CN101837966A - Method for preparing nanometer ferric phosphate - Google Patents
Method for preparing nanometer ferric phosphate Download PDFInfo
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- CN101837966A CN101837966A CN 201010159268 CN201010159268A CN101837966A CN 101837966 A CN101837966 A CN 101837966A CN 201010159268 CN201010159268 CN 201010159268 CN 201010159268 A CN201010159268 A CN 201010159268A CN 101837966 A CN101837966 A CN 101837966A
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Abstract
The invention relates to a method for preparing nanometer ferric phosphate, and belongs to the technical field of preparing anode materials of lithium ion batteries. The method is characterized by comprising the following steps of: inputting mixed solution of one of phosphoric acid and soluble phosphate solution, one of water-soluble ferrous salt and an oxidant or water-soluble ferric salt solution and a water-solution dispersing agent, and alkali aqueous solution into a rotary packing bed at a certain feeding speed by using a metering pump; adjusting a rotary speed of the rotary packing bed; controlling a pH value of the reaction system by using the alkali solution; discharging nanometer ferric phosphate particles generated by crystallization along with the mixed solution by a discharging port of the rotary packing bed; and filtering, washing and drying the nanometer ferric phosphate particles to obtain the nanometer-grade ferric phosphate (FePO4.2H2O) powder. The method has the advantages of simple method, easy operation and high efficiency; and the ferric phosphate prepared by the method reaches the nanometer grade, the particle size is uniform, the distribution range is narrow, and the method can be applied to industrialized production. The nanometer ferric phosphate is the good precursor material for preparing anode materials (iron-lithium phosphate) of high-power lithium ion batteries.
Description
Technical field
The present invention relates to a kind of new preparation method of nano ferric phosphate, specifically relate to a kind of method of using rotating packed-bed reactor to prepare nano ferric phosphate.This nano ferric phosphate is the good persursor material of preparation superpower power type lithium-ion battery anode material ferric lithium phosphate.
Background technology
Tertiary iron phosphate is a kind of Chemicals, is widely used in fields such as pigment, pottery, foodstuff additive.Be widely used in preparing the positive pole material phosphoric acid ferripotassium of lithium ion battery in recent years.
Iron lithium phosphate (LiFePO4) is a kind of novel anode material that grew up in recent years, having advantages such as safety performance is good, have extended cycle life (more than 2000 times), starting material wide material sources (lithium, iron, phosphorus), low price, non-environmental-pollution, is the generally acknowledged power type of new generation of industry or the positive electrode material of accumulation energy type lithium ion battery first-selection.Positive electrode material is determining chemical property, security and the manufacturing cost etc. of battery to a certain extent as the important component part of kalium ion battery.
Though ferric phosphate lithium cell has advantage above-mentioned aspect many, but still there is weak point in it at aspects such as high rate during charging-discharging, low-temperature performance, energy density per unit volumes, these problems have had a strong impact on performances such as the energy density, power density of battery, have also influenced use, the processing property of battery, the too high large-scale promotion application that also is unfavorable for series of cells of the battery manufacturing cost that the material consistency problem causes.Therefore, must fundamentally solve the bottleneck problem that material exists, promptly promote the intrinsic performance of phosphoric acid ferripotassium material from aspects such as material synthesis technique, modification processing.
At present, LiFePO 4 material is the research focus of the domestic and international industry, and research property article and patent are a lot.But the enterprise that really forms scale production seldom, and the preparation technology of employing mainly is a high temperature solid-state method: select different lithium salts, molysite and P contained compound to mix, at a certain temperature high temperature sintering.Solid phase method is at potassium, iron, phosphorus ratio, aspects such as product purity, crystallization shape, granularity control acquire a certain degree of difficulty, add the difficulty of carbon dope technology and atmosphere control, the stability of different batches product is affected, and this is the common problem that runs in the present LiFePO 4 material industrialization process.Therefore, patent of the present invention is started with from the presoma tertiary iron phosphate of synthesizing iron lithium phosphate and is selected suitable operational path, addresses these problems targetedly.
