CN104051731A - Pollution-free and zero-discharge lithium iron phosphate preparation method - Google Patents

Pollution-free and zero-discharge lithium iron phosphate preparation method Download PDF

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Publication number
CN104051731A
CN104051731A CN201410141204.7A CN201410141204A CN104051731A CN 104051731 A CN104051731 A CN 104051731A CN 201410141204 A CN201410141204 A CN 201410141204A CN 104051731 A CN104051731 A CN 104051731A
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lifepo4
temperature
crystal
autoclave
pollution
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CN104051731B (en
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孙青林
汪浩
魏宏政
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Nanyang Fengyuan New Energy Technology Co., Ltd
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魏宏政
孙青林
汪浩
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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
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention relates to a pollution-free and zero-discharge lithium iron phosphate preparation method. The pollution-free and zero-discharge lithium iron phosphate preparation method accords with the green chemistry and fine chemical idea of environmental friendliness, sustainable development and no pollution. According to the pollution-free and zero-discharge lithium iron phosphate preparation method, a lithium source, an iron source and a phosphorus source are dissolved and mixed in an appropriate environment, the mixture is synthesized into high-purity lithium iron phosphate crystals under the control of synthesis conditions in reaction process, different components of the product are controlled so that separation treatment is easy, a lithium iron phosphate crystal precursor is extracted and then is clathrated, the clathrated lithium iron phosphate crystal precursor is subjected to carbonization annealing heat treatment, the residual liquid and byproduct are subjected to green treatment and then be recycled, and heat produced by cooling is recovered and recycled. The lithium iron phosphate material obtained by the preparation method has good electrochemical performances, high purity and good processing performances. The preparation method realizes reasonable element content, has stable batch, no pollution and zero discharge and is convenient for large-scale production.

