WO2023036308A1 - 一种新型绿色磷酸铁锂前驱体及其制备方法、应用 - Google Patents

一种新型绿色磷酸铁锂前驱体及其制备方法、应用 Download PDF

Info

Publication number
WO2023036308A1
WO2023036308A1 PCT/CN2022/118186 CN2022118186W WO2023036308A1 WO 2023036308 A1 WO2023036308 A1 WO 2023036308A1 CN 2022118186 W CN2022118186 W CN 2022118186W WO 2023036308 A1 WO2023036308 A1 WO 2023036308A1
Authority
WO
WIPO (PCT)
Prior art keywords
lithium
iron phosphate
product
preparation
phosphoric acid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2022/118186
Other languages
English (en)
French (fr)
Chinese (zh)
Inventor
于晓琳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Liangfu New Energy Technology Co Ltd
Original Assignee
Shanghai Liangfu New Energy Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Liangfu New Energy Technology Co Ltd filed Critical Shanghai Liangfu New Energy Technology Co Ltd
Priority to AU2022342227A priority Critical patent/AU2022342227B2/en
Priority to KR1020247011610A priority patent/KR102843962B1/ko
Priority to CA3231076A priority patent/CA3231076A1/en
Priority to EP22866769.7A priority patent/EP4400475A4/en
Priority to JP2024515845A priority patent/JP7728047B2/ja
Priority to US18/688,381 priority patent/US12209017B2/en
Priority to MX2024003002A priority patent/MX2024003002A/es
Publication of WO2023036308A1 publication Critical patent/WO2023036308A1/zh
Anticipated expiration legal-status Critical
Priority to ZA2024/02648A priority patent/ZA202402648B/en
Ceased legal-status Critical Current

Links

Images

Classifications

    • 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
    • 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
    • C01B25/37—Phosphates of heavy metals
    • C01B25/375—Phosphates of heavy metals of iron
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • 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
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • 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
    • 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