Tertiary iron phosphate is one of presoma of synthesizing iron lithium phosphate, and the structure of itself and iron lithium phosphate is closely similar, as long as structure, pattern and the globule size of better controlled tertiary iron phosphate, just can control the performance of iron lithium phosphate preferably.By contrast, tertiary iron phosphate has more superiority than presomas such as the Ferrox that has now adopted, ferrous sulfate, ferric oxide.Traditional preparation method of ferric phosphate mainly contains two kinds of liquid-phase precipitation method, solid phase methods.Wherein common continuously stirring formula liquid-phase precipitation method, the iron phosphate grains that obtains is bigger, at several microns to tens microns, and broad particle distribution, be difficult to prepare the nano ferric phosphate particle.Adopt wustite and phosphatic high temperature solid-state method Composition Control difficulty, complex process, manufacturing cost height.Because the power power cell needs good heavy-current discharge performance, therefore, the preparation nano ferric phosphate just becomes the key point of preparation nano ferric phosphate potassium.
The suspension packed bed reactor is a kind ofly can realize the full blended reactor of gas-liquid-solid three-phase, is a kind of novel gas-liquid mass transfer apparatus that grows up the eighties in 20th century.Its ultimate principle is to utilize the rotary packed bed middle powerful centrifugal force-hypergravity that produces, the flow velocity of gas, liquid and the specific surface area of filler are improved and not liquid flooding greatly, liquid in high dispersive, high turbulence, by force mix and the interface rapidly more under the news with gas with great speed of relative movement reverse contact in crooked duct, greatly strengthened mass transfer process, transfer unit height has reduced by 1～2 order of magnitude, demonstrates the advantage that many legacy equipments do not possess fully.At present, rotating packed bed in preparation, oil-field flooding deoxidation, the feedwater deoxidation of nano-powder material, contain SO
2Aspect widespread uses such as flue gas desulfurization, biooxidation reactions, dedusting technology.But utilize the patent of this reactor made nano ferric phosphate and article not to appear in the newspapers.
Summary of the invention
The purpose of this invention is to provide the nano ferric phosphate preparation methods that a kind of technology is simple, with low cost, production efficiency is high.
The preparation method of a kind of nano ferric phosphate that the present invention proposes, this method prepares nano ferric phosphate with rotating packed-bed reactor, it is characterized in that, it be with phosphoric acid or soluble phosphoric acid salts solution both one of, one of water-soluble divalent iron salt and oxygenant or water-soluble trivalent ferric salt solution, mixing solutions with water soluble dispersing agent formation, and alkaline aqueous solution, above-mentioned two kinds of material solutions are mixed in storage tank respectively, two kinds of material solutions are sprayed simultaneously by opening for feed and liquid distributor with volume pump, be distributed on the protruded packing in the rotating packed bed layer, regulate phosphorous, iron, the input speed of the mixing solutions of oxygenant and dispersion agent and the rotating speed of rotating packed bed, pH value with alkaline solution control reaction feed liquid, under centrifugal action, make the quick thorough mixing of material solution, the nano ferric phosphate particle that reactive crystallization generates is discharged by the discharge port of rotating packed bed with mixed solution, after filtration, washing, operations such as drying obtain white amorphous nano-scale tertiary iron phosphate (FePO after handling
42H
2O) powder;
Described rotating packed bed comprises around a centre gangway district in axle center and centers on the annular fill area of this central area, this annular fill area is fixed with weighting material, and should the annular fill area and this centre gangway district only be fluid communication by both interfaces, and should be fluid communication with rotating packed bed a excircle by the annular fill area by this ring packing district.This rotation fill out fair bed designed chuck can steam heating or recirculated water heating and cooling, also the section meter has been reserved inlet mouth and venting port, can be used for solution-air, gas-solid and gas-liquid-solid reaction or carries out reactive liquid solution and liquid-solid reaction under protective atmosphere;
Described phosphorus source is phosphoric acid or soluble phosphate, as phosphoric acid, primary ammonium phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate etc.;
Described source of iron is water-soluble divalent iron salt or trivalent iron salt, as Iron nitrate, ferrous sulfate, iron protochloride, iron nitrate, ferric sulfate, iron(ic) chloride, ironic acetate etc.; The used oxygenant of described divalent iron salt is a hydrogen peroxide;
Described water soluble dispersing agent is sodium laurylsulfonate, sodium lauryl sulphate, polyoxyethylene glycol, polyvinyl alcohol etc.
