CN110668413A - Method for producing battery-grade iron phosphate by using waste lithium iron phosphate cathode material - Google Patents

Method for producing battery-grade iron phosphate by using waste lithium iron phosphate cathode material Download PDF

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CN110668413A
CN110668413A CN201911014850.6A CN201911014850A CN110668413A CN 110668413 A CN110668413 A CN 110668413A CN 201911014850 A CN201911014850 A CN 201911014850A CN 110668413 A CN110668413 A CN 110668413A
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iron phosphate
lithium iron
powder
oxidized
particle size
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赵本富
王筱静
郝彦青
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Zigong Tongfarong New Materials Co Ltd
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Zigong Tongfarong New Materials Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/37Phosphates of heavy metals
    • C01B25/375Phosphates of heavy metals of iron

Abstract

The invention provides a method for producing battery-grade iron phosphate by using a waste lithium iron phosphate positive electrode material, the ferric phosphate contained in the lithium iron phosphate is separated out separately through different working procedures of acid dissolution, impurity filtration, dispersing agent dispersion treatment, iron ion oxidation, water washing, drying and the like, the method does not involve the formation of other intermediate products such as ferric salt or lithium salt and the like in the process of recovering and generating the lithium iron phosphate, it only separates and refines the ferric phosphate, which makes the recycling manufacturing method not generate a large amount of waste, therefore, the recovery efficiency of the iron phosphate is effectively improved, the recovery cost is reduced, and the waste output is reduced.

