CN117865105A - Demagnetizing method of lithium iron phosphate material - Google Patents
Demagnetizing method of lithium iron phosphate material Download PDFInfo
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- CN117865105A CN117865105A CN202410050615.9A CN202410050615A CN117865105A CN 117865105 A CN117865105 A CN 117865105A CN 202410050615 A CN202410050615 A CN 202410050615A CN 117865105 A CN117865105 A CN 117865105A
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- CN
- China
- Prior art keywords
- iron phosphate
- lithium iron
- phosphate material
- demagnetizing
- sintering
- 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.)
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 57
- 239000000463 material Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000005245 sintering Methods 0.000 claims abstract description 22
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 18
- 239000011574 phosphorus Substances 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 230000001502 supplementing effect Effects 0.000 claims abstract description 17
- 239000012046 mixed solvent Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- VAKIVKMUBMZANL-UHFFFAOYSA-N iron phosphide Chemical compound P.[Fe].[Fe].[Fe] VAKIVKMUBMZANL-UHFFFAOYSA-N 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 4
- 239000004254 Ammonium phosphate Substances 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 3
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 3
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000398 iron phosphate Inorganic materials 0.000 claims 2
- 239000013589 supplement Substances 0.000 claims 1
- 230000005347 demagnetization Effects 0.000 abstract description 8
- 238000009776 industrial production Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 7
- 230000005389 magnetism Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 238000007689 inspection Methods 0.000 description 3
- 230000002950 deficient Effects 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000005955 Ferric phosphate Substances 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229940032958 ferric phosphate Drugs 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- DPTATFGPDCLUTF-UHFFFAOYSA-N phosphanylidyneiron Chemical compound [Fe]#P DPTATFGPDCLUTF-UHFFFAOYSA-N 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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 demagnetization method of a lithium iron phosphate material, which comprises the following steps: uniformly mixing the phosphorus supplementing agent and the solvent according to a certain proportion to obtain a mixed solvent; soaking a lithium iron phosphate material to be demagnetized with a mixed solvent according to a certain proportion to obtain a mixed intermediate; and sintering and crushing the mixed intermediate to obtain the demagnetized lithium iron phosphate material. The demagnetizing effect is good. The process flow is easy to control, has low requirements on equipment, and is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a demagnetization method of a lithium iron phosphate material.
Background
As a representative of the secondary battery with the highest comprehensive performance, commercialization of lithium ion batteries can be traced back to the 90 th century of 20 th century, and through many years of research, lithium iron phosphate batteries occupy a large part of market share by virtue of high energy density, better safety performance and long cycle life. The synthesis process of lithium iron phosphate is most mature by a high-temperature solid phase method, wherein the content of magnetic substances in the product also fluctuates greatly due to the influences of adverse factors such as raw material quality, unstable manufacturing process, uneven kiln heating and the like, and the main content of the magnetic substances is iron phosphide, so that the yield of the finished product is greatly reduced.
At present, the main stream treatment method of the defective lithium iron phosphate positive electrode material with high magnetic substance content is to recycle, and the comprehensive process of wet leaching, oxidation separation, evaporation crystallization, carbonization and purification is adopted to obtain the battery-grade ferric phosphate and lithium carbonate. The whole treatment process has higher difficulty, low recovery rate and serious resource waste.
Disclosure of Invention
In view of the above, the present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides a demagnetization method of a lithium iron phosphate material. The lithium iron phosphate material treated by the demagnetizing method provided by the invention has good purifying effect on the lithium iron phosphate material, and the demagnetizing method of the lithium iron phosphate material has low process equipment requirements and is easy to implement and suitable for large-scale industrial production.
Therefore, the embodiment of the invention provides a demagnetization method of a lithium iron phosphate material, which comprises the following steps:
s10, uniformly mixing the phosphorus supplementing agent and the solvent according to a certain proportion to obtain a mixed solvent;
s20, soaking the lithium iron phosphate material to be demagnetized with the mixed solvent according to a certain proportion to obtain a mixed intermediate;
s30, sintering and crushing the mixed intermediate to obtain the demagnetized lithium iron phosphate material.
Preferably, the lithium iron phosphate material to be demagnetized includes iron phosphide impurities.
Preferably, the mixing intermediate is formulated in a graphite sagger.
Preferably, the phosphorus supplementing agent comprises at least one of sodium phosphate, ammonium phosphate and phosphoric acid.
Preferably, the adding amount of the phosphorus supplementing agent accounts for 0.1-5 per mill of the mass ratio of the lithium iron phosphate material to be demagnetized.
Preferably, the solvent comprises at least one of water, ethanol, propanol, acetone, ethylene glycol.
Preferably, the input amount of the solvent accounts for 10-100% of the mass ratio of the lithium iron phosphate material to be demagnetized.
