CN114162800A - Production method of lithium ion battery anode material - Google Patents
Production method of lithium ion battery anode material Download PDFInfo
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- CN114162800A CN114162800A CN202111349541.1A CN202111349541A CN114162800A CN 114162800 A CN114162800 A CN 114162800A CN 202111349541 A CN202111349541 A CN 202111349541A CN 114162800 A CN114162800 A CN 114162800A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- 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
Abstract
The invention discloses a method for producing a lithium ion battery anode material, which comprises the following steps: s1: lithium salt burdening; s2: mixing and dispersing lithium salt and pure water to obtain a lithium salt mixture; s3: respectively burdening phosphoric acid and iron powder, and reacting the burdened phosphoric acid and the iron powder with each other to prepare a ferro-phosphorus compound; s4: adding a mixture of hydrogen peroxide, pure water and lithium salt into the ferrophosphorus compound, and mixing and grinding to obtain mixed slurry; s5: c, carbon source proportioning; s6: the finished product slurry prepared by the invention has smaller fineness, can obtain a nano-grade slurry product, can effectively improve or increase the stacking density of the anode material lithium iron phosphate, enables the monomer particles to reach the quality requirement of 0.3-0.5 micron, greatly improves the quality and the carbon coating property, can achieve the production purposes of energy conservation and emission reduction, is beneficial to the conversion to energy conservation and emission reduction and low-carbon production modes, and has lower cost.
Description
Technical Field
The invention relates to an electrode, in particular to a method for producing a lithium ion battery anode material.
Background
The traditional anode material preparation process adopts finished products of lithium source compounds, iron source compounds, ferrophosphorus compounds, carbon sources and other additives to be mixed and ground according to a certain proportion to prepare the anode material, and the particle size of the ground mixed slurry is multimodal and linear due to different characteristics of various compounds in the mixing and grinding process, so that the battery capacity density is low, the endurance mileage is low, the slurry is flammable and explosive, and the like, namely the particle size of the mixed and ground slurry is uneven, and the quality of the battery product is difficult to improve.
Disclosure of Invention
The invention aims to provide a method for producing a lithium ion battery cathode material, which aims to solve one or more technical problems in the prior art and at least provide a beneficial choice or creation condition.
The solution of the invention for solving the technical problem is as follows:
a method for producing a lithium ion battery anode material comprises the following steps: s1: lithium salt burdening; s2: mixing and dispersing lithium salt and pure water to obtain a lithium salt mixture; s3: respectively burdening phosphoric acid and iron powder, and reacting the burdened phosphoric acid and the iron powder with each other to prepare a ferro-phosphorus compound; s4: adding a mixture of hydrogen peroxide, pure water and lithium salt into the ferrophosphorus compound, and mixing and grinding to obtain mixed slurry; s5: c, carbon source proportioning; s6: and adding a carbon source into the mixed slurry, and mixing and grinding to obtain the finished slurry.
The technical scheme at least has the following beneficial effects: the lithium salt is directly selected to prepare the lithium salt mixture, the ferrophosphorus compound is prepared by the mutual reaction of phosphoric acid and iron powder, the production cost is lower, the prepared ferrophosphorus compound is slurry, an iron source compound and the ferrophosphorus compound do not need to be ground, dried and crushed, the lithium salt mixture can be directly added into the ferrophosphorus compound, the production efficiency is improved, the fineness of the finished product slurry prepared by adding a carbon source is smaller, a nanoscale slurry product can be obtained, the stacking density of the anode material lithium iron phosphate can be effectively improved, the monomer particles of the anode material lithium iron phosphate can reach the quality requirement of 0.3-0.5 micrometer, the quality and the carbon coating property are greatly improved, the production purpose of energy conservation and emission reduction can be achieved, and the conversion to the production modes of energy conservation, emission reduction and low carbon is facilitated.
As a further improvement of the above technical solution, the lithium salt mixture obtained in S2 is ground for multiple times by a sand mill to obtain a coarse grinding material, and then the coarse grinding material is ground for multiple times by the sand mill to obtain a fine grinding material, wherein the lithium salt mixture added in S4 is the fine grinding material. The lithium salt mixture is subjected to rough grinding firstly and then is subjected to fine grinding, the grinding quality of the lithium salt mixture can be improved, the lithium salt mixture added in S4 is a fine grinding material after grinding, the particle size of the initial mixture can be closer, the problem of poor grinding effect caused by large particle size difference is avoided, and the grinding efficiency and quality are improved.
