of the metal solution and the preparation requirement, proportioning the main raw materials to prepare a ternary solution, carrying out second permanent magnet iron removal on the prepared ternary solution, recovering iron removal slag, and removing foreign matters in the stage called the ternary solution preparation stage, and then, allowing the ternary solution to enter the next stage;
step 2: conveying the prepared ternary liquid subjected to second permanent magnet iron removal treatment, and an ammonia water solution and a sodium hydroxide solution subjected to first permanent magnet iron removal treatment to a reaction kettle simultaneously for mixing to perform precipitation synthesis reaction, performing third permanent magnet iron removal treatment on a solid phase obtained after filter pressing and washing steps, and mixing the solid phase with a pure water solution subjected to first permanent magnet iron removal treatment to obtain a slurry solution, wherein when the ternary liquid is a nickel-cobalt-aluminum ternary liquid, the washing process sequentially adopts the sodium hydroxide solution subjected to first permanent magnet iron removal treatment and the pure water solution for washing; when the ternary liquid is nickel-cobalt-manganese ternary liquid, washing by using a pure water solution subjected to first permanent magnet iron removal treatment in the washing process; the obtained slurry is treated by a fourth permanent magnet deironing treatment, and the stage is called as the removal of magnetic foreign matters in the ternary liquid reaction-slurry stage;
and step 3: the slurry enters the dehydration, drying and screening processes, foreign matter screening at this stage comprises two parts, magnetic foreign matter is removed through fifth permanent magnet deironing, then other foreign matter is screened out by adopting a screening machine, and then electromagnetic deironing is carried out, namely a permanent magnet deironing device and an electromagnetic deironing device are arranged before and after screening, automatic valves are arranged before and after screening, and after the step, the whole process of foreign matter screening of the ternary material is finished;
and recovering all the deironing slag after deironing until secondary utilization.
Specifically, sampling points are arranged in the stages from the raw material preparation stage to the reaction-slurrying stage and before and after screening for sampling detection, so that the data change of the magnetic particle content in the material can be detected by feeding the sample in the whole stage in real time.
Specifically, permanent magnet iron removal and electromagnetic iron removal are set in the dehydration-screening stage as the preferred scheme, the material is sampled before and after screening to detect the content of magnetic foreign matters in the material, and the material is directly screened to obtain the ternary precursor if the material meets the quality requirement before screening.
As shown in fig. 3, an apparatus for reducing a ternary precursor magnetic foreign substance includes: a raw material storage tank 1, an auxiliary solution storage tank 2, a ternary solution preparation tank 3, a reaction kettle 4, a filter press 5, a slurrying tank 6, a dryer 7 and a sieving machine 8;
the raw material storage tank 1 comprises a solution unit tank for storing a main raw material (comprising nickel sulfate, cobalt sulfate and one of sodium metaaluminate and manganese sulfate) required for preparing a ternary solution; the auxiliary solution storage tank 2 comprises a unit tank for storing auxiliary solutions required by preparing the ternary solution, wherein the auxiliary solutions comprise pure water solution, ammonia water solution and sodium hydroxide solution; the discharge ports of the raw material storage tank and the auxiliary solution storage tank are connected with the feed port of the first permanent magnet iron remover 9;
the ternary liquid preparation tank 3 is used for preparing ternary liquid, the reaction kettle 4 is used for precipitation synthesis reaction of materials, the filter press 5 is used for filter pressing and washing the materials, the slurrying tank 6 is used for preparing the slurrying liquid, the dryer 7 is used for dehydrating and drying the materials, and the screening machine 8 is used for screening the materials and removing other foreign matters;
the three-component liquid preparation tank 3, the reaction kettle 4, the filter press 5 and the pulp tank 6 are connected with a discharge port of the first permanent magnet iron remover 9, a discharge port of the three-component liquid preparation tank 3 is connected with a feed port of the second permanent magnet iron remover 10, a discharge port of the second permanent magnet iron remover 10 is connected with a feed port of the reaction kettle 4, a discharge port of the reaction kettle 4 is connected with a feed port of the filter press 5, a discharge port of the filter press 5 is connected with a feed port of the third permanent magnet iron remover 11, a discharge port of the third permanent magnet iron remover 11 is connected with a feed port of the pulp tank 6, a discharge port of the pulp tank 6 is connected with a feed port of the fourth permanent magnet iron remover 12, a discharge port of the fourth permanent magnet iron remover 12 is connected with a feed port of the dryer 7, and a discharge port of the dryer 7 is connected with a feed port of the screening machine 8.