Preferably, the sintering temperature is 450-750 ℃ and the sintering time is 8-12 h.
Preferably, the sintering is performed under an inert atmosphere.
Preferably, the oxygen content in the sintering atmosphere is between 0.1ppm and 10ppm.
According to the method for removing the magnetism of the lithium iron phosphate material, disclosed by the embodiment of the invention, the phosphorus supplementing agent and the solvent are added to be mixed with the lithium iron phosphate material to be removed, and the mixed intermediate is subjected to high-temperature sintering and crushing after being mixed, so that the lithium iron phosphate material with the magnetism removed can be obtained, and the electrochemical performance requirement is met. The demagnetizing method has simple process flow and low equipment requirement, and is suitable for large-scale industrial production.
Drawings
Fig. 1 is a flowchart of a method for demagnetizing a lithium iron phosphate material according to an embodiment of the present invention.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below with reference to the drawings are exemplary and intended to illustrate the invention and should not be construed as limiting the invention.
The following disclosure provides many different embodiments, or examples, for implementing different structures of the invention. In order to simplify the present disclosure, components and arrangements of specific examples are described below. They are, of course, merely examples and are not intended to limit the invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples. This repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art will recognize the applicability of other processes and/or the use of other materials.
Referring to fig. 1, an embodiment of the present invention provides a method for removing magnetism of a lithium iron phosphate material, wherein the method is performed on a defective product of a high-magnetism lithium iron phosphate material in lithium iron phosphate production, the high-magnetism lithium iron phosphate material cannot meet a battery performance requirement, and the lithium iron phosphate material subjected to the removal magnetism treatment of the present invention can meet the requirement.
The demagnetizing method comprises the following steps:
s10, uniformly mixing the phosphorus supplementing agent and the solvent according to a certain proportion to obtain a mixed solvent;
s20, soaking the lithium iron phosphate material to be demagnetized with the mixed solvent according to a certain proportion to obtain a mixed intermediate;
s30, sintering and crushing the mixed intermediate to obtain the demagnetized lithium iron phosphate material.
The step S10 specifically comprises the steps of pumping a certain amount of solvent into a dispensing tank, and starting stirring; and adding a certain amount of phosphorus supplementing agent into the dispensing tank, and fully stirring until the phosphorus supplementing agent is completely dissolved to obtain the mixed solvent.
The step S20 specifically comprises the steps of adding a certain amount of prepared mixed solvent into a graphite sagger, adding a certain amount of unqualified lithium iron phosphate anode material into the graphite sagger, stirring until the black powder is completely soaked, and completing mixing to obtain the mixed intermediate.
Further, the lithium iron phosphate material to be demagnetized includes iron phosphide impurities. The high magnetic substances removed by the embodiment of the invention mainly comprise iron phosphide. Wherein the impurity ferric phosphide passes throughThe demagnetizing mechanism of the invention is as follows: PO (Positive oxide) 4 2- +2O 2 +2Li + +Fe 2 P→2LiFePO 4 。
Further, the mixed intermediate is formulated in a graphite sagger.
Further, the phosphorus supplementing agent comprises at least one of sodium phosphate, ammonium phosphate and phosphoric acid.
Further, the input amount of the phosphorus supplementing agent accounts for 0.1-5 per mill of the mass ratio of the lithium iron phosphate material to be demagnetized.
Further, the solvent comprises at least one of water, ethanol, propanol, acetone and ethylene glycol.
Further, the input amount of the solvent accounts for 10-100% of the mass ratio of the lithium iron phosphate material to be demagnetized.
Further, the sintering temperature is 450-750 ℃ and the sintering time is 8-12 h.
Further, the sintering is performed under an inert atmosphere.
Further, the oxygen content in the sintering atmosphere is 0.1ppm to 10ppm.
The following describes the specific procedures and effects of the method for demagnetizing lithium iron phosphate materials according to the present invention in further detail with reference to specific examples, but is not limited to the scope of the present invention.
Example 1
The embodiment performs the demagnetization treatment on the high-magnetism lithium iron phosphate material, and specifically comprises the following steps:
1. 0.8 kg of solvent and 12 g of phosphorus supplementing agent are added into a graphite sagger and stirred uniformly.
2. Then, 4kg of lithium iron phosphate black (magnetic substance 29ppm, compacted density 2.33 g/cm) was added to the sagger 3 ) Stirring until the black powder is completely soaked. Sintering (high temperature 720 deg.c and oxygen content 5.8 ppm) in furnace, crushing and inspection. Measuring 0.12ppm of magnetic substance, compacting 2.44g/cm 3 。
Example 2
The embodiment performs the demagnetization treatment on the high-magnetism lithium iron phosphate material, and specifically comprises the following steps:
1. 1 kg of solvent and 6g of phosphorus supplementing agent are added into a graphite sagger and stirred uniformly.