As a further improvement of the above technical solution, in S2, the coarse grinding materials are conveyed into grinding tanks, the coarse grinding materials are transferred in at least two grinding tanks, and the coarse grinding materials are ground once by a sand grinder every time the coarse grinding materials are transferred until the fine grinding requirements are met, so as to obtain the fine grinding materials. When the coarse grinding materials are all transferred from one grinding tank to another grinding tank, the coarse grinding materials are ground once through the sand mill, so that the particle size distribution of the slurry can be ensured, and the grinding efficiency is improved.
As a further improvement of the technical scheme, the particle size of the coarse grinding material is 0.7-1.5 microns. During coarse grinding, the lithium salt mixture is ground to the value within the particle size range, so that the grinding time of the fine grinding material can be better matched, and the whole grinding efficiency is improved.
As a further improvement of the technical scheme, the grain diameter of the fine grinding material is 300-500 nanometers. After fine grinding, the lithium salt mixture is ground to the value within the particle size range, so that the degree of similarity of the particle size of the material in the next working procedure is better improved, and the grinding efficiency is improved.
As a further improvement of the technical scheme, in the step S3, a stirring mill or a sand mill is started, phosphoric acid is automatically metered and added through a flow meter to the stirring mill or the sand mill by a set required amount, and the addition amount error is 0.015% -0.01%; and starting a heating function of the stirring mill or the sand mill, heating phosphoric acid at the temperature of 80-95 ℃, adding iron powder to react to generate iron phosphate, wherein the content of phosphoric acid is 60-70%, the content of iron powder is 30-40%, and the reaction time is 4-6 h, starting a self-circulating pump connected with the stirring mill or the sand mill to perform slurry self-circulation after the set reaction time is reached, and obtaining the ferrophosphorus compound after the reaction is finished. Thus, the slurry ferrophosphorus compound can be directly prepared by phosphoric acid and iron powder, and the obtained slurry has finer fineness.
As a further improvement of the technical proposal, a plurality of ceramic grinding media with different diameters are added into the stirring mill. Under the impact, shearing and friction of the ceramic grinding medium, the reaction of iron and phosphoric acid is sufficient and faster, and the fineness of the slurry obtained by the reaction is finer.
In the S4, the addition amount of hydrogen peroxide is 0.6-1.5%, the addition amount of pure water is 50-55%, and the addition amount of the lithium salt mixture is 4-13.5%. The mixed slurry with excellent quality can be obtained by mixing and grinding under the mixture ratio.
As a further improvement of the above technical solution, in S1, the lithium salt is sieved and then fed into the raw material bin for temporary storage, the raw material bin is controlled to drop to the material amount in the metering bin for batching, positive pressure pneumatic conveying is adopted when the lithium salt is fed into the raw material bin, and the conveying gas source is dry compressed air or nitrogen. After screening the lithium salt, put into former feed bin earlier, control the weight that falls to the measurement storehouse in according to the use amount to the realization is to the batching of lithium salt, and is adopting malleation air conveying in the transfer to the lithium salt, and the conveying gas source is dry compressed air or nitrogen gas, avoids solid raw materials to wet and leads to the pipeline to block up.
As a further improvement of the above technical solution, the present invention further includes S7: and pumping the finished slurry into an electromagnetic iron remover through a feeding pump, then feeding the finished slurry into a finished product tank or a middle transfer slurry tank, and drying. And conveying the finished slurry to a finished tank for temporary storage, drying, and carrying out a thermosetting phase reaction after drying more thoroughly, so that the tap density of the prepared anode material is obviously improved.
Detailed Description
The conception, the specific structure, and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below, so that the objects, the features, and the effects of the present invention can be fully understood. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention. In addition, all the connection relations mentioned herein do not mean that the components are directly connected, but mean that a better connection structure can be formed by adding or reducing connection accessories according to the specific implementation situation. All technical characteristics in the invention can be interactively combined on the premise of not conflicting with each other.
A method for producing a lithium ion battery anode material comprises the following steps: s1: lithium salt burdening; s2: mixing and dispersing lithium salt and pure water to obtain a lithium salt mixture; s3: respectively burdening phosphoric acid and iron powder, and reacting the burdened phosphoric acid and the iron powder with each other to prepare a ferro-phosphorus compound; s4: adding a mixture of hydrogen peroxide, pure water and lithium salt into the ferrophosphorus compound, and mixing and grinding to obtain mixed slurry; s5: c, carbon source proportioning; s6: and adding a carbon source into the mixed slurry, and mixing and grinding to obtain the finished slurry.