Described alkaline aqueous solution is the aqueous solution such as sodium hydroxide, potassium hydroxide and the ammoniacal liquor etc. of metal hydroxides.
In aforesaid method, the concentration of described phosphoric acid or soluble phosphoric acid salts solution is 0.10-2.0molL
-1, the concentration of water-soluble divalent iron salt or ferric salt solution is 0.10-2.0molL
-1
In aforesaid method, the quality of the water soluble dispersing agent that adds in the mixing solutions of described every liter of phosphoric acid or soluble phosphoric acid salts solution and water-soluble divalent iron salt or trivalent iron salt is 0.00-0.1g.
In aforesaid method, the concentration of the used oxidants hydrogen peroxide aqueous solution of described water-soluble divalent iron salt is 0.15-3.00molL
-1
In aforesaid method, the concentration of described alkaline aqueous solution is 0.20-8.0molL
-1, inlet amount is standard between 1.6-6.0 with control pH.
In aforesaid method, the rotating speed of described rotating packed bed is controlled between the 500-3000rpm.
In aforesaid method, the input speed of described phosphoric acid or soluble phosphoric acid salts solution is at 0.10-2.00Lmin
-1Between.
In aforesaid method, described temperature of reaction is controlled between 15-80 ℃.
In aforesaid method, the nano ferric phosphate (FePO that described rotating packed bed reaction generates
42H
2O), white amorphous powder, granularity is between 10-100nm.
Compared with prior art, the present invention has novel part:
1. use rotating packed-bed reactor, equipment is simple, volume is little, low-temperature atmosphere-pressure reaction, energy consumption are little, and therefore, preparation cost is low.
2. technology is simple, easy to operate, production efficiency is high, and general traditional liquid-phase precipitation needs the reaction that finish in several hours to tens hours, adopts this reactor several seconds just can finish to several minutes.In addition, the present invention used raw materials used all be Chemicals common, cheap and easy to get, reaction process does not have side reaction to take place and does not produce hazardous and noxious substances, environmental friendliness.
3. the nano ferric phosphate composition for preparing is stable, globule size is even, particle size distribution is narrow.
Description of drawings
Fig. 1 rotating packed bed synoptic diagram.
Fig. 2 is the X-ray diffracting spectrum of the prepared nano ferric phosphate of embodiment five.
Fig. 3 is the TEM image of the nano ferric phosphate of example five preparations.
Embodiment
Embodiment one
The rotating speed of regulating rotating packed bed is 500rmin
-1, with 0.1molL
-1The mixing solutions of iron nitrate and phosphoric acid is with 0.1Lmin
-1Speed be input in the rotating packed bed by volume pump, import 0.20molL with volume pump simultaneously
-1Ammonia soln with control reaction system the pH value be 1.70,60 ℃ of temperature of reaction, material solution is quick thorough mixing under big centrifugal action, reactive crystallization generates the nano ferric phosphate particle, reacted mixed solution is discharged by the discharge port of rotating packed bed, after filtration, postprocessing working procedures such as washing, drying obtain the nano level tertiary iron phosphate.
Embodiment two
The rotating speed of regulating rotating packed bed is 2000rmin
-1, with 0.5molL
-1Ferric sulfate and SODIUM PHOSPHATE, MONOBASIC and 0.05gL
-1The mixing solutions of sodium laurylsulfonate with 0.2Lmin
-1Speed be input in the rotating packed bed by volume pump, import 2.0molL with volume pump simultaneously
-1Sodium hydroxide solution with control reaction system the pH value be 3.00,15 ℃ of temperature of reaction, material solution is quick thorough mixing under big centrifugal action, reactive crystallization generates the nano ferric phosphate particle, reacted mixed solution is discharged by the discharge port of rotating packed bed, after filtration, postprocessing working procedures such as washing, drying obtain the nano level tertiary iron phosphate.