Definitions

  • the invention provides a novel green lithium iron phosphate precursor and its preparation method and application.
  • Lithium iron phosphate also known as lithium iron phosphate
  • LiFePO 4 material has a stable structure, abundant raw material sources, environmental friendliness and low cost.
  • a theoretical capacity of 170mAh/g a stable discharge platform of 3.5V and many other advantages, especially its safety performance and cycle life are unmatched by other materials, making lithium iron phosphate the most attractive cathode material today.
  • the synthesis methods of LiFePO 4 mainly focus on the synthesis process using iron phosphate as raw material.
  • the synthesis method using iron phosphate as raw material is generally to react iron phosphate with lithium source and carbon source, which has the problems of low solid content (generally 35%-40%) of the obtained product and high cost of subsequent processes.
  • iron powder can also be used as raw material to synthesize LiFePO 4 through the reaction of iron powder, phosphoric acid, lithium source and carbon source.
  • WO2004036671A1 describes the reaction of metallic iron and phosphoric acid in an aqueous solution, adding lithium carbonate or lithium hydroxide to prepare a lithium iron phosphate precursor and drying it, adding a carbon source after one calcination, and performing a second calcination to obtain a finished product of lithium iron phosphate.
  • the insoluble ferrous compound ferrous phosphate Fe 3 (PO 4 ) 2 ⁇ 8H 2 O
  • the solid content of the synthetic product cannot be increased, which is not conducive to the increase of production capacity and the cost saving of the drying process.
  • iron powder is first reacted in an aqueous solution containing phosphoric acid and citric acid, and then lithium hydroxide is added to prepare a lithium iron phosphate precursor.
  • the surface of the iron powder first reacts with phosphoric acid to generate an insoluble ferrous compound, ferrous phosphate (Fe 3 (PO 4 ) 2 8H 2 O), and the product on the surface hinders the further reaction of the metal iron powder with phosphoric acid. As a result, the reaction is not sufficient, and citric acid cannot give full play to the chelation effect.
  • iron phosphate is used as raw material to prepare lithium iron phosphate, and the solid content is relatively low, resulting in high process cost; when iron powder is used as raw material to prepare lithium iron phosphate, the solid content is difficult to control so that the reaction can be carried out smoothly. , and can reduce the energy consumption of subsequent processes.
  • the present invention aims to solve the problem in the prior art that when iron phosphate is used as raw material to prepare lithium iron phosphate, the solid content is relatively low, resulting in high process cost; when iron powder is used as raw material to prepare lithium iron phosphate, the solid content is difficult to control so that the reaction It can be carried out smoothly, and the energy consumption of the subsequent process can be reduced, and a new type of green lithium iron phosphate precursor and its preparation method and application are provided.
  • the inventors have found that when the iron source is used as the raw material in the preparation method of lithium iron phosphate in the prior art, for the smooth progress of the reaction, the solid content is inevitably too low, which leads to the defect of high energy consumption in the subsequent process ; And if the solid content is increased, it will cause the problem that the viscosity is too high and cannot be stirred.
  • the inventor unexpectedly found that by first reacting the product A obtained by fully reacting the iron source with phosphoric acid, and then carrying out the mixed reaction with the product B obtained after fully reacting the organic acid, lithium source and carbon source, it is possible to make the lithium iron phosphate precursor
  • the solid content reaches more than 50%, even 60%, which greatly reduces the energy consumption in the process of producing lithium iron phosphate from the lithium iron phosphate precursor, and has a simple preparation method and low cost.
  • the method of the present invention can prepare a lithium iron phosphate precursor with an extremely small particle size, and has a high charge-discharge rate. It has been proved experimentally that this effect cannot be achieved if the organic acid is not added in the reaction of product B.
  • the present invention solves the above-mentioned technical problems through the following technical solutions.
  • the invention provides a kind of preparation method of lithium iron phosphate precursor, it comprises the steps:
  • the preparation sequence of the product A and the product B is not limited;
  • step S1 the mixed reaction of the iron source and the phosphoric acid solution is completed, and those skilled in the art know that the reaction generally does not produce gas.
  • the iron source is known to those skilled in the art.
  • the present invention is a process for preparing lithium iron phosphate after including the step of preparing iron phosphate. Therefore, those skilled in the art know that the described Sources of iron do not include iron phosphate.
  • the iron source is a compound containing iron and oxygen, more preferably one or more of iron powder, ferric oxide, ferric oxide and ferric nitrate, and more preferably iron One or more of powder, ferric oxide and ferric oxide.