According to the method, the lithium salt is directly selected to prepare the lithium salt mixture, the ferrophosphorus compound is prepared by the mutual reaction of phosphoric acid and iron powder, the production cost is lower, the prepared ferrophosphorus compound is slurry, the iron source compound and the ferrophosphorus compound do not need to be ground, dried and crushed, the lithium salt mixture can be directly added into the ferrophosphorus compound, the production efficiency is improved, the fineness of the finished slurry prepared by adding the carbon source is smaller, the nanoscale slurry product can be obtained, the stacking density of the anode material lithium iron phosphate can be effectively improved, the monomer particles can reach the quality requirement of 0.3-0.5 micrometer, the quality and the carbon coating property are greatly improved, the production purpose of energy conservation and emission reduction can be achieved, and the conversion to the production modes of energy conservation, emission reduction and low carbon is facilitated.
In S1, lithium salt solid powder is fed through a feeding station, the powder is fed to a crusher through a rotary valve to control feeding amount to be coarsely crushed, if the powder does not need coarse crushing, the powder is screened through a screening machine, screened powder enters a transfer bin, a material level switch or a weight sensor is arranged on the transfer bin to control automatic start and stop of a comprehensive process, the material in the transfer bin falls to a pressure feed tank to convey the powder to a raw material bin for temporary storage, the raw material bin is provided with the weight sensor to control the feeding amount through the rotary valve through weight loss measurement, the material amount of equipment automatically falls to a metering bin, the metering bin is provided with the weight sensor and a precision feeder, and the weight sensor controls the set feeding weight to carry out proportioning on the powder. The process adopts a DCS control system and a formula management system to realize full-automatic powder conveying and metering proportioning, and realizes high-precision batching through repeated weight rechecking and checking of a raw material bin and a metering bin. The lithium salt solid raw material is conveyed by adopting positive pressure pneumatic conveying, and a conveying gas source is dry compressed air or nitrogen so as to avoid the blockage of a conveying pipeline caused by the wetting of the solid raw material; the automatic batching and controlling device is composed of a bearing sensor, an accurate feeder and a formula control system, so that automatic batching and automatic control are realized.
In the S2, a weight sensor is arranged in a premixing tank, pure water is metered by a flowmeter and passes through the weight sensor of the premixing tank to be approved for the addition of the pure water, the pure water is automatically added into the premixing tank according to the set addition, a homogenizing pump is automatically started, the homogenizing pump and the premixing tank are subjected to self-circulation slurry dispersion, powder in a metering bin above the premixing tank automatically falls into the premixing tank to be subjected to solid-liquid mixing dispersion, and the solid content of the solid-liquid ratio in the process is WT 20% -26%, so that a lithium salt mixture is obtained; monitoring the temperature of the slurry in real time through a temperature sensor configured in a premixing tank, monitoring the pH value of the slurry in real time through a pH value sensor and reaching the set premixing time, automatically monitoring that a discharge valve of the premixing tank is opened after premixing is finished, feeding the lithium salt mixture into a filter, a heat exchanger and an iron remover, then feeding the lithium salt mixture into a sand mill for grinding, and feeding the outlet of the sand mill into a rough grinding tank through a pipeline; the premixing tank is provided with a low-speed stirrer, and the anchor type stirring paddle is used for stirring the slurry, so that the slurry is prevented from precipitating; the solid-liquid mixing efficiency is accelerated by adopting a double high-speed dispersion machine and a homogenizing pump, so that the solid is fully wetted and uniformly dispersed into the liquid; a chilled water jacket cavity is arranged outside the premixing tank, and a spiral chilled water circulation pipeline is arranged inside the premixing tank, so that the temperature of the slurry is reduced, the molecular activity of the slurry is reduced, and the agglomeration of fine particles of the slurry is avoided; the drive motor adopted by the premixing tank is a permanent magnet motor, and is directly connected with the stirring shaft or the dispersing shaft for driving or is connected with the speed reducer for driving, so that the energy-saving effect is realized.
And after the slurry in the premixing tank is discharged, automatically closing a discharge valve of the premixing tank, and repeating the steps S1 and S2 to realize continuous production.