Further, the equipment further comprises a fifth permanent magnet iron remover 13 and an electromagnetic iron remover 14, wherein a feed inlet of the fifth permanent magnet iron remover 13 is connected with a discharge outlet of the dryer 7, a discharge outlet of the fifth permanent magnet iron remover 13 is connected with a feed inlet of the screening machine 8, and a discharge outlet of the screening machine 8 is connected with a feed inlet of the electromagnetic iron remover 14.
The first permanent magnet deironing device 9, the second permanent magnet deironing device 10, the third permanent magnet deironing device 11, the fourth permanent magnet deironing device 12 and the fifth permanent magnet deironing device 13 are drawer type permanent magnet deironing devices.
Example 1
A method for reducing magnetic foreign matters of a ternary (nickel cobalt aluminum) precursor comprises the following steps:
step (1), ternary solution preparation stage: the raw material storage tank 1 comprises unit raw material storage tanks of nickel sulfate, cobalt sulfate and sodium metaaluminate which are used as main raw materials, the auxiliary solution storage tank 2 comprises unit tanks for storing pure aqueous solution, ammonia aqueous solution and sodium hydroxide solution, and the main raw materials and the auxiliary solutions are respectively treated by a first permanent magnet iron remover 9. Then, according to the concentration and preparation requirements of the metal solution, nickel sulfate, cobalt sulfate and sodium metaaluminate are prepared into a nickel-cobalt-aluminum ternary solution with the concentration of 80g/L in a ternary solution preparation tank 3 according to the molar ratio of 80;
step (2), reaction-slurrying: and (3) simultaneously conveying the ternary solution to a reaction kettle 4 for precipitation synthesis reaction according to 300L/h of flow rate, 40L/h of sodium hydroxide solution (with the concentration of 20%) and 30L/h of ammonia water (with the concentration of 12%) which are treated by a first permanent magnet iron remover 9, wherein the reaction time is 120h. Then, a filter pressing step is carried out through a filter press 5, meanwhile, a sodium hydroxide solution (40 ℃) with the concentration of 2% and treated by a first permanent magnet iron remover is sequentially adopted for washing for 4 times, pure water at 40 ℃ is adopted for washing for 4 times, the obtained solid phase after washing is treated by a third permanent magnet iron remover 11 and then conveyed to a slurrying tank 6, the pure water solution treated by the first permanent magnet iron removal is introduced for dilution, a semi-finished product slurrying solution for washing nickel cobalt aluminum is obtained, the obtained slurrying solution is treated by a fourth permanent magnet iron remover 12, and iron removal slag is recovered;
step (3), dehydration-precursor: and (3) the qualified pulp liquid after detection enters a dryer 7 to be dehydrated and dried, then other foreign matters are screened out by a screening machine 8, and the screened product is subjected to foreign matter detection to reach the product standard, so that the nickel-cobalt-aluminum ternary precursor material is obtained.