Embodiment three
The rotating speed of regulating rotating packed bed is 1500rmin
-1, with 1.0molL
-1Ironic acetate and phosphoric acid 0.1gL
-1Polyoxyethylene glycol mixing solutions and with 1.0Lmin
-1Speed be input in the rotating packed bed by volume pump, import 2.0molL with volume pump simultaneously
-1Potassium hydroxide solution with control reaction system the pH value be 6.00,45 ℃ of temperature of reaction, material solution is quick thorough mixing under big centrifugal action, reactive crystallization generates the nano ferric phosphate particle, reacted mixed solution is discharged by the discharge port of rotating packed bed, after filtration, postprocessing working procedures such as washing, drying obtain the nano level tertiary iron phosphate.
Embodiment four
The rotating speed of regulating rotating packed bed is 1000rmin
-1, with 2.0molL
-1Iron(ic) chloride and ammonium di-hydrogen phosphate and 0.01gL
-1The mixing solutions of sodium lauryl sulphate with 2.0Lmin
-1Speed be input to simultaneously in the rotating packed bed by volume pump, import 4.0molL with volume pump simultaneously
-1Ammonia soln with control reaction system the pH value be 3.60,30 ℃ of temperature of reaction, material solution is quick thorough mixing under big centrifugal action, reactive crystallization generates the nano ferric phosphate particle, reacted mixed solution is discharged by the discharge port of rotating packed bed, after filtration, postprocessing working procedures such as washing, drying obtain the nano level tertiary iron phosphate.
Embodiment five
The rotating speed of regulating rotating packed bed is 3000rmin
-1, with 1.0molL
-1Iron nitrate and potassium primary phosphate and 0.05gL
-1The mixing solutions of polyvinyl alcohol with 0.5Lmin
-1Speed be input to simultaneously in the rotating packed bed by volume pump, import 2.2molL with volume pump simultaneously
-1Ammonia soln with control reaction system the pH value be 2.30, temperature of reaction is 80 ℃, material solution is quick thorough mixing under big centrifugal action, reactive crystallization generates the nano ferric phosphate particle, reacted mixed solution is discharged by the discharge port of rotating packed bed, after filtration, postprocessing working procedures such as washing, drying obtain the nano level tertiary iron phosphate.
Embodiment six
The rotating speed of regulating rotating packed bed is 2500rmin
-1, with 0.1molL
-1The mixing solutions of Iron nitrate and phosphoric acid and 0.15molL
-1Aqueous hydrogen peroxide solution with 1.0Lmin
-1Speed be input in the rotating packed bed by volume pump, use 8molL
-1It is 5.60 that ammoniacal liquor is regulated the pH value, temperature of reaction is 50 ℃, material solution is quick thorough mixing under big centrifugal action, reactive crystallization generates the nano ferric phosphate particle, reacted mixed solution is discharged by the discharge port of rotating packed bed, after filtration, postprocessing working procedures such as washing, drying obtain the nano level tertiary iron phosphate.
Embodiment seven
The rotating speed of regulating rotating packed bed is 500rmin
-1, with 1.0molL
-1The mixing solutions of ferrous sulfate and phosphoric acid and 1.50molL
-1Aqueous hydrogen peroxide solution with 0.5Lmin
-1Speed be input in the rotating packed bed by volume pump, use 2.0molL
-1It is 1.60 that ammoniacal liquor is regulated the pH value, temperature of reaction is 20 ℃, material solution is quick thorough mixing under big centrifugal action, reactive crystallization generates the nano ferric phosphate particle, reacted mixed solution is discharged by the discharge port of rotating packed bed, after filtration, postprocessing working procedures such as washing, drying obtain the nano level tertiary iron phosphate.