And grinding the lithium salt mixture obtained in the step S2 for multiple times by using a sand mill to obtain a coarse grinding material, and grinding the coarse grinding material for multiple times by using the sand mill to obtain a fine grinding material, wherein the lithium salt mixture added in the step S4 is the fine grinding material.
Lithium salt mixture in the coarse grinding tank continues to enter a sand mill through a filter, a heat exchanger and an iron remover to be ground and returned to the coarse grinding tank, the lithium salt mixture is circularly ground, the lithium salt mixture is subjected to grinding by setting grinding time, online granularity detection, slurry temperature monitoring and PH value monitoring of the coarse grinding tank, when the automatic detection grinding time reaches the setting time and the granularity detection is qualified, coarse grinding materials are obtained, and the coarse grinding materials in the coarse grinding tank enter a grinding tank A through the filter and a material transferring pump. The coarse grinding process requires that the particle size of the slurry after coarse grinding is 0.7-1.5 microns.
The coarse grinding materials in the grinding tank A enter a fine grinding sand mill for grinding through a filter, a heat exchanger and an iron remover, the outlet of the sand mill is connected with a grinding tank B, the grinding tank C is used as a temporary storage tank for the coarse ground slurry, a system automatically detects which empty grinding tank A/B/C is used as the temporary storage tank for the coarse ground slurry, when the slurry in the grinding tank A is completely discharged to the grinding tank B, a discharge valve of the grinding tank A is closed, a discharge valve of the grinding tank B is opened, the slurry in the grinding tank B is ground back to the grinding tank A through the filter, the heat exchanger, the iron remover and the sand mill, and the slurry is ground back and forth for several times according to the procedures; through PH value detection, viscosity detection and online particle size detection of the outlet of the sand mill, after the detection is qualified, slurry in the grinding tank enters the stirring tank through the filter and the material transferring pump. At this point the grind A/B tank will be ground in grind C tank by the process described above. The grain diameter of the slurry after grinding in the working procedure is 300-500 nanometers, and the fine grinding material is obtained. 3 grinding jars ABC are adopted in the process of the section to participate in grinding, the grinding process is that any two jars are used as grinding jars to be inverted, switched and ground, the other jar is used as a temporary storage jar for coarse grinding slurry, the control system ensures the production continuity, and the double-jar inverted grinding enables the slurry to be ground completely through a sand mill, so that the particle size distribution of the slurry is ensured. The sand mill adopts a dual-drive dynamic separation type sand mill MORPH KDP, and the materials of parts inside the grinding cavity are zirconia ceramics, silicon carbide ceramics, silicon nitride ceramics, high polymer materials, polyurethane rubber and other non-metal materials, so that the introduction of metal magnetic pollutants in the grinding process is avoided; the separation device of the sand mill is in a dynamic screen-free separation mode, and the viscosity of the lithium salt compound is increased in the process of fineness reduction, so that discharge blockage can be avoided by using the dynamic screen-free horizontal or vertical sand mill; the dynamic separation sand mill without the screen can use a grinding medium of 0.03 mm-1 mm, and can obtain slurry with fine fineness and more uniform slurry. In the process, parameter data of the slurry, such as pH value, fineness, viscosity, temperature, flow, efficiency, pressure and the like, which influence the energy density of the anode material can be automatically detected by combining a plurality of sensors. The lithium salt mixture is subjected to rough grinding firstly and then is subjected to fine grinding, the grinding quality of the lithium salt mixture can be improved, the lithium salt mixture added in S4 is a fine grinding material after grinding, the particle size of the initial mixture can be closer, the problem of poor grinding effect caused by large particle size difference is avoided, and the grinding efficiency and quality are improved.
In the S3, a ferrous iron or ferric iron powder general storage bin and a rotary valve control the blanking speed to enter a screening machine, screened powder enters a transfer bin, a material level switch or a weight sensor is arranged on the transfer bin to control the automatic start and stop of the overall process, the material in the transfer bin falls into a pressure feed tank or other pneumatic conveying modes to convey the powder to a raw material bin for temporary storage, the raw material bin is provided with the weight sensor to control the blanking amount through the rotary valve through weight loss measurement, the material amount of the equipment automatically falls into a metering bin, the metering bin is provided with the weight sensor and a precision feeder, and the precise feeder is controlled to set the blanking weight through the weight sensor by adopting a vector metering method to carry out the proportioning of the powder. The process adopts a DCS control system and a formula management system to realize full-automatic powder conveying and metering proportioning, and realizes high-precision batching through repeated weight rechecking and checking of a raw material bin and a metering bin.