Description

The method of LiFePO4 is prepared in a kind of pollution-free zero discharge
Technical field
The invention belongs to chemical industry synthetic material field, the present invention relates to specifically a kind of green chemistry process method that LiFePO4 is prepared in pollution-free zero discharge.
Background technology
NTT from Japan in 1996 discloses AyMPO first 4(A is alkali metal, and M is both combinations of CoFe: LiFeCOPO 4) the anode material of lithium battery of olivine structural after, the Research Groups such as the vertical John. B. Goodenough of university of Texas, USA in 1997, have reported LiFe PO 4olivine structural (LiM PO 4), European has also found the LiFePO of natural olivine structural 4.LiFePO 4also be found to have commercialization secondary battery material lithium as sour in cobalt, lithium nickelate, the superior function that the materials such as ternary are incomparable.This material possesses raw material wide material sources, cheap, memory-less effect, has extended cycle life, and security performance is good, and high-temperature behavior is good, not containing heavy metal, and the series of advantages such as non-environmental-pollution.
Although LiFePO 4there is plurality of advantages, also be considered to very promising lithium ion secondary battery anode material, cause the energetically research and development manufacture of various countries to this material, consequent patent and paper are also too numerous to enumerate, great majority research and development are manufactured and are all only laid particular emphasis in the pursuit of material self performance and value, and ignored one, are about to as the produced pollution in global energy carrier materials production process of new generation.
Yet we but think a kind of birth of new green energy resource, should be to be all green from the aborning of it, rather than in order to obtain a kind of new green energy resource, before obtaining, just cause serious environmental pollution, may lose more than gain like this.The LiFePO that traditional solid phase method and liquid phase method or microwave are synthetic 4, not only the time long, energy consumption is large, particle size distribution is uneven, performance is undesirable, discharges a large amount of waste gas simultaneously, the pollutants such as waste water, dust cause serious environmental pollution.Traditional high temperature solid-state method adopts Li 2cO 3+ 2FeC 2o 4+ 2NH 4h 2pO 4=2LiFePO 4+ 2NH 3↑+5CO 2↑+3H 2o, 1 ton of LiFePO of every production 4, will produce about 350m 3cO 2gas also will produce approximately 153 m simultaneously 3nH 3gas, these gases all have very large pollution to air, and be difficult to reclaim, also have a large amount of moisture discharge.We consider analysis to these problems just, and planning of science activities has designed a kind of green chemistry process method that high-quality LiFePO4 is prepared in pollution-free zero discharge.
Summary of the invention
The object of this invention is to provide a kind of pollution-free zero discharge and prepare the method for LiFePO4, environmental friendliness, sustainable development, free of contamination Green Chemistry have been fully demonstrated, fine chemistry industry theory, by the control to synthesis condition course of reaction, the LiFePO4 crystal of synthesis of high purity, carries out the rear cycling and reutilization of green processing to remaining liquid and byproduct.
The lithium iron phosphate preparation method of a kind of pollution-free zero discharge provided by the invention, is characterized in that comprising the following steps:
First by H 3pO 4, FeCl 2and LiOH, within 1: 1: 3 in molar ratio, weigh, then respectively by load weighted H 3pO 4, FeCl 2supersaturation is dissolved in deionized water with LiOH, forms the H of molecular level 3pO 4precursor solution, FeCl 2precursor solution and LiOH precursor solution, then by described H 3pO 4precursor solution adds in autoclave, and makes high pressure temperature in the kettle rise to 50-110 ℃, then slowly adds FeCl 2precursor solution, makes H 3pO 4precursor solution and FeCl 2after precursor solution mixes, in described autoclave, pass into inert gas, then in described autoclave, add LiOH precursor solution, then in autoclave, starting temperature reaction is FeCl 2+ H 3pO 4+ 3LiOH → 2LiCl ?+ LiFePO 4↓+3H 2o, in temperature reaction process, make high pressure temperature in the kettle rise to 120-260 ℃ with 1-10 ℃/min speed, described autoclave internal pressure is controlled at 0.2-4.7MPa, whole temperature reaction process continues 4-15 hour, in whole temperature reaction process, material in autoclave is not stopped to stir, after temperature reaction, by carrying out cold oil circulation with the supporting heat-conducting oil furnace of autoclave, make in autoclave with 1-20 ℃/min rate of temperature fall cooling down to room temperature, heat-conducting oil furnace carries out cold oil and follows the thermal energy storage of rear cold oil recovery and be cycled to used in follow-up concentration, again the material in autoclave is introduced to solid-liquid separating equipment by baiting valve and drainage pump and isolate LiFePO4 crystal and LiCl solution, LiFePO4 crystal water is fully washed, deionized water as cycling and reutilization after the water deionization processing of again washing LiFePO4 crystal being used is used, by LiCl solution, by cell reaction, be 2H 2o+2Cl -=Cl 2↑+H 2↑+2OH -and 2H 2o+2LiCl=Cl 2↑+H 2↑+2LiOH is cycled to used in the LiOH solution generating in cell reaction and prepares LiFePO4 crystal after concentration, and the chlorine generating in cell reaction is passed in water and generates hydrochloric acid, adds iron powder to generate again FeCl in hydrochloric acid 2solution, this FeCl 2after solution concentration, be cycled to used in and prepare LiFePO4 crystal, using the hydrogen generating in cell reaction, after collecting, as fuel gas buring, provide heat energy for concentration and heating high-pressure still, the water that concentration produces recycles as deionized water after deionization is processed.