Description

Method for producing battery-grade iron phosphate by using waste lithium iron phosphate cathode material
Technical Field
The invention relates to the technical field of waste battery material recovery, in particular to a method for producing battery-grade iron phosphate by using a waste lithium iron phosphate positive electrode material.
Background
The lithium iron phosphate anode material is widely used for manufacturing the battery anode, and when the battery fails, the lithium iron phosphate anode material in the battery anode can be correspondingly recycled. At present, the main method for recovering lithium iron phosphate positive electrode materials in the positive electrode of the battery is to crush the lithium iron phosphate positive electrode materials and remove metallic aluminum impurities, then perform corresponding acid solution treatment to further remove impurities such as carbon powder, iron salt, aluminum salt and the like contained in the lithium iron phosphate positive electrode materials, and finally use the obtained lithium salt solution for processing and manufacturing lithium carbonate or other lithium salts; for removing the obtained impurities, as the impurities are usually mixtures containing heavy metals, in order to reduce the pollution to the environment, the mixtures are generally used as manufacturing additives of building bricks or subjected to deep landfill treatment; although the existing recovery method for the lithium iron phosphate cathode material can effectively solve the problems of environmental pollution and resource waste after the lithium iron phosphate is discarded, the waste residue yield of the recovery method is high, generally, 6-10 tons of waste residues are correspondingly formed while 1 ton of lithium carbonate is produced, and the waste residue treatment difficulty and the recovery cost of the recovery method are high.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for producing battery-grade iron phosphate by using a waste lithium iron phosphate positive electrode material, which comprises the following steps of S1, crushing and screening the lithium iron phosphate positive electrode material to obtain lithium iron phosphate powder meeting the specific granularity condition; step S2, under the specific temperature environment condition, carrying out oxidation and calcination treatment on the lithium iron phosphate powder to remove combustible substances at least containing organic adhesives or carbon powder and obtain lithium iron phosphate oxide powder, and then carrying out acidification reaction and filtration separation treatment on the lithium iron phosphate oxide powder and a dispersing agent under the specific acid environment condition to obtain a reaction product of iron phosphate; step S3, performing specific chemical reaction treatment on the iron phosphate to obtain an iron phosphate primary product; step S4, the primary product of the iron phosphate is refined to obtain the battery-grade iron phosphate, the recovery manufacturing method is different from the prior art that the lithium iron phosphate is subjected to reaction conversion to obtain other lithium salts, the main component iron phosphate in the lithium iron phosphate can be separated independently, and the battery-grade iron phosphate is obtained to be directly used for manufacturing other types of batteries.
The invention provides a method for producing battery-grade ferric phosphate by using a waste lithium iron phosphate positive electrode material, which is characterized by comprising the following steps of:
step S1, crushing and screening the lithium iron phosphate positive electrode material to obtain lithium iron phosphate powder meeting the specific granularity condition;
step S2, under a specific temperature environment condition, carrying out oxidation and calcination treatment on the lithium iron phosphate powder to remove combustible substances at least containing organic adhesives or carbon powder and obtain lithium iron phosphate oxide powder, and then carrying out acidification reaction and filtration separation treatment on the lithium iron phosphate oxide powder and a dispersing agent under a specific acid environment condition to obtain a reaction product of iron phosphate;
step S3, performing specific chemical reaction treatment on the iron phosphate to obtain an iron phosphate primary product;
step S4, refining the iron phosphate primary product to obtain battery-grade iron phosphate;
further, in step S1, the crushing and screening of the lithium iron phosphate positive electrode material to obtain the lithium iron phosphate powder satisfying the specific particle size condition specifically includes,
step S101, performing primary grinding and crushing treatment on the lithium iron phosphate to obtain primary lithium iron phosphate powder;
step S102, performing particle size value detection processing on the lithium iron phosphate primary powder to determine the current average particle size value of the lithium iron phosphate primary powder;
step S103, obtaining a matching relation between the current average particle size value of the lithium iron phosphate primary powder and the specific particle size condition, and performing crushing treatment and/or screening treatment in different modes on the lithium iron phosphate powder according to the matching relation to obtain the lithium iron phosphate powder;
further, in the step S103, before obtaining the matching relationship between the current average particle size value of the lithium iron phosphate primary powder and the specific particle size condition, determining the specific particle size condition, specifically, determining a particle size range corresponding to the specific particle size condition as 100-200 meshes;
alternatively, the first and second electrodes may be,
in the step S103, performing crushing processing and/or screening processing in different modes on the lithium iron phosphate powder according to the matching relationship to obtain the lithium iron phosphate powder specifically includes,
step S1031, if the matching relation indicates that the current average particle size value of the lithium iron phosphate primary powder meets the specific particle size condition, screening the lithium iron phosphate treated powder to remove non-lithium iron phosphate solid impurities in the lithium iron phosphate treated powder, so as to obtain the lithium iron phosphate powder;
step S1032, if the matching relation indicates that the current average particle size value of the lithium iron phosphate primary powder does not meet the specific particle size condition, performing secondary grinding and crushing treatment on the lithium iron phosphate primary powder so that the average particle size value meets the specific particle size condition, and performing screening treatment on the lithium iron phosphate treated powder so as to remove non-lithium iron phosphate solid impurities in the lithium iron phosphate treated powder, thereby obtaining the lithium iron phosphate powder;
further, in the step S2, the step of performing an acidification reaction and a filtration separation treatment on the lithium iron phosphate oxide powder and the dispersant under a specific acid environment condition to obtain a reaction product of iron phosphate specifically includes,
step S201, preparing an acid solution with a liquid-solid ratio and/or an acidity value meeting the specific acid environmental conditions;
step S202, dissolving the lithium iron phosphate oxide powder in the acid solution to obtain an oxidized lithium iron phosphate acid solution, and adding the dispersing agent to the oxidized lithium iron phosphate solution to fully mix for the acidification reaction;
step S203, performing the filtration separation treatment on the oxidized lithium iron phosphate acid solution to remove insoluble impurities in the oxidized lithium iron phosphate acid solution;
further, in the step S201, the acid solution configured such that the liquid-solid ratio and/or the acidity value satisfies the specific acid environment condition specifically includes,
preparing an acid solution which meets the requirements that the liquid-solid ratio is 2-10 and/or the acidity value is 30-150 g/l;
further, step S204 is further included after step S203, where step S204 specifically includes,
carrying out pH value adjustment treatment on the oxidized lithium iron phosphate filtrate to adjust the pH value of the oxidized lithium iron phosphate filtrate to 0.5-2.5;
further, the step S202 of adding the dispersing agent to the oxidized lithium iron phosphate solution and sufficiently mixing to perform the acidification reaction specifically includes,
step S2021, adding a CTAB dispersant to the oxidized lithium iron phosphate solution, and maintaining the temperature of the oxidized lithium iron phosphate solution within a predetermined temperature range;
step S2022, adding ferrous oxide ions into the oxidized lithium iron phosphate solution, and simultaneously carrying out the acidification reaction of the ferrous oxide ions in the lithium iron phosphate solution for a preset time;
further, the step S2021 of adding a CTAB dispersant to the oxidized lithium iron phosphate solution specifically includes,
adding a CTAB dispersing agent with the ferric salt content of 0.5-2.5% into the oxidized lithium iron phosphate solution;
alternatively, the first and second electrodes may be,
specifically, the step S2021 of maintaining the temperature of the oxidized lithium iron phosphate solution in the predetermined temperature range includes,
maintaining the temperature of the oxidized lithium iron phosphate solution at 50-90 ℃;
alternatively, the first and second electrodes may be,
in the step S2022, the adding of the oxidized divalent iron ions to the oxidized lithium iron phosphate solution specifically includes,
adding 3-20% of hydrogen peroxide into the oxidized lithium iron phosphate solution to oxidize ferrous ions;
alternatively, the first and second electrodes may be,
in the step S2022, the step of allowing the ferrous oxide ions to perform the acidification reaction in the lithium iron phosphate solution for a predetermined period of time specifically includes,
carrying out an acidification reaction of the oxidized ferrous iron ions in the oxidized lithium iron phosphate solution for 0.5-5 h;
further, in the step S4, refining the primary iron phosphate product to obtain battery-grade iron phosphate specifically includes,
step S401, performing soft water washing treatment on the primary ferric phosphate product to reduce the impurity content of the primary ferric phosphate product;