Starting the stirring mill, and automatically metering and adding phosphoric acid into the stirring mill by a flow meter according to the set required amount, wherein the addition error is 0.015-0.01%; and starting a heating function of the stirring mill, and heating phosphoric acid at the heating temperature of 80-95 ℃. Adding iron powder to react to generate iron phosphate, wherein the content of phosphoric acid is 60-70%, the content of iron powder is 30-40%, the reaction time is 4-6 h, starting a stirring mill self-circulation pump to perform slurry self-circulation after the set reaction time is reached, detecting the pH value through a pH sensor to obtain a ferrophosphorus compound, adding a strong oxidant hydrogen peroxide through a flow meter after the reaction is completed, adding 0.6-1.5% of hydrogen peroxide, adding 50-55% of pure water, adding a precursor slurry of a lithium salt mixture, adding 4-13.5% of the lithium salt mixture, starting a stirring mill self-circulation iron remover valve, performing iron removal treatment on the stirring mill, continuously and circularly grinding the stirring mill, after the grinding time is reached, feeding the stirring mill slurry into a fine grinding tank A through a filter, and finishing the step S4.
Thus, the liquid iron phosphate compound is directly prepared, and a lithium source and a carbon source can be directly added to directly prepare the anode material without independently preparing powder; iron and phosphoric acid were used as reaction vessels using a stirred mill apparatus. Ceramic grinding media need to be added into the stirring and grinding cylinder, under the impact, shearing and friction of the grinding media, iron and phosphoric acid react sufficiently and quickly, and the fineness of slurry obtained through reaction is finer; the materials of the parts of the stirring mill participating in grinding are zirconia ceramics, alumina ceramics, silicon carbide ceramics, titanium alloy and the like, and the stirring mill has stronger corrosion resistance and better heat transfer performance; the stirring mill belt is provided with a heating jacket and a cooling jacket, and the heating jacket and the cooling jacket are in a spiral semi-coil form.
In step S5, the carbon source is glucose or fructose powder, the powder is fed through a feeding station, the powder is fed to a screening machine for screening by a rotary valve to control the feeding amount, the screened powder enters a transfer bin, a level switch or a weight sensor is arranged on the transfer bin to control the automatic start and stop of the overall process, the material in the transfer bin falls into a pressure feed tank or other pneumatic conveying modes to convey the powder to a raw material bin for temporary storage, the raw material bin is provided with a weight sensor to control the feeding amount by the rotary valve through weight loss measurement, the material amount of the equipment automatically falls into a metering bin, the metering bin is provided with a weight sensor and a precision feeder, and the weight sensor controls the set feeding weight to the precision feeder to match the powder by a vector metering method. The process adopts a DCS control system and a formula management system to realize full-automatic powder conveying and metering proportioning, and realizes high-precision batching through repeated weight rechecking and checking of a raw material bin and a metering bin.
In step S6, the four-material mixed grinding fine grinding tank a/B/C and the sand mill form a double-tank grinding process, wherein when 2 tanks are used for grinding, the other tank is used as a temporary storage tank for the slurry stirring and grinding, the system automatically identifies 2 arbitrary grinding tanks and 1 temporary storage tank, and the temporary storage tank is used as the temporary storage of the slurry stirring and grinding. After the stirring and grinding slurry is added into the fine grinding tank A or B, adding a carbon source through the working procedure 9, starting a grinding tank stirrer for stirring, adding pure water after the pH value of the fine grinding tank is detected, and metering the required amount of the added pure water through a flowmeter and a weight sensor of the fine grinding tank by the pure water; the slurry of the fine grinding tank A/B enters a filter, a heat exchanger, an iron remover and a sand mill to be ground and then enters a fine grinding tank C, when the slurry of the fine grinding tank A is completely ground and enters the fine grinding tank C, a discharge valve of the fine grinding tank A is automatically closed, a discharge valve of the fine grinding tank C is automatically opened, the slurry of the fine grinding tank C enters the fine grinding tank A after being ground by the filter, the heat exchanger, the iron remover and the sand mill, repeated tank-reversing grinding is carried out on the two tanks, and after the set time is reached and the online granularity detection of the outlet of the sand mill is qualified, the slurry enters a finished product tank A or B or C through the filter and a material transferring pump. The particle size of the slurry after grinding in the procedure is 250-450 nm, and the finished slurry is obtained.