Further, after temperature reaction, material in autoclave is carried out to Separation of Solid and Liquid, gained solid is LiFePO4 crystal, isolated LiFePO4 crystal is washed, keep the percentage by weight of water in the LiFePO4 crystal after washing 30-80%, after washing, form LiFePO4 crystal suspension-turbid liquid, then in LiFePO4 crystal suspension-turbid liquid, add inclusion compound, the mol ratio of the inclusion compound adding and LiFePO4 crystal is 1-2.5: 1, inclusion compound supersaturation is dissolved in LiFePO4 crystal suspension-turbid liquid, then by physical and chemical effect, inclusion process is completed under saturated solution and the interactional mechanism of ultrasonic dispersion, form LiFePO4 inclusion compound crystal presoma, clathrate process completes final vacuum or low temperature drying LiFePO4 inclusion compound crystal presoma, again LiFePO4 inclusion compound crystal presoma is added in inert atmosphere protection or vacuum furnace, carry out high temperature cabonization annealing, carbonization annealing temperature is controlled at 600-800 ℃, constant temperature time was controlled between 4-6 hours, adopt air-cooled heat reclaim unit make vacuum furnace be down to normal temperature and reclaim the heat energy in temperature-fall period, the heat circulation reclaiming is for described concentration, finally obtain the LiFePO4 crystal being coated.
Further, described inclusion compound is hydroquinones or β-cyclodextrin.
The present invention, by the research that becomes more meticulous to synthesis technique, designs the reasonable cycle for the treatment of utilization to byproduct to the science of synthetic route.Electrochemical performances of lithium iron phosphate prepared by this technique is good, batch stable and consistent, and good processability, can be competent at the high requirement of electrokinetic cell to positive electrode, and whole production process meets fine chemistry industry, Green Chemistry theory is pollution-free.Method used in the present invention is pollution-free, does not produce three industrial wastes after recovery, and the product reclaiming all becomes raw material, directly utilizes, and for producing next time again, can make this manufacture of materials cost decline 1/3, and do not produce pollution by this process cycles after reclaiming.
Accompanying drawing explanation
Fig. 1 is technological process rough schematic of the present invention;
Fig. 2 is the gram volume resolution chart of the prepared LiFePO 4 material of the present invention;
Fig. 3 is the multiplying power resolution chart of the prepared LiFePO 4 material of the present invention;
Fig. 4 is the cycle performance resolution chart of the prepared LiFePO 4 material of the present invention;
Fig. 5 is the particle size distribution figure of the prepared LiFePO 4 material of the present invention;
Fig. 6 is the XRD figure of the prepared LiFePO 4 material of the present invention.
Embodiment
Embodiment mono-
Referring to Fig. 1, a kind of lithium iron phosphate preparation method of pollution-free zero discharge, is characterized in that comprising the following steps:
First by H 3pO 4, FeCl 2and LiOH, within 1: 1: 3 in molar ratio, weigh, then respectively by load weighted H 3pO 4, FeCl 2supersaturation is dissolved in deionized water with LiOH, forms the H of molecular level 3pO 4precursor solution, FeCl 2precursor solution and LiOH precursor solution, then by described H 3pO 4precursor solution adds in autoclave, and makes high pressure temperature in the kettle rise to 50-110 ℃, then slowly adds FeCl 2precursor solution, makes H 3pO 4precursor solution and FeCl 2after precursor solution mixes, in described autoclave, pass into inert gas, then in described autoclave, add LiOH precursor solution, then in autoclave, starting temperature reaction is FeCl 2+ H 3pO 4+ 3LiOH → 2LiCl ?+ LiFePO 4↓+3H 2o, in temperature reaction process, make high pressure temperature in the kettle rise to 120-260 ℃ with 1-10 ℃/min speed, described autoclave internal pressure is controlled at 0.2-4.7MPa, whole temperature reaction process continues 4-15 hour, in whole temperature reaction process, material in autoclave is not stopped to stir, after temperature reaction, by carrying out cold oil circulation with the supporting heat-conducting oil furnace of autoclave, make in autoclave with 1-20 ℃/min rate of temperature fall cooling down to room temperature, heat-conducting oil furnace carries out cold oil and follows the thermal energy storage of rear cold oil recovery and be cycled to used in follow-up concentration, again the material in autoclave is introduced to solid-liquid separating equipment by baiting valve and drainage pump and isolate LiFePO4 crystal and LiCl solution, LiFePO4 crystal water is fully washed, deionized water as cycling and reutilization after the water deionization processing of again washing LiFePO4 crystal being used is used, by LiCl solution, by cell reaction, be 2H 2o+2Cl -=Cl 2↑+H 2↑+2OH -and 2H 2o+2LiCl=Cl 2↑+H 2↑+2LiOH is cycled to used in the LiOH solution generating in cell reaction and prepares LiFePO4 crystal after concentration, and the chlorine generating in cell reaction is passed in water and generates hydrochloric acid, adds iron powder to generate again FeCl in hydrochloric acid 2solution, this FeCl 2after solution concentration, be cycled to used in and prepare LiFePO4 crystal, using the hydrogen generating in cell reaction, after collecting, as fuel gas buring, provide heat energy for concentration and heating high-pressure still, the water that concentration produces recycles as deionized water after deionization is processed.