Embodiment eight
The rotating speed of regulating rotating packed bed is 3000rmin
-1, with 0.5molL
-1The mixing solutions of iron protochloride and SODIUM PHOSPHATE, MONOBASIC and 0.75molL
-1Aqueous hydrogen peroxide solution with 2.0Lmin
-1Speed be input in the rotating packed bed by volume pump, use 3.0molL
-1It is 2.20 that ammoniacal liquor is regulated the pH value, temperature of reaction is 80 ℃, material solution is quick thorough mixing under big centrifugal action, reactive crystallization generates the nano ferric phosphate particle, reacted mixed solution is discharged by the discharge port of rotating packed bed, after filtration, postprocessing working procedures such as washing, drying obtain the nano level tertiary iron phosphate.
Embodiment nine
The rotating speed of regulating rotating packed bed is 1800rmin
-1, with 0.5molL
-1The mixing solutions of Iron nitrate and ammonium di-hydrogen phosphate and 0.75molL
-1Aqueous hydrogen peroxide solution with 0.1Lmin
-1Speed be input in the rotating packed bed by volume pump, use 5.0molL
-1It is 4.20 that ammoniacal liquor is regulated the pH value, temperature of reaction is 40 ℃, material solution is quick thorough mixing under big centrifugal action, reactive crystallization generates the nano ferric phosphate particle, reacted mixed solution is discharged by the discharge port of rotating packed bed, after filtration, postprocessing working procedures such as washing, drying obtain the nano level tertiary iron phosphate.
Embodiment ten
The rotating speed of regulating rotating packed bed is 1000rmin
-1, with 2.0molL
-1The mixing solutions of iron protochloride and phosphoric acid with and 3.0molL
-1Aqueous hydrogen peroxide solution with 1.5Lmin
-1Speed be input in the rotating packed bed by volume pump, use 6.0molL
-1It is 3.50 that ammoniacal liquor is regulated the pH value, temperature of reaction is 60 ℃, material solution is quick thorough mixing under big centrifugal action, reactive crystallization generates the nano ferric phosphate particle, reacted mixed solution is discharged by the discharge port of rotating packed bed, after filtration, postprocessing working procedures such as washing, drying obtain the nano level tertiary iron phosphate.
Claims (9)
1. the preparation method of a nano ferric phosphate, this method prepares nano ferric phosphate with rotating packed-bed reactor, it is characterized in that, it be with phosphoric acid or soluble phosphoric acid salts solution both one of, one of water-soluble divalent iron salt and oxygenant or water-soluble trivalent ferric salt solution, mixing solutions with water soluble dispersing agent formation, and alkaline aqueous solution, above-mentioned two kinds of material solutions are mixed in storage tank respectively, two kinds of material solutions are sprayed simultaneously by opening for feed and liquid distributor with volume pump, be distributed on the protruded packing in the rotating packed bed layer, regulate phosphorous, iron, the input speed of the mixing solutions of oxygenant and dispersion agent and the rotating speed of rotating packed bed, pH value with alkaline solution control reaction feed liquid, under centrifugal action, make the quick thorough mixing of material solution, the nano ferric phosphate particle that reactive crystallization generates is discharged by the discharge port of rotating packed bed with mixed solution, after filtration, washing, operations such as drying obtain white amorphous nano-scale tertiary iron phosphate (FePO after handling
42H
2O) powder;
Described rotating packed bed comprises around a centre gangway district in axle center and centers on the annular fill area of this central area, this annular fill area is fixed with weighting material, and should the annular fill area and this centre gangway district only be fluid communication by both interfaces, and should be fluid communication with rotating packed bed a excircle by the annular fill area by this ring packing district.This rotating packed bed has designed chuck can steam heating or recirculated water heating and cooling, and also inlet mouth and venting port have been reserved in design, can be used for solution-air, gas-solid and gas-liquid-solid reaction or carry out reactive liquid solution and liquid-solid reaction under protective atmosphere;
Described phosphorus source is phosphoric acid or soluble phosphate, as phosphoric acid, primary ammonium phosphate, SODIUM PHOSPHATE, MONOBASIC, phosphoric acid dioxy potassium etc.;
Described source of iron is water-soluble divalent iron salt or trivalent iron salt, as Iron nitrate, ferrous sulfate, iron protochloride, iron nitrate, ferric sulfate, iron(ic) chloride, ironic acetate etc.; The used oxygenant of described divalent iron salt is a hydrogen peroxide;
Described water soluble dispersing agent is sodium laurylsulfonate, sodium lauryl sulphate, polyoxyethylene glycol, polyvinyl alcohol etc.