In order to obtain uniform thin-layer carbon coating in S6, nano-scale slurry products are obtained through mixed grinding of slurry.
The present invention further comprises S7: and pumping the slurry into the electromagnetic iron remover or the permanent magnet iron remover through a feed pump, returning the slurry to the finished product tank A or B or C, circularly removing iron for a plurality of times or for a period of time, temporarily storing the slurry, and waiting for the next drying procedure to prepare the lithium ion battery anode material. And conveying the finished slurry to a finished tank for temporary storage, drying, and carrying out a thermosetting phase reaction after drying more thoroughly, so that the tap density of the prepared anode material is obviously improved. While the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that the present invention is not limited to the details of the embodiments shown and described, but is capable of numerous equivalents and substitutions without departing from the spirit of the invention as set forth in the claims appended hereto.
Claims (10)
1. A method for producing a lithium ion battery anode material is characterized by comprising the following steps: the method comprises the following steps:
s1: lithium salt burdening;
s2: mixing and dispersing lithium salt and pure water to obtain a lithium salt mixture;
s3: respectively burdening phosphoric acid and iron powder, and reacting the burdened phosphoric acid and the iron powder with each other to prepare a ferro-phosphorus compound;
s4: adding a mixture of hydrogen peroxide, pure water and lithium salt into the ferrophosphorus compound, and mixing and grinding to obtain mixed slurry;
s5: c, carbon source proportioning;
s6: and adding a carbon source into the mixed slurry, and mixing and grinding to obtain the finished slurry.
2. The method for producing the positive electrode material of the lithium ion battery according to claim 1, wherein: and grinding the lithium salt mixture obtained in the step S2 for multiple times by using a sand mill to obtain a coarse grinding material, and grinding the coarse grinding material for multiple times by using the sand mill to obtain a fine grinding material, wherein the lithium salt mixture added in the step S4 is the fine grinding material.
3. The method for producing the positive electrode material of the lithium ion battery according to claim 2, wherein: and S2, conveying the coarse grinding materials into grinding tanks, transferring the coarse grinding materials in at least two grinding tanks, and grinding the coarse grinding materials once through a sand mill every time of transferring until the fine grinding requirements are met to obtain the fine grinding materials.
4. The method for producing the positive electrode material of the lithium ion battery according to claim 2, wherein: the grain size of the coarse grinding material is 0.7-1.5 microns.
5. The method for producing the positive electrode material of the lithium ion battery according to claim 2, wherein: the grain size of the fine abrasive is 300-500 nanometers.
6. The method for producing the positive electrode material of the lithium ion battery according to claim 1, wherein: in the step S3, starting a stirring mill or a sand mill, automatically metering and adding phosphoric acid into the stirring mill or the sand mill by a flow meter according to the set required amount, wherein the addition amount error is 0.015-0.01%; and starting a heating function of the stirring mill or the sand mill, heating phosphoric acid at the temperature of 80-95 ℃, adding iron powder to react to generate iron phosphate, wherein the content of phosphoric acid is 60-70%, the content of iron powder is 30-40%, and the reaction time is 4-6 h, starting a self-circulating pump connected with the stirring mill or the sand mill to perform slurry self-circulation after the set reaction time is reached, and obtaining the ferrophosphorus compound after the reaction is finished.
7. The method for producing the positive electrode material of the lithium ion battery according to claim 6, wherein: a plurality of ceramic grinding media with different diameters are added into the stirring mill.
8. The method for producing the positive electrode material of the lithium ion battery according to claim 1, wherein: in the S4, the addition amount of hydrogen peroxide is 0.6-1.5%, the addition amount of pure water is 50-55%, and the addition amount of the lithium salt mixture is 4-13.5%.
9. The method for producing the positive electrode material of the lithium ion battery according to claim 1, wherein: in S1, the lithium salt is sieved and then fed into the raw material bin for temporary storage, the raw material bin is controlled to fall to the material amount in the metering bin for proportioning, the lithium salt is fed into the raw material bin and then conveyed by positive pressure pneumatic conveying, and the conveying gas source is dry compressed air or nitrogen.
10. The method for producing the positive electrode material of the lithium ion battery according to claim 1, wherein: further comprising S7: and pumping the finished slurry into an electromagnetic iron remover through a feeding pump, then feeding the finished slurry into a finished product tank or a middle transfer slurry tank, and drying.
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