  • the iron content in the iron powder is more than 95wt%, more preferably more than 99wt%, further more preferably more than 99.5wt%, such as 99.7wt%, such as primary reduced iron powder, One or more of secondary reduced iron powder, carbonyl reduced iron powder and electrolytic iron powder.
  • the purity of the ferric oxide is above 95wt%, more preferably above 99wt%, even more preferably above 99.5wt%.
  • the purity of the ferric oxide is above 95wt%, more preferably above 99wt%, even more preferably above 99.5wt%.
  • the mesh of the iron source is 200-1000 mesh, more preferably 200-500 mesh, for example, 250 mesh or 300 mesh.
  • the phosphoric acid solution generally refers to a phosphoric acid aqueous solution, and the mass percentage concentration of phosphoric acid in the phosphoric acid solution is preferably 20-85%, such as 49%, 59% or 62%.
  • the phosphoric acid in the phosphoric acid solution can be conventional phosphoric acid in the field, such as industrial grade phosphoric acid, food grade phosphoric acid, electrical grade phosphoric acid or electronic grade phosphoric acid, etc.
  • the electrical grade phosphoric acid can be purchased from Guangxi Qinzhou Chengxing Chemical Industry Co., Ltd. Technology Co., Ltd.
  • the reaction temperature of the mixture of the iron source and the phosphoric acid solution is 20-95°C, more preferably 30-90°C, such as 35°C, 45°C or 55°C.
  • the mixture of the iron source and the phosphoric acid solution is prepared by adding the iron source to the phosphoric acid solution under stirring.
  • the molar ratio of iron element to phosphoric acid is (0.94-1.05):1, more preferably (0.96-1.0):1, for example 0.98: 1.
  • the grinding operation and conditions may be conventional grinding operations, such as sand milling or ball milling.
  • the grinding is carried out using a sand mill.
  • the sand mill is preferably a vertical sand mill, a horizontal sand mill (such as a nanoscale horizontal sand mill), a basket sand mill or a double-cone rod sand mill.
  • the particle size of the grinding beads used in the sand mill is preferably 0.1-3.0 mm, such as 0.3 mm or 0.4 mm.
  • the grinding beads used in the sand mill are preferably zirconia beads.
  • the viscosity of the product A is 8000-20000 cps, more preferably 10000-20000 cps, such as 15000 cps.
  • the organic acid solution generally refers to an organic acid solution, and the mass percentage concentration of the organic acid in the organic acid solution is preferably 5-98%, such as 55%, 62% or 72% %.
  • the organic acid in the organic acid solution is a carboxylic acid compound and/or ascorbic acid, and the carboxylic acid compound is preferably formic acid, acetic acid, oxalic acid, citric acid, tartaric acid and malic acid.
  • the organic acid is, for example, citric acid and/or oxalic acid, or malic acid and/or tartaric acid.
  • the lithium source is one or more of lithium hydroxide monohydrate, lithium carbonate, lithium dihydrogen phosphate, lithium phosphate and lithium acetate, more preferably lithium hydroxide monohydrate and/or Or lithium acetate; Described lithium carbonate is preferably technical grade lithium carbonate or battery grade lithium carbonate.
  • the molar ratio of the lithium element in the lithium source to the phosphoric acid in the phosphoric acid solution is 0.98-1.05, such as 1.02, 1.03 or 1.04.
  • the carbon source includes one or more of glucose, sucrose, starch, phenolic resin, cyclodextrin, polyethylene, polyethylene glycol and polyvinyl alcohol, more preferably polyvinyl alcohol , a mixture of cyclodextrin and polyethylene glycol.
  • the carbon source is added in an amount of 1% to 60% by mass of the iron source, more preferably 5% to 50%, and even more preferably 10% to 40%.
  • the reaction temperature of the mixture of organic acid, lithium source and carbon source is 20-95°C, more preferably 30-90°C, such as 35°C, 40°C or 45°C.
  • the mixture of the organic acid, the lithium source and the carbon source is prepared by adding the lithium source and the carbon source into the organic acid solution under stirring.
  • the mixture of the product A and the product B is generally just mixing the product A and the product B.
  • S2 the grinding operation and conditions can be conventional in the art.
  • the preferred implementation of the grinding can be the same as S1.
  • the particle size of the lithium iron phosphate precursor is 170-250 nm, such as 200 nm or 220 nm.
  • the present invention also provides a precursor of lithium iron phosphate, which is prepared by the method for preparing the precursor of lithium iron phosphate as described above.
  • the particle size of the lithium iron phosphate precursor is 170-250 nm.
  • the present invention also provides a kind of preparation method of lithium iron phosphate, it comprises the steps:
  • the lithium iron phosphate precursor as described above was spray dried, calcined and crushed.
  • the operations and conditions of the spray drying, the calcination and the crushing can be conventional in the field.
  • the inlet temperature may be 280°C.
  • the outlet temperature may be 110°C.
  • the calcination conditions can be: under a nitrogen atmosphere with a purity of 99.999%, gradually increase the temperature from room temperature to 650°C at a rate of 5°C/min, keep the temperature at 650°C for 10 hours, and cool down to obtain a sintered product.
  • the present invention also provides a kind of lithium iron phosphate, which is prepared by the above-mentioned preparation method of lithium iron phosphate.
  • the present invention also provides an application of the aforementioned lithium iron phosphate in the preparation of positive electrode materials for lithium ion batteries.
