CN112607722A - Preparation method of high-compaction-density iron phosphate - Google Patents
Preparation method of high-compaction-density iron phosphate Download PDFInfo
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- CN112607722A CN112607722A CN202011376957.8A CN202011376957A CN112607722A CN 112607722 A CN112607722 A CN 112607722A CN 202011376957 A CN202011376957 A CN 202011376957A CN 112607722 A CN112607722 A CN 112607722A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- 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
- C01P2006/12—Surface area
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method of iron phosphate with high compaction density. The preparation method comprises the following steps: s1, adding an iron source and a phosphorus source into a reaction container, then adding a proper amount of water, heating under continuous stirring, reacting at 70-98 ℃ for 0.5-2h, and filtering to obtain a ferrous phosphate mother liquor; s2, adding a hydrogen peroxide solution into the product obtained in the step S1, continuously stirring and heating, reacting at 40-60 ℃ for 1-4h, and filtering to obtain a crude iron phosphate product; s3, washing the ferrous sulfate crude product in ethanol, and washing and filtering to obtain an iron phosphate precipitate; and S4, drying, calcining and cooling the iron phosphate precipitate, and then carrying out air flow crushing and screening to remove iron to obtain the high-compaction-density iron phosphate. The preparation method of the high-compaction-density iron phosphate has simple process, and can obtain the high-compaction-density iron phosphate which has small primary particle size, large BET (BET) and small adhesion among primary particles in agglomerated particles and is easy to grind.
Description
Technical Field
The invention relates to the field of new energy materials, and in particular relates to a preparation method of high-compaction-density iron phosphate.
Background
With the continuous progress of human society and the continuous development of scientific technology, energy problems become one of the first problems of the current society. The lithium ion battery is a new generation of green high-energy battery, has the advantages of high voltage, large energy density, good cycle performance, small self-discharge, no memory effect, wide working temperature range and the like, is widely applied to mobile phones, notebook computers, digital cameras, video cameras, electronic instruments and the like, and has bright application prospect in the fields of UPS, electric tools, electric bicycles, electric automobiles, energy storage batteries and the like. In recent years, the output of lithium ion batteries is rapidly increased, and the application field is continuously expanded, so that the lithium ion batteries become high-tech products which have important significance for national economy and people's life in the twenty-first century.
At present, lithium ion batteries are becoming mature in the field of small batteries for portable electronic products, and the application range is gradually expanding towards the fields of medium-high capacity and medium-high power type and energy storage type batteries. The anode material is an important component of the lithium ion battery, and the performance of the anode material determines the comprehensive performance of the battery to a great extent. Research and performance improvement of cathode materials are one of the core of the development of lithium ion batteries. Iron phosphate is often used as a raw material for manufacturing lithium iron phosphate of a lithium battery, the demand for the iron phosphate is increasing along with the application of new energy, and due to poor conductivity of the lithium iron phosphate, particles of the lithium iron phosphate need to be made as small as possible and nano, so that the conductivity can be greatly improved, the internal resistance can be reduced, and the capacity can be improved due to carbon coating. However, the lithium iron phosphate has small particles and generally has a low compaction density.
How to prepare the iron phosphate with high compaction density becomes the key for the development of the current lithium iron phosphate.
Disclosure of Invention
The invention aims to provide a preparation method of iron phosphate with high compaction density aiming at the defects of the prior art.
The invention is realized by the following technical scheme:
a preparation method of high-compaction-density iron phosphate comprises the following steps:
s1, adding the raw materials into a reaction vessel in a molar ratio of 1: 2-3 of an iron source and a phosphorus source, wherein the iron source is a mixture of iron powder and iron oxide, then a proper amount of water is added to ensure that the mass percent of iron in the system is 2% -5%, the temperature is raised under continuous stirring, the mixture reacts for 0.5-2h at 70-98 ℃, and a ferrous phosphate mother liquor is obtained after filtration;
s2, adding a hydrogen peroxide solution into the product obtained in the step S1, continuously stirring and heating, reacting at 40-60 ℃ for 1-4h, and filtering to obtain a crude iron phosphate product;
s3, washing the ferrous sulfate crude product in ethanol, and washing and filtering to obtain an iron phosphate precipitate;
and S4, drying, calcining and cooling the iron phosphate precipitate, and then carrying out air flow crushing and screening to remove iron to obtain the high-compaction-density iron phosphate.
Preferably, the iron content in the iron powder in the step S1 is 99.0% -99.9%.
Preferably, the phosphorus source in step S1 is a phosphoric acid solution.