Example 2
A method for reducing magnetic foreign matters in a ternary (nickel-cobalt-manganese) precursor comprises the following steps:
step (1), preparing a ternary solution: the raw material storage tank 1 comprises unit raw material storage tanks of nickel sulfate, cobalt sulfate and manganese sulfate as main raw materials, the auxiliary solution storage tank 2 comprises unit tanks for storing pure aqueous solution, ammonia aqueous solution and sodium hydroxide solution, and the main raw materials and the auxiliary solutions are respectively treated by a first permanent magnet iron remover 9. Then, according to the concentration and preparation requirements of the metal solution, nickel sulfate, cobalt sulfate and manganese sulfate are prepared into a nickel-cobalt-manganese ternary solution in a ternary solution preparation tank 3 according to the molar ratio of 1;
step (2), reaction-slurrying: and (3) mixing the prepared ternary solution, a sodium hydroxide solution with the concentration of 4mol/L and an ammonia water solution with the concentration of 6mol/L (treated by a first permanent magnet iron remover 9) according to the ratio of 2:2:1, and simultaneously conveying the mixture to a reaction kettle 4 for precipitation synthesis reaction, and reacting for 15 hours at the temperature of 80 ℃. Then, performing filter pressing by a filter press 5, washing for 4 times by pure water treated by a first permanent magnet iron remover, treating a solid phase obtained after washing by a third permanent magnet iron remover 11, conveying to a slurry tank 6, introducing pure water solution treated by the first permanent magnet iron remover for dilution to obtain a nickel-cobalt-manganese washing semi-finished product slurry solution, treating the obtained slurry solution by a fourth permanent magnet iron remover 12, and recovering iron-removed slag;
step (3), dehydration-precursor: and (3) the qualified pulp liquid after detection enters a dryer 7 to be dehydrated and dried, then other foreign matters are screened out by a screening machine 8, and the screened product is subjected to foreign matter detection to reach the product standard, so that the nickel-cobalt-manganese ternary precursor material is obtained.
Example 3
A method for reducing a ternary (nickel cobalt aluminum) precursor magnetic foreign matter comprises the following steps:
step (1), preparing a ternary solution: the raw material storage tank 1 comprises unit raw material storage tanks of nickel sulfate, cobalt sulfate and sodium metaaluminate which are used as main raw materials, the auxiliary solution storage tank 2 comprises unit tanks for storing pure aqueous solution, ammonia aqueous solution and sodium hydroxide solution, and the main raw materials and the auxiliary solutions are respectively treated by a first permanent magnet iron remover 9. Then, nickel sulfate, cobalt sulfate and sodium metaaluminate are prepared into a nickel-cobalt-aluminum mixed ternary solution with the concentration of 120g/L in a ternary solution preparation tank 3 according to the molar ratio of 90;
step (2), reaction-slurrying: and (3) simultaneously conveying the ternary solution to a reaction kettle 4 for precipitation synthesis reaction according to 550L/h of flow rate, 120L/h of sodium hydroxide solution (with the concentration of 40%) and 60L/h of ammonia water (with the concentration of 22%) (treated by a first permanent magnet iron remover 9), wherein the reaction time is 50h. Then, performing a filter pressing step through a filter press 5, washing for 1 time by sequentially adopting a sodium hydroxide solution (80 ℃) with the concentration of 5% and treated by a first permanent magnet iron remover, washing for 1 time by pure water at 80 ℃, conveying a solid phase obtained after washing to a slurrying tank 6 after being treated by a third permanent magnet iron remover 11, introducing the pure water solution treated by the first permanent magnet iron remover for dilution to obtain a nickel-cobalt-aluminum washing semi-finished slurrying solution, treating the obtained slurrying solution by a fourth permanent magnet iron remover 12, and recovering iron-removed slag;
step (3), dehydration-precursor: and (3) the slurry enters a dryer 7 for dehydration and drying, magnetic foreign matters are removed through a fifth permanent magnet iron remover 13, other foreign matters are screened out through a screening machine 8, and finally, after electromagnetic iron removal through an electromagnetic iron remover 14, the product standard is reached through detection, so that the nickel-cobalt-aluminum ternary precursor material is obtained.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.