  • the reagents and raw materials used in the present invention are all commercially available.
  • the solid content can be greatly increased, the energy consumption of the subsequent process is small, the preparation method is simple, green and environmentally friendly, no three wastes are discharged, the cost is low, and the positive electrode material iron phosphate using iron source as raw material is realized. Low-cost production of lithium. Moreover, the particle size of the lithium iron phosphate precursor prepared by the present invention is extremely small, and the charge and discharge rate is high.
  • Fig. 1 is the XRD pattern of the lithium iron phosphate of embodiment 1.
  • Example 2 is a scanning electron micrograph of the lithium iron phosphate of Example 1.
  • Example 3 is the charge and discharge curves of the lithium iron phosphate in Example 1 at different rates.
  • reaction product slurry is spray-dried, sintered, and crushed to obtain a lithium iron phosphate positive electrode material.
  • the conditions of spray drying are: the inlet temperature is 280°C, and the outlet temperature is 110°C.
  • Calcination conditions are as follows: in a nitrogen atmosphere with a purity of 99.999%, gradually increase the temperature from room temperature to 650°C at a rate of 5°C/min, keep the temperature at 650°C for 10 hours, and cool down to obtain a sintered product.
  • the lithium iron phosphate cathode material prepared in Example 1 was subjected to PXRD (powder X-Ray diffraction) and scanning electron microscope (SEM) tests.
  • the PXRD data in Figure 1 was obtained by Bruker D8 ADVANCE test.
  • the SEM picture of Fig. 2 is obtained by SU8010 test of Hitachi Company.
  • reaction product slurry is spray-dried, sintered, and crushed to obtain a lithium iron phosphate positive electrode material.
  • the conditions of spray drying are: the inlet temperature is 280°C, and the outlet temperature is 110°C.
  • Calcination conditions are as follows: in a 99.999% pure nitrogen atmosphere, gradually increase the temperature from room temperature to 650°C at a rate of 5°C/min, keep the temperature at 650°C for 10 hours, and cool down to obtain a sintered product.
  • reaction product slurry is spray-dried, sintered, and crushed to obtain a lithium iron phosphate positive electrode material.
  • the conditions of spray drying are: the inlet temperature is 280°C, and the outlet temperature is 110°C.
  • Calcination conditions are as follows: in a nitrogen atmosphere with a purity of 99.999%, gradually increase the temperature from room temperature to 650°C at a rate of 5°C/min, keep the temperature at 650°C for 10 hours, and cool down to obtain a sintered product.
  • reaction product slurry is spray-dried, sintered, and crushed to obtain a lithium iron phosphate positive electrode material.
  • the conditions of spray drying are: the inlet temperature is 280°C, and the outlet temperature is 110°C.
  • Calcination conditions are as follows: in a nitrogen atmosphere with a purity of 99.999%, gradually increase the temperature from room temperature to 650°C at a rate of 5°C/min, keep the temperature at 650°C for 10 hours, and cool down to obtain a sintered product.
  • reaction product slurry is spray-dried, sintered, and crushed to obtain a lithium iron phosphate positive electrode material.
  • the conditions of spray drying are: the inlet temperature is 280°C, and the outlet temperature is 110°C.
  • Calcination conditions are as follows: in a 99.999% pure nitrogen atmosphere, gradually increase the temperature from room temperature to 650°C at a rate of 5°C/min, keep the temperature at 650°C for 10 hours, and cool down to obtain a sintered product.
  • reaction product slurry is spray-dried, sintered and crushed to obtain a lithium iron phosphate cathode material.
  • the conditions of spray drying are: the inlet temperature is 280°C, and the outlet temperature is 110°C.
  • Calcination conditions are as follows: in a nitrogen atmosphere with a purity of 99.999%, gradually increase the temperature from room temperature to 650°C at a rate of 5°C/min, keep the temperature at 650°C for 10 hours, and cool down to obtain a sintered product.
  • reaction product slurry is spray-dried, sintered, and crushed to obtain a lithium iron phosphate positive electrode material.
  • the conditions of spray drying are: the inlet temperature is 280°C, and the outlet temperature is 110°C.
  • Calcination conditions are as follows: in a nitrogen atmosphere with a purity of 99.999%, gradually increase the temperature from room temperature to 650°C at a rate of 5°C/min, keep the temperature at 650°C for 10 hours, and cool down to obtain a sintered product.
  • Example 1 Example 2
  • Example 3 Example 4
  • Example 5 Comparative example 2 Comparative example 3 Finished slurry solid content/% 50 53 60 50 50 17 35 Dehydration amount required for 1kg precursor/kg 1.0 0.88 0.66 1.0 1.0 4.88 1.86 Dehydration energy consumption required for 1kg precursor Low Low Low Low Low high high
  • Examples 1-5 can significantly reduce the amount of dehydration required for the prepared precursor, thereby significantly reducing the energy consumption required for dehydration.
  • comparative example 1 based on the preparation method of the prior art, only the solid content is increased, and there is a problem that the viscosity is too high to be stirred.
  • Comparative Examples 2-3 the organic acid was not added in the reaction of product B, and the effect of the present invention could not be realized.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)
PCT/CN2022/118186 2021-09-10 2022-09-09 一种新型绿色磷酸铁锂前驱体及其制备方法、应用 Ceased WO2023036308A1 (zh)