The detailed process of described cell reaction is as follows:
The device that described cell reaction adopts is ion-exchange membrane electrolyzer, and cathode chamber and the anode chamber of ion-exchange membrane electrolyzer separate with cation-exchange membrane ;described LiCl solution enters anode chamber, H during energising 20 electrolysis generates hydrogen at cathode surface, Li +ion by ionic membrane by anode chamber and OH -in conjunction with LiOH; LiOH is the raw material of preparing LiFePO4; Cl -ion generates chlorine at anode surface, by Cl 2pass in water and generate chlorine water, chlorine water finally becomes hydrochloric acid after treatment, and hydrochloric acid reacts with iron powder and generates frerrous chloride, and frerrous chloride is also the raw material of preparing LiFePO4.
The detailed equation of described cell reaction is as follows:
Anode: 2Cl --2e -→ Cl 2↑, the Cl that anode pool produces 2.By Cl 2pass in water and generate chlorine water, chlorine water finally becomes hydrochloric acid Fe+2HCl=FeCl after treatment 2+ H 2↑
?negative electrode: 2H ++ 2e -→ H 2↑, the OH that cathode pool produces -select to see through with cationic membrane the Li of coming +in conjunction with generating LiOH.As OH -+ Li +→ LiOH
Overall reaction: 2H2O+2Cl-=Cl2 ↑+H2 ↑+2OH-and 2H2O+2LiCl=Cl2 ↑+H2 ↑+2LiOH.
The described concentrated steam producing is by condensing tower recycling.
Embodiment bis-
In the described method step of embodiment mono-, further, after temperature reaction, material in autoclave is carried out to Separation of Solid and Liquid, gained solid is LiFePO4 crystal, isolated LiFePO4 crystal is washed, keep the percentage by weight of water in the LiFePO4 crystal after washing 30-80%, after washing, form LiFePO4 crystal suspension-turbid liquid, then in LiFePO4 crystal suspension-turbid liquid, add inclusion compound, the mol ratio of the inclusion compound adding and LiFePO4 crystal is 1-2.5: 1, inclusion compound supersaturation is dissolved in LiFePO4 crystal suspension-turbid liquid, then by physical and chemical effect, inclusion process is completed under saturated solution and the interactional mechanism of ultrasonic dispersion, form LiFePO4 inclusion compound crystal presoma, clathrate process completes final vacuum or low temperature drying LiFePO4 inclusion compound crystal presoma, again LiFePO4 inclusion compound crystal presoma is added in inert atmosphere protection or vacuum furnace, carry out high temperature cabonization annealing, carbonization annealing temperature is controlled at 600-800 ℃, constant temperature time was controlled between 4-6 hours, adopt air-cooled heat reclaim unit make vacuum furnace be down to normal temperature and reclaim the heat energy in temperature-fall period, the heat circulation reclaiming is for described concentration, finally obtain the LiFePO4 crystal being coated.
Embodiment tri-
In the described method step of embodiment bis-, further, described inclusion compound is hydroquinones or β-cyclodextrin.
Detect and analyze:
The detection of entrusting the global group in Xinxiang to do, the preparation-obtained LiFePO 4 material of preparation method by the LiFePO 4 material of a kind of carbo-nitriding provided by the present invention, after testing, the theoretical gram volume of LiFePO4 is 170mAH/g, LiFePO 4 material prepared by this method can be stablized and accomplishes 163mAH/g, specifically referring to gram volume resolution chart accompanying drawing 2; The high rate performance of LiFePO 4 material prepared by this method, the standard of European Union be that 1C charges and discharge and is not less than 130mAH/g, the domestic good 1C that can reach relatively doing at present charges and discharge 135mAH/g, and LiFePO 4 material prepared by this method, data are that 1C charges and discharge 154mAH/g left and right after testing, specifically referring to multiplying power resolution chart accompanying drawing 3; In addition, the lattice stability of LiFePO 4 material prepared by this method embodies by cycle performance, current provided figure be 50 times undamped, specifically referring to Fig. 4; Have, the physical property of this LiFePO 4 material material, can direct-detection, comprises granularity again, can detect by laser fineness gage, and I am Fig. 5 with particle size distribution figure; As for this synthetic powder body material, be the purity of target product LiFePO4 and this product, can carry out check analysis by XRD collection of illustrative plates, I am also Fig. 6 with XRD figure; Finally, batch stability of this LiFePO 4 material, by according to the same method of this technique, same condition, repeats 10 tests, detects gram volume all between 158-163 mAH/g, fluctuation is in 3% left and right, and we think that a batch stability consistency is controlled.