Preferably, the mass ratio of the iron powder to the iron oxide in the step S1 is 10-40: 1.
Preferably, in the step S4, the drying temperature is 100 to 120 ℃, and the drying time is 3 to 5 hours.
Preferably, in the step S4, the calcining temperature is 800-1000 ℃, and the calcining time is 6-8 h.
Preferably, in the step S4, the pulverization is stopped after the air stream pulverization to 1 to 10 μm of the particles.
The preparation method of the high-compaction-density iron phosphate has simple process, and can obtain the high-compaction-density iron phosphate which has small primary particle size, large BET (BET) and small adhesion among primary particles in agglomerated particles and is easy to grind.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A preparation method of high-compaction-density iron phosphate comprises the following steps:
s1, adding the raw materials into a reaction vessel in a molar ratio of 1: 2, wherein the iron source is a mixture of iron powder and iron oxide, and the mass ratio of the iron powder to the iron oxide is 10: 1; then adding a proper amount of water to ensure that the mass percent content of iron in the system is 2%, heating while continuously stirring, reacting at 70-98 ℃ for 0.5, and filtering to obtain a ferrous phosphate mother liquor;
s2, adding a hydrogen peroxide solution into the product obtained in the step S1, continuously stirring and heating, reacting for 4 hours at 40 ℃, and filtering to obtain a crude iron phosphate product;
s3, washing the ferrous sulfate crude product in ethanol, and washing and filtering to obtain an iron phosphate precipitate;
s4, drying the iron phosphate precipitate at the drying temperature of 120 ℃ for 3 h; calcining the dried iron phosphate at 800 ℃ for 8 h; after cooling, the mixture is pulverized into particles with the particle size of 1-10 mu m by air flow, and the pulverization is stopped to obtain the high-compaction-density iron phosphate.
Example 2
A preparation method of high-compaction-density iron phosphate comprises the following steps:
s1, adding the raw materials into a reaction vessel in a molar ratio of 1: 2, wherein the iron source is a mixture of iron powder and iron oxide, and the mass ratio of the iron powder to the iron oxide is 10: 1; then adding a proper amount of water to ensure that the mass percent content of iron in the system is 2%, heating while continuously stirring, reacting at 70-98 ℃ for 0.5, and filtering to obtain a ferrous phosphate mother liquor;
s2, adding a hydrogen peroxide solution into the product obtained in the step S1, continuously stirring and heating, reacting at 60 ℃ for 1h, and filtering to obtain a crude iron phosphate product;
s3, washing the ferrous sulfate crude product in ethanol, and washing and filtering to obtain an iron phosphate precipitate;
s4, drying the iron phosphate precipitate at 100 ℃ for 5 h; calcining the dried iron phosphate at 1000 ℃ for 6 h; after cooling, the mixture is pulverized into particles with the particle size of 1-10 mu m by air flow, and the pulverization is stopped to obtain the high-compaction-density iron phosphate.
Example 3
A preparation method of high-compaction-density iron phosphate comprises the following steps:
s1, adding the raw materials into a reaction vessel in a molar ratio of 1: 2, wherein the iron source is a mixture of iron powder and iron oxide, and the mass ratio of the iron powder to the iron oxide is 10: 1; then adding a proper amount of water to ensure that the mass percent content of iron in the system is 2%, heating while continuously stirring, reacting at 70-98 ℃ for 0.5, and filtering to obtain a ferrous phosphate mother liquor;
s2, adding a hydrogen peroxide solution into the product obtained in the step S1, continuously stirring and heating, reacting for 3 hours at 50 ℃, and filtering to obtain a crude iron phosphate product;
s3, washing the ferrous sulfate crude product in ethanol, and washing and filtering to obtain an iron phosphate precipitate;
s4, drying the iron phosphate precipitate at the drying temperature of 110 ℃ for 4 h; calcining the dried iron phosphate at 900 ℃ for 7 h; after cooling, the mixture is pulverized into particles with the particle size of 1-10 mu m by air flow, and the pulverization is stopped to obtain the high-compaction-density iron phosphate.