Priority Applications (8)

Application Number Priority Date Filing Date Title
AU2022342227A AU2022342227B2 (en) 2021-09-10 2022-09-09 Novel green lithium iron phosphate precursor, preparation method therefor and application thereof
KR1020247011610A KR102843962B1 (ko) 2021-09-10 2022-09-09 신규 녹색 리튬인산철 전구체, 이의 제조 방법, 및 이의 용도
CA3231076A CA3231076A1 (en) 2021-09-10 2022-09-09 Novel green lithium iron phosphate precursor, preparation method therefor and application thereof
EP22866769.7A EP4400475A4 (en) 2021-09-10 2022-09-09 Novel green lithium iron phosphate precursor, preparation method therefor and application thereof
JP2024515845A JP7728047B2 (ja) 2021-09-10 2022-09-09 新規な緑色リン酸鉄リチウム前駆体、及びその製造方法、使用
US18/688,381 US12209017B2 (en) 2021-09-10 2022-09-09 Green lithium iron phosphate precursor, preparation method therefor and application thereof
MX2024003002A MX2024003002A (es) 2021-09-10 2022-09-09 Precursor novedoso de fosfato de hierro y litio verde, método de preparación del mismo y aplicación del mismo.
ZA2024/02648A ZA202402648B (en) 2021-09-10 2024-04-05 Novel green lithium iron phosphate precursor, preparation method therefor and application thereof

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN202111064354.9A CN113896182B (zh) 2021-09-10 2021-09-10 一种绿色磷酸铁锂前驱体及其制备方法、应用
CN202111064354.9 2021-09-10

Publications (1)

Publication Number Publication Date
WO2023036308A1 true WO2023036308A1 (zh) 2023-03-16

Family

ID=79027682

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2022/118186 Ceased WO2023036308A1 (zh) 2021-09-10 2022-09-09 一种新型绿色磷酸铁锂前驱体及其制备方法、应用

Country Status (10)

Country Link
US (1) US12209017B2 (enExample)
EP (1) EP4400475A4 (enExample)
JP (1) JP7728047B2 (enExample)
KR (1) KR102843962B1 (enExample)
CN (1) CN113896182B (enExample)
AU (1) AU2022342227B2 (enExample)
CA (1) CA3231076A1 (enExample)
MX (1) MX2024003002A (enExample)
WO (1) WO2023036308A1 (enExample)
ZA (1) ZA202402648B (enExample)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116395659A (zh) * 2023-04-14 2023-07-07 河南龙佰新能源材料技术有限公司 一种高倍率磷酸铁锂正极材料的制备方法
CN116635327A (zh) * 2023-03-20 2023-08-22 广东邦普循环科技有限公司 一种磷酸锰铁锂及制备其的方法与用途
CN117133913A (zh) * 2023-08-25 2023-11-28 上海量孚新能源科技有限公司 磷酸铁锂前驱体、磷酸铁锂材料及其制备方法和应用
CN117509589A (zh) * 2023-10-20 2024-02-06 贵州航盛锂能科技有限公司 一种磷酸铁锂的制备方法及其应用
WO2025050414A1 (zh) * 2023-09-08 2025-03-13 广东邦普循环科技有限公司 一种磷酸锰铁锂及其制备方法和应用