Described alkaline aqueous solution is the aqueous solution such as oxygen sodium oxide, potassium hydroxide and the ammoniacal liquor etc. of metal hydroxides.
2. the method for claim 1 is characterized in that, the concentration of described phosphoric acid or soluble phosphoric acid salts solution is 0.10-2.0molL
-1, the concentration of water-soluble divalent iron salt or ferric salt solution is 0.10-2.0molL
-1
3. method as claimed in claim 1 or 2 is characterized in that, the quality of the water soluble dispersing agent that adds in the mixing solutions of described every liter of phosphoric acid or soluble phosphoric acid salts solution and water-soluble divalent iron salt or trivalent iron salt is 0.00-0.1g.
4. as claim 1 or 2 or 3 described methods, it is characterized in that the concentration of the used oxidants hydrogen peroxide aqueous solution of described water-soluble divalent iron salt is 0.15-3.00molL
-1
5. the method for claim 1 is characterized in that, the concentration of described alkaline aqueous solution is 0.20-8.0molL
-1, inlet amount is standard between 1.6-6.0 with control pH.
6. the method for claim 1 is characterized in that, the rotating speed of described rotating packed bed is controlled between the 500-3000rpm.
7. the method for claim 1 is characterized in that, the input speed of described phosphoric acid or soluble phosphoric acid salts solution is at 0.10-2.00Lmin
-1Between.
8. the method for claim 1 is characterized in that, described temperature of reaction is controlled between 15-80 ℃.
9. the method for claim 1 is characterized in that, the nano ferric phosphate (FePO that described rotating packed bed reaction generates
42H
2O), white amorphous powder, granularity is between 10-100nm.
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|---|---|---|---|
| CN2010101592681A CN101837966B (en) | 2009-10-16 | 2010-04-29 | Method for preparing nanometer ferric phosphate |
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|---|---|---|---|
| CN200910093734.8 | 2009-10-16 | ||
| CN200910093734A CN101693531A (en) | 2009-10-16 | 2009-10-16 | Method for preparing nano iron phosphate |
| CN200910235404.8 | 2009-10-23 | ||
| CN200910235404A CN101695998A (en) | 2009-10-23 | 2009-10-23 | Method for preparing nano ferric phosphate |
| CN2010101592681A CN101837966B (en) | 2009-10-16 | 2010-04-29 | Method for preparing nanometer ferric phosphate |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120569A (en) * | 2011-01-31 | 2011-07-13 | 李宝峰 | Preparation method of ferric phosphate |
| CN102709556A (en) * | 2012-06-04 | 2012-10-03 | 清华大学 | Spherical ultrafine iron phosphate preparation method |
| CN107098325A (en) * | 2016-02-23 | 2017-08-29 | 河南博之捷环保科技有限公司 | A kind of ferric phosphate preparation method with controllability |
| CN108439361A (en) * | 2018-04-09 | 2018-08-24 | 杭州电子科技大学 | A kind of preparation method of spherical nano ferric phosphate |
| CN111268663A (en) * | 2020-01-19 | 2020-06-12 | 江苏乐能电池股份有限公司 | Preparation method of high-compaction iron phosphate particles |
| CN111377426A (en) * | 2020-03-05 | 2020-07-07 | 黄冈林立新能源科技有限公司 | Preparation method of anhydrous iron phosphate nanoparticles |
| CN115432689A (en) * | 2022-09-30 | 2022-12-06 | 福建紫金锂元材料科技有限公司 | Preparation method of high-performance long-life lithium iron phosphate cathode material |
| CN116161636A (en) * | 2023-02-20 | 2023-05-26 | 湖北锂宝新材料科技发展有限公司 | Method for preparing battery-grade anhydrous ferric phosphate from lithium-extracted ferric phosphate waste residues |