Claims (3)

1. a lithium iron phosphate preparation method for pollution-free zero discharge, is characterized in that comprising the following steps:
First by H 3pO 4, FeCl 2and LiOH, within 1: 1: 3 in molar ratio, weigh, then respectively by load weighted H 3pO 4, FeCl 2supersaturation is dissolved in deionized water with LiOH, forms the H of molecular level 3pO 4precursor solution, FeCl 2precursor solution and LiOH precursor solution, then by described H 3pO 4precursor solution adds in autoclave, and makes high pressure temperature in the kettle rise to 50-110 ℃, then slowly adds FeCl 2precursor solution, makes H 3pO 4precursor solution and FeCl 2after precursor solution mixes, in described autoclave, pass into inert gas, then in described autoclave, add LiOH precursor solution, then in autoclave, starting temperature reaction is FeCl 2+ H 3pO 4+ 3LiOH → 2LiCl ?+ LiFePO 4↓+3H 2o, in temperature reaction process, make high pressure temperature in the kettle rise to 120-260 ℃ with 1-10 ℃/min speed, described autoclave internal pressure is controlled at 0.2-4.7MPa, whole temperature reaction process continues 4-15 hour, in whole temperature reaction process, material in autoclave is not stopped to stir, after temperature reaction, by carrying out cold oil circulation with the supporting heat-conducting oil furnace of autoclave, make in autoclave with 1-20 ℃/min rate of temperature fall cooling down to room temperature, heat-conducting oil furnace carries out cold oil and follows the thermal energy storage of rear cold oil recovery and be cycled to used in follow-up concentration, again the material in autoclave is introduced to solid-liquid separating equipment by baiting valve and drainage pump and isolate LiFePO4 crystal and LiCl solution, LiFePO4 crystal water is fully washed, deionized water as cycling and reutilization after the water deionization processing of again washing LiFePO4 crystal being used is used, by LiCl solution, by cell reaction, be 2H 2o+2Cl -=Cl 2↑+H 2↑+2OH -and 2H 2o+2LiCl=Cl 2↑+H 2↑+2LiOH is cycled to used in the LiOH solution generating in cell reaction and prepares LiFePO4 crystal after concentration, and the chlorine generating in cell reaction is passed in water and generates hydrochloric acid, adds iron powder to generate again FeCl in hydrochloric acid 2solution, this FeCl 2after solution concentration, be cycled to used in and prepare LiFePO4 crystal, using the hydrogen generating in cell reaction, after collecting, as fuel gas buring, provide heat energy for concentration and heating high-pressure still, the water that concentration produces recycles as deionized water after deionization is processed.
2. the lithium iron phosphate preparation method of pollution-free zero discharge as claimed in claim 1, it is characterized in that: after temperature reaction, material in autoclave is carried out to Separation of Solid and Liquid, gained solid is LiFePO4 crystal, isolated LiFePO4 crystal is washed, keep the percentage by weight of water in the LiFePO4 crystal after washing 30-80%, after washing, form LiFePO4 crystal suspension-turbid liquid, then in LiFePO4 crystal suspension-turbid liquid, add inclusion compound, the mol ratio of the inclusion compound adding and LiFePO4 crystal is 1-2.5: 1, inclusion compound supersaturation is dissolved in LiFePO4 crystal suspension-turbid liquid, then by physical and chemical effect, inclusion process is completed under saturated solution and the interactional mechanism of ultrasonic dispersion, form LiFePO4 inclusion compound crystal presoma, clathrate process completes final vacuum or low temperature drying LiFePO4 inclusion compound crystal presoma, again LiFePO4 inclusion compound crystal presoma is added in inert atmosphere protection or vacuum furnace, carry out high temperature cabonization annealing, carbonization annealing temperature is controlled at 600-800 ℃, constant temperature time was controlled between 4-6 hours, adopt air-cooled heat reclaim unit make vacuum furnace be down to normal temperature and reclaim the heat energy in temperature-fall period, the heat circulation reclaiming is for described concentration, finally obtain the LiFePO4 crystal being coated.
3. a kind of method of preparing LiFePO4 with clathrate process as claimed in claim 2, is characterized in that: described inclusion compound is hydroquinones or β-cyclodextrin.
CN201410141204.7A 2014-04-10 2014-04-10 A kind of method that LiFePO4 is prepared in pollution-free zero-emission Active CN104051731B (en)