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113896182B (zh) * 2021-09-10 2023-05-23 上海量孚新能源科技有限公司 一种绿色磷酸铁锂前驱体及其制备方法、应用
CN114735670B (zh) 2022-04-12 2023-11-03 宜昌邦普时代新能源有限公司 高性能磷酸铁锂的制备方法及其应用
US20240034626A1 (en) * 2022-07-26 2024-02-01 Watix Technology LLC Method for preparing high performance lithium iron phosphate nanopowder
CN115353085B (zh) * 2022-09-21 2023-09-22 上海量孚新能源科技有限公司 一种含补锂剂的磷酸铁锂复合材料及其制备方法、应用和含其的电池
TWI827275B (zh) * 2022-09-27 2023-12-21 台灣立凱電能科技股份有限公司 磷酸鋰鐵正極材料的製備方法
CN116281932A (zh) * 2023-04-18 2023-06-23 上海量孚新能源科技有限公司 一种磷酸锰铁锂及制备方法、应用
WO2025043375A1 (zh) 2023-08-25 2025-03-06 上海量孚新能源科技有限公司 磷酸铁锂前驱体、磷酸铁锂材料及其制备方法和应用
TWI911872B (zh) * 2023-08-25 2026-01-11 大陸商上海量孚新能源科技有限公司 磷酸鐵鋰前驅物、磷酸鐵鋰材料及其製備方法和應用
KR20250156980A (ko) * 2024-04-26 2025-11-04 주식회사 에코프로비엠 리튬 이차 전지용 양극 활물질의 제조 방법
CN118206097B (zh) * 2024-05-21 2024-09-27 上海量孚新能源科技有限公司 磷酸锰铁前驱体及其制备方法、磷酸锰铁锂、含其的正极片、二次电池
CN119018871B (zh) * 2024-10-25 2025-10-17 上海量孚新能源科技有限公司 磷酸铁锂前驱体及其制备方法、磷酸铁锂及其制备方法和应用
CN120504305B (zh) * 2025-07-22 2025-10-21 上海量孚新能源科技有限公司 一种磷酸铁锂材料及其制备方法和应用

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004036671A1 (ja) 2002-10-18 2004-04-29 Japan As Represented By President Of The University Of Kyusyu ２次電池用正極材料の製造方法、および２次電池
JP2007305585A (ja) 2006-05-11 2007-11-22 Aquire Energy Co Ltd 充電式バッテリ製造用の陰極材料
CN102348634A (zh) 2009-03-13 2012-02-08 杰富意化学株式会社 磷酸铁锂的制造方法
CN107814372A (zh) * 2017-11-02 2018-03-20 沈阳国科金能新材料有限公司 一种磷酸铁锂正极材料的制备方法和应用
CN109607506A (zh) * 2018-12-29 2019-04-12 合肥融捷能源材料有限公司 一种提升磷酸铁锂前驱体振实密度的方法
CN109742352A (zh) * 2018-12-29 2019-05-10 浙江南都电源动力股份有限公司 磷酸铁锂/碳复合材料的制备方法
CN112390241A (zh) * 2020-11-17 2021-02-23 湖北融通高科先进材料有限公司 一种磷酸铁锂材料及以混合铁源和混合锂源为原料制备磷酸铁锂材料的方法
CN113896182A (zh) * 2021-09-10 2022-01-07 上海量孚新能源科技有限公司 一种新型绿色磷酸铁锂前驱体及其制备方法、应用