| CN117534050A (en) * | 2023-12-25 | 2024-02-09 | 广东惠云钛业股份有限公司 | Ferric phosphate with small and uniform particle size and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1635648A (en) * | 2004-12-30 | 2005-07-06 | 清华大学 | Method for preparing high-density spherical ferric lithium phosphate as anode material of lithium-ion battery |
| CN101222044A (en) * | 2007-12-06 | 2008-07-16 | 南开大学 | Novel conductive agent doping/coating lithium iron phosphate material and its production method |
| CN101337666A (en) * | 2008-08-04 | 2009-01-07 | 清华大学 | Method for preparing spherical ferric lithium phosphate by oxidation control crystal-carbon thermal reduction method |
-
2010
- 2010-04-29 CN CN2010101592681A patent/CN101837966B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1635648A (en) * | 2004-12-30 | 2005-07-06 | 清华大学 | Method for preparing high-density spherical ferric lithium phosphate as anode material of lithium-ion battery |
| CN101222044A (en) * | 2007-12-06 | 2008-07-16 | 南开大学 | Novel conductive agent doping/coating lithium iron phosphate material and its production method |
| CN101337666A (en) * | 2008-08-04 | 2009-01-07 | 清华大学 | Method for preparing spherical ferric lithium phosphate by oxidation control crystal-carbon thermal reduction method |
Non-Patent Citations (3)
| Title |
|---|
| 《化学工业与工程技术》 20060630 李艳等 超重力法制备纳米材料的研究现状 第3.5、3.6节 1-9 第27卷, 第3期 2 * |
| 《北京化工大学学报》 20031231 刘方涛等 超重力反应沉淀法（HGRP）制备纳米BaTiO3的研究 第2.4节 1-9 第30卷, 第1期 2 * |
| 《山西化工》 20020228 李军平 纳米硫酸钡粒子超重力法制备及其表征 第1.1节 1-9 第22卷, 第1期 2 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102120569A (en) * | 2011-01-31 | 2011-07-13 | 李宝峰 | Preparation method of ferric phosphate |
| CN102709556A (en) * | 2012-06-04 | 2012-10-03 | 清华大学 | Spherical ultrafine iron phosphate preparation method |
| CN102709556B (en) * | 2012-06-04 | 2014-06-18 | 清华大学 | Spherical ultrafine iron phosphate preparation method |
| CN107098325A (en) * | 2016-02-23 | 2017-08-29 | 河南博之捷环保科技有限公司 | A kind of ferric phosphate preparation method with controllability |
| CN107098325B (en) * | 2016-02-23 | 2019-02-05 | 河南博之捷环保科技有限公司 | A kind of ferric phosphate preparation method with controllability |
| CN108439361A (en) * | 2018-04-09 | 2018-08-24 | 杭州电子科技大学 | A kind of preparation method of spherical nano ferric phosphate |
| CN111268663A (en) * | 2020-01-19 | 2020-06-12 | 江苏乐能电池股份有限公司 | Preparation method of high-compaction iron phosphate particles |
| CN111377426A (en) * | 2020-03-05 | 2020-07-07 | 黄冈林立新能源科技有限公司 | Preparation method of anhydrous iron phosphate nanoparticles |
| CN115432689A (en) * | 2022-09-30 | 2022-12-06 | 福建紫金锂元材料科技有限公司 | Preparation method of high-performance long-life lithium iron phosphate cathode material |
| CN116161636A (en) * | 2023-02-20 | 2023-05-26 | 湖北锂宝新材料科技发展有限公司 | Method for preparing battery-grade anhydrous ferric phosphate from lithium-extracted ferric phosphate waste residues |
| CN116161636B (en) * | 2023-02-20 | 2024-04-05 | 湖北锂宝新材料科技发展有限公司 | Method for preparing battery-grade anhydrous ferric phosphate from lithium-extracted ferric phosphate waste residues |
| CN117534050A (en) * | 2023-12-25 | 2024-02-09 | 广东惠云钛业股份有限公司 | Ferric phosphate with small and uniform particle size and preparation method thereof |
| CN117534050B (en) * | 2023-12-25 | 2024-04-30 | 广东惠云钛业股份有限公司 | Ferric phosphate with small and uniform particle size and preparation method thereof |
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