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WO2016119593A1 (en) * 2015-01-27 2016-08-04 江苏华东锂电技术研究院有限公司 Lithium iron phosphate solvothermal preparation process
US20170320738A1 (en) * 2015-01-27 2017-11-09 Jiangsu Huadong Institute of Li-Ion Battery Co., L td. Solvothermal apparatus for making lithium iron phosphate
CN108609594A (en) * 2018-03-29 2018-10-02 宁夏滨河新材料科技有限公司 The method that wastewater treatment recycles in ferric phosphate production
CN110615419A (en) * 2019-07-01 2019-12-27 湖北虹润高科新材料有限公司 Iron phosphate production facility

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CN102356488A (en) * 2009-03-27 2012-02-15 住友大阪水泥股份有限公司 Method for producing positive electrode active material for lithium ion battery, positive electrode active material for lithium ion battery, electrode for lithium ion battery, and lithium ion battery
CN103080000A (en) * 2010-09-03 2013-05-01 昭和电工株式会社 Method for producing lithium metal phosphate
CN103258993A (en) * 2013-04-24 2013-08-21 北京化工大学 Preparation method of lithium iron phosphate powder for anode material of lithium ion battery

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CN101999187A (en) * 2008-04-25 2011-03-30 住友大阪水泥股份有限公司 Method for production of cathode active material for lithium ion battery, cathode active material for lithium ion battery produced by the method, electrode for lithium ion battery, and lithium ion battery
CN102356488A (en) * 2009-03-27 2012-02-15 住友大阪水泥股份有限公司 Method for producing positive electrode active material for lithium ion battery, positive electrode active material for lithium ion battery, electrode for lithium ion battery, and lithium ion battery
CN103080000A (en) * 2010-09-03 2013-05-01 昭和电工株式会社 Method for producing lithium metal phosphate
CN103258993A (en) * 2013-04-24 2013-08-21 北京化工大学 Preparation method of lithium iron phosphate powder for anode material of lithium ion battery

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016119593A1 (en) * 2015-01-27 2016-08-04 江苏华东锂电技术研究院有限公司 Lithium iron phosphate solvothermal preparation process
US20170320738A1 (en) * 2015-01-27 2017-11-09 Jiangsu Huadong Institute of Li-Ion Battery Co., L td. Solvothermal apparatus for making lithium iron phosphate
CN108609594A (en) * 2018-03-29 2018-10-02 宁夏滨河新材料科技有限公司 The method that wastewater treatment recycles in ferric phosphate production
CN108609594B (en) * 2018-03-29 2021-08-17 宁夏滨河新材料科技有限公司 Method for treating and recycling wastewater in iron phosphate production
CN110615419A (en) * 2019-07-01 2019-12-27 湖北虹润高科新材料有限公司 Iron phosphate production facility

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