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI279020B (en) * 2004-11-03 2007-04-11 Tatung Co Ltd Preparation of olivine LiFePO4 cathode materials for lithium batteries via a solution method
JP4999887B2 (ja) 2009-06-18 2012-08-15 株式会社関 高純度パラジウム製品、及びその鋳造方法
JP5581065B2 (ja) 2010-01-14 2014-08-27 Ｊｆｅケミカル株式会社 リン酸鉄リチウムの製造方法
CA2842165C (en) * 2011-07-20 2017-04-11 Advanced Lithium Electrochemistry Co., Ltd. Preparation method of battery composite material and precursor thereof
CN102683697B (zh) * 2012-05-14 2014-12-17 国光电器股份有限公司 一种石墨烯基LiFePO4/C复合材料的制备方法
KR101973052B1 (ko) * 2012-08-10 2019-04-26 삼성에스디아이 주식회사 리튬 금속인산화물의 제조방법
US9136534B2 (en) * 2013-03-15 2015-09-15 Nano One Materials Corp. Complexometric precursors formulation methodology for industrial production of high performance fine and ultrafine powders and nanopowders for specialized applications
CN103208614B (zh) * 2013-04-15 2015-10-21 黄科竣 一种锂离子电池用磷酸铁锂正极材料的合成方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004036671A1 (ja) 2002-10-18 2004-04-29 Japan As Represented By President Of The University Of Kyusyu ２次電池用正極材料の製造方法、および２次電池
JP2007305585A (ja) 2006-05-11 2007-11-22 Aquire Energy Co Ltd 充電式バッテリ製造用の陰極材料
CN102348634A (zh) 2009-03-13 2012-02-08 杰富意化学株式会社 磷酸铁锂的制造方法
CN107814372A (zh) * 2017-11-02 2018-03-20 沈阳国科金能新材料有限公司 一种磷酸铁锂正极材料的制备方法和应用
CN109607506A (zh) * 2018-12-29 2019-04-12 合肥融捷能源材料有限公司 一种提升磷酸铁锂前驱体振实密度的方法
CN109742352A (zh) * 2018-12-29 2019-05-10 浙江南都电源动力股份有限公司 磷酸铁锂/碳复合材料的制备方法
CN112390241A (zh) * 2020-11-17 2021-02-23 湖北融通高科先进材料有限公司 一种磷酸铁锂材料及以混合铁源和混合锂源为原料制备磷酸铁锂材料的方法
CN113896182A (zh) * 2021-09-10 2022-01-07 上海量孚新能源科技有限公司 一种新型绿色磷酸铁锂前驱体及其制备方法、应用

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116635327A (zh) * 2023-03-20 2023-08-22 广东邦普循环科技有限公司 一种磷酸锰铁锂及制备其的方法与用途
CN116395659A (zh) * 2023-04-14 2023-07-07 河南龙佰新能源材料技术有限公司 一种高倍率磷酸铁锂正极材料的制备方法
CN117133913A (zh) * 2023-08-25 2023-11-28 上海量孚新能源科技有限公司 磷酸铁锂前驱体、磷酸铁锂材料及其制备方法和应用
WO2025050414A1 (zh) * 2023-09-08 2025-03-13 广东邦普循环科技有限公司 一种磷酸锰铁锂及其制备方法和应用
CN117509589A (zh) * 2023-10-20 2024-02-06 贵州航盛锂能科技有限公司 一种磷酸铁锂的制备方法及其应用

Also Published As

Publication number Publication date
KR102843962B1 (ko) 2025-08-08
MX2024003002A (es) 2024-05-29
US20240417259A1 (en) 2024-12-19
US12209017B2 (en) 2025-01-28
CN113896182A (zh) 2022-01-07
JP7728047B2 (ja) 2025-08-22
CA3231076A1 (en) 2023-03-16
JP2024535003A (ja) 2024-09-26
AU2022342227A1 (en) 2024-05-02
ZA202402648B (en) 2024-12-18
EP4400475A4 (en) 2025-03-19
CN113896182B (zh) 2023-05-23
EP4400475A1 (en) 2024-07-17
KR20240055829A (ko) 2024-04-29
AU2022342227B2 (en) 2026-01-15