2. Then, 4kg of lithium iron phosphate black (magnetic material 8.86ppm, compacted density 2.38 g/cm) was added to the sagger 3 ) Stirring until the black powder is completely soaked. Sintering (high temperature 680 deg.c, oxygen content 2.3 ppm) in furnace, crushing and inspection. Measuring 0.15ppm of magnetic substance, compacting 2.46g/cm 3 。
Example 3
The embodiment performs the demagnetization treatment on the high-magnetism lithium iron phosphate material, and specifically comprises the following steps:
1. 4kg of solvent and 12 g of phosphorus supplementing agent are added into a graphite sagger and stirred uniformly.
2. Then, 4kg of lithium iron phosphate black (magnetic substance 29ppm, compacted density 2.33 g/cm) was added to the sagger 3 ) Stirring until the black powder is completely soaked. Sintering (high temperature 720 deg.c and oxygen content 5.8 ppm) in furnace, crushing and inspection. Measuring 0.59ppm of magnetic substance, compacting 2.45g/cm 3 。
Example 4
The embodiment performs the demagnetization treatment on the high-magnetism lithium iron phosphate material, and specifically comprises the following steps:
1. 1 kg of solvent and 12 g of phosphorus supplementing agent are added into a graphite sagger and stirred uniformly.
2. Then, 4kg of lithium iron phosphate black (magnetic substance 29ppm, compacted density 2.33 g/cm) was added to the sagger 3 ) Stirring until the black powder is completely soaked. Sintering (high temperature 620 ℃ C., oxygen content 5.8 ppm) in a furnace, and crushing the discharged materials and checking. The magnetic material was measured at 0.07ppm and compacted at 2.43g/cm 3 。
According to the method for removing the magnetism of the lithium iron phosphate material, disclosed by the embodiment of the invention, the phosphorus supplementing agent and the solvent are added to be mixed with the lithium iron phosphate material to be removed, and the mixed intermediate is subjected to high-temperature sintering and crushing after being mixed, so that the lithium iron phosphate material with the magnetism removed can be obtained, and the electrochemical performance requirement is met. The demagnetizing method has simple process flow and low equipment requirement, and is suitable for large-scale industrial production.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that: many changes, modifications, substitutions and variations may be made to the embodiments without departing from the spirit and principles of the invention, the scope of which is defined by the claims and their equivalents.
Claims (10)
1. A method of demagnetizing lithium iron phosphate material, the method comprising:
s10, uniformly mixing the phosphorus supplementing agent and the solvent according to a certain proportion to obtain a mixed solvent;
s20, soaking the lithium iron phosphate material to be demagnetized with the mixed solvent according to a certain proportion to obtain a mixed intermediate;
s30, sintering and crushing the mixed intermediate to obtain the demagnetized lithium iron phosphate material.
2. The method of claim 1, wherein the lithium iron phosphate material to be demagnetized comprises iron phosphide impurities.
3. The method of demagnetizing lithium iron phosphate material according to claim 1, characterized in that the mixed intermediate is formulated in a graphite sagger.
4. The method of claim 1, wherein the phosphorus supplement comprises at least one of sodium phosphate, ammonium phosphate, and phosphoric acid.
5. The method for removing magnetic iron phosphate material according to claim 4, wherein the amount of the phosphorus supplementing agent is 0.1-5% of the mass of the iron phosphate material to be removed.
6. The method of demagnetizing lithium iron phosphate material according to claim 1, characterized in that the solvent comprises at least one of water, ethanol, propanol, acetone, ethylene glycol.
7. The method for demagnetizing lithium iron phosphate material according to claim 6, wherein the solvent is added in an amount of 10-100% by mass of the lithium iron phosphate material to be demagnetized.
8. The method of demagnetizing lithium iron phosphate material according to claim 1, wherein the sintering temperature is 450-750 ℃ and the sintering time is 8-12 h.
9. The method of demagnetizing lithium iron phosphate material according to claim 1, characterized in that the sintering is performed under an inert atmosphere.
10. The method of demagnetizing lithium iron phosphate material according to claim 9, characterized in that the oxygen content in the sintering atmosphere is 0.1ppm-10ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410050615.9A CN117865105A (en) | 2024-01-12 | 2024-01-12 | Demagnetizing method of lithium iron phosphate material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410050615.9A CN117865105A (en) | 2024-01-12 | 2024-01-12 | Demagnetizing method of lithium iron phosphate material |
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| CN117865105A true CN117865105A (en) | 2024-04-12 |
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| CN202410050615.9A Pending CN117865105A (en) | 2024-01-12 | 2024-01-12 | Demagnetizing method of lithium iron phosphate material |
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- 2024-01-12 CN CN202410050615.9A patent/CN117865105A/en active Pending
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