Claims (9)

1. A method of reducing a ternary precursor magnetic foreign material, the method comprising:
(1) Preparing a ternary liquid: respectively carrying out first permanent magnet iron removal on a main raw material and an auxiliary solution required by the ternary liquid, preparing the main raw material into the ternary liquid according to the preparation requirement, and then carrying out second permanent magnet iron removal; the auxiliary solution comprises a pure water solution, an ammonia water solution and a sodium hydroxide solution;
(2) Reaction-slurrying: mixing the ternary solution obtained in the step (1) with an ammonia water solution and a sodium hydroxide solution which are subjected to first permanent magnet iron removal treatment, carrying out precipitation reaction, filter pressing and washing to obtain a solid phase, carrying out third permanent magnet iron removal on the solid phase, mixing the solid phase with a pure water solution which is subjected to first permanent magnet iron removal treatment to obtain a slurry solution, and carrying out fourth permanent magnet iron removal on the slurry solution;
(3) Dehydration-precursor: and (3) dehydrating and drying the slurry obtained in the step (2), and then screening to obtain a ternary precursor.
2. The method according to claim 1, wherein in the step (3), the slurry is dehydrated and dried after being subjected to fourth permanent magnet iron removal, then is screened after being subjected to fifth permanent magnet iron removal, and finally is subjected to electromagnetic iron removal to obtain the ternary precursor.
3. The method of claim 1, wherein sampling and detecting steps are provided after the second permanent magnet is removed from iron in the step (1), after the slurry is prepared in the step (2), before the screening in the step (3) and after the screening.
4. The method as claimed in claim 1, wherein the main raw materials required for the ternary liquid in step (1) comprise nickel sulfate, cobalt sulfate and one of sodium metaaluminate and manganese sulfate.
5. The method according to claim 1, wherein in the step (2), when the ternary liquid is nickel-cobalt-aluminum ternary liquid, the washing process is sequentially washing with a sodium hydroxide solution subjected to first permanent magnet iron removal treatment and a pure water solution; when the ternary liquid is nickel-cobalt-manganese ternary liquid, the washing process adopts pure water solution subjected to first permanent magnet iron removal treatment for washing.
6. The method of claim 1, wherein the iron-removed slag generated by the first permanent magnet iron removal, the second permanent magnet iron removal, the third permanent magnet iron removal, the fifth permanent magnet iron removal and the electromagnetic iron removal is recycled.
7. An apparatus for use in the method of any one of claims 1 to 6, wherein the apparatus comprises: a raw material storage tank, an auxiliary solution storage tank, a ternary solution preparation tank, a reaction kettle, a filter press, a slurrying tank, a dryer and a screening machine; the discharge ports of the raw material storage tank and the auxiliary solution storage tank are connected with the feed port of the first permanent magnet iron remover; the feed inlets of the ternary liquid preparation tank, the reaction kettle, the filter press and the pulping tank are all connected with the discharge outlet of the first permanent magnet iron remover, and the ternary liquid preparation tank, the second permanent magnet iron remover, the reaction kettle, the filter press, the third permanent magnet iron remover, the pulping tank, the fourth permanent magnet iron remover, the dryer and the screening machine are sequentially connected.
8. The equipment of claim 7, further comprising a fifth permanent magnet iron remover and an electromagnetic iron remover, wherein a feeding port of the fifth permanent magnet iron remover is connected with a discharging port of the dryer, a discharging port of the fifth permanent magnet iron remover is connected with a feeding port of the sieving machine, and a discharging port of the sieving machine is connected with a feeding port of the electromagnetic iron remover.
9. The apparatus of claim 7, wherein the first, second, third, fourth, and fifth permanent magnet deironing devices are drawer permanent magnet deironing devices.
CN202211206740.1A 2022-09-30 2022-09-30 Method and equipment for reducing magnetic foreign matters of ternary precursor Pending CN115432747A (en)

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