Similar Documents

Publication Publication Date Title
CN113896182B (zh) 一种绿色磷酸铁锂前驱体及其制备方法、应用
CN102348634B (zh) 磷酸铁锂的制造方法
WO2021159618A1 (zh) 一种高功率型的锂离子电池用正极材料及其制备方法
CN108933239B (zh) 一种锰酸锂包覆镍钴锰酸锂正极材料的制备方法
CN102386391B (zh) 一种制备三元复合正极材料LiNixCoyMn1-x-yO2的方法
CN104201324B (zh) 一种模板法合成锂离子电池正极材料镍钴锰酸锂的方法
CN101369651A (zh) 一种制备锂离子电池正极三元系材料LiCoxNiyMn2O2的新方法
CN113991112A (zh) 一种掺杂纳米二氧化钛磷酸铁锂正极材料的制备方法
CN101875488A (zh) 综合利用钛铁矿制备钛酸锂和磷酸铁锂前驱体的方法
CN118039883B (zh) 一种磷酸铁锂材料及其制备方法、应用和锂离子电池
CN113800574B (zh) 一种镍锰铁铝锂正极材料及其制备方法
CN104692465B (zh) 锂离子电池正极材料α-LiFeO2纳米粉体的制备方法
CN117303337A (zh) 一种磷酸锰铁锂复合正极材料掺杂制备方法
CN112694137A (zh) 小粒径无钴富锂锰基固溶体与钒酸锂复合材料及制备方法
CN114520319A (zh) 一种锂二次电池镍基正极材料及其制备方法
CN117361486A (zh) 一种磷酸亚铁复合磷酸亚锰铁制备磷酸锰铁锂的方法及应用
CN113314707B (zh) 一种改性镍钴铝酸锂正极材料及其制备方法和应用
CN106335924B (zh) 一种NaV2O5的制备方法
CN113285071B (zh) 磷酸铁锂及其制备方法与应用
CN112010277B (zh) 一种含钒矿料制备钠离子电池氟磷酸氧钒钠正极材料的方法及制得的正极材料
CN110350162B (zh) 一种倍率型镍钴铝正极材料及其制备方法和应用
CN106129383A (zh) 一种具有纳米级两相梯度分布结构的球形锂离子电池正极材料及其合成方法
CN119430122A (zh) 一种以磷酸铁锂废粉制备磷酸锰铁锂正极材料的方法
CN117673316A (zh) 一种聚阴离子钠离子电池正极材料及其制备方法与应用
CN115285962A (zh) 一种低成本磷酸系正极材料的制备方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 22866769

Country of ref document: EP

Kind code of ref document: A1

WWE Wipo information: entry into national phase

Ref document number: 3231076

Country of ref document: CA

ENP Entry into the national phase

Ref document number: 2024515845

Country of ref document: JP

Kind code of ref document: A

WWE Wipo information: entry into national phase

Ref document number: 2401001598

Country of ref document: TH

WWE Wipo information: entry into national phase

Ref document number: 202447026401

Country of ref document: IN

WWE Wipo information: entry into national phase

Ref document number: AU2022342227

Country of ref document: AU

ENP Entry into the national phase

Ref document number: 20247011610

Country of ref document: KR

Kind code of ref document: A

WWE Wipo information: entry into national phase

Ref document number: 202490695

Country of ref document: EA

WWE Wipo information: entry into national phase

Ref document number: 2022866769

Country of ref document: EP

NENP Non-entry into the national phase

Ref country code: DE

ENP Entry into the national phase

Ref document number: 2022866769

Country of ref document: EP

Effective date: 20240410

WWE Wipo information: entry into national phase

Ref document number: 11202401631Q

Country of ref document: SG

ENP Entry into the national phase

Ref document number: 2022342227

Country of ref document: AU

Date of ref document: 20220909

Kind code of ref document: A

WWG Wipo information: grant in national office

Ref document number: 11202401631Q

Country of ref document: SG