Example 4
A preparation method of high-compaction-density iron phosphate comprises the following steps:
s1, adding the raw materials into a reaction vessel in a molar ratio of 1: 2, wherein the iron source is a mixture of iron powder and iron oxide, and the mass ratio of the iron powder to the iron oxide is 10: 1; then adding a proper amount of water to ensure that the mass percent content of iron in the system is 2%, heating while continuously stirring, reacting at 70-98 ℃ for 0.5, and filtering to obtain a ferrous phosphate mother liquor;
s2, adding a hydrogen peroxide solution into the product obtained in the step S1, continuously stirring and heating, reacting at 45 ℃ for 2.5 hours, and filtering to obtain a crude iron phosphate product;
s3, washing the ferrous sulfate crude product in ethanol, and washing and filtering to obtain an iron phosphate precipitate;
s4, drying the iron phosphate precipitate at 105 ℃ for 4.5 h; calcining the dried iron phosphate at 850 ℃ for 6.5 h; after cooling, the mixture is pulverized into particles with the particle size of 1-10 mu m by air flow, and the pulverization is stopped to obtain the high-compaction-density iron phosphate.
Example 5
A preparation method of high-compaction-density iron phosphate comprises the following steps:
s1, adding the raw materials into a reaction vessel in a molar ratio of 1: 2, wherein the iron source is a mixture of iron powder and iron oxide, and the mass ratio of the iron powder to the iron oxide is 10: 1; then adding a proper amount of water to ensure that the mass percent content of iron in the system is 2%, heating while continuously stirring, reacting at 70-98 ℃ for 0.5, and filtering to obtain a ferrous phosphate mother liquor;
s2, adding a hydrogen peroxide solution into the product obtained in the step S1, continuously stirring and heating, reacting at 55 ℃ for 2.8 hours, and filtering to obtain a crude iron phosphate product;
s3, washing the ferrous sulfate crude product in ethanol, and washing and filtering to obtain an iron phosphate precipitate;
s4, drying the iron phosphate precipitate at 115 ℃ for 3.5 h; calcining the dried iron phosphate at 950 ℃ for 6.5 h; after cooling, the mixture is pulverized into particles with the particle size of 1-10 mu m by air flow, and the pulverization is stopped to obtain the high-compaction-density iron phosphate.
The high compaction density iron phosphates prepared in examples 1 to 5 were respectively subjected to performance testing, and the test results were as follows:
through detection, the iron phosphate prepared by the invention has high compaction density, and the electrochemical performance of the prepared lithium iron phosphate is excellent.
It should be understood that the examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that any changes and modifications to the present invention may occur to those skilled in the art after reading the present teachings, and such equivalents are also intended to be limited by the appended claims.
Claims (7)
1. A preparation method of high-compaction-density iron phosphate comprises the following steps:
s1, adding the raw materials into a reaction vessel in a molar ratio of 1: 2-3 of an iron source and a phosphorus source, wherein the iron source is a mixture of iron powder and iron oxide, then a proper amount of water is added to ensure that the mass percent of iron in the system is 2% -5%, the temperature is raised under continuous stirring, the mixture reacts for 0.5-2h at 70-98 ℃, and a ferrous phosphate mother liquor is obtained after filtration;
s2, adding a hydrogen peroxide solution into the product obtained in the step S1, continuously stirring and heating, reacting at 40-60 ℃ for 1-4h, and filtering to obtain a crude iron phosphate product;
s3, washing the ferrous sulfate crude product in ethanol, and washing and filtering to obtain an iron phosphate precipitate;
and S4, drying, calcining and cooling the iron phosphate precipitate, and then carrying out air flow crushing and screening to remove iron to obtain the high-compaction-density iron phosphate.
2. The method for preparing iron phosphate with high compaction density according to claim 1, wherein the iron content in the iron powder in the step S1 is 99.0% -99.9%.
3. The method for preparing high compacted density iron phosphate according to claim 1, wherein the phosphorus source in step S1 is a phosphoric acid solution.
4. The method for preparing high compacted density iron phosphate according to claim 1, wherein the mass ratio of iron powder to iron oxide in step S1 is 10-40: 1.
5. The method for preparing high-compaction-density iron phosphate according to claim 1, wherein in the step S4, the drying temperature is 100-120 ℃ and the drying time is 3-5 h.
6. The method for preparing high-compaction-density iron phosphate according to any one of claims 1 to 5, wherein in the step S4, the calcining temperature is 800-1000 ℃ and the calcining time is 6-8 h.
7. The method for preparing high-compaction-density iron phosphate according to claim 6, wherein the step S4 is characterized in that the airflow pulverization is stopped after the pulverization is carried out to 1-10 μm of particles.
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| CN202011376957.8A CN112607722A (en) | 2020-11-30 | 2020-11-30 | Preparation method of high-compaction-density iron phosphate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113845100A (en) * | 2021-11-16 | 2021-12-28 | 湖北融通高科先进材料有限公司 | Iron phosphate and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113845100A (en) * | 2021-11-16 | 2021-12-28 | 湖北融通高科先进材料有限公司 | Iron phosphate and preparation method and application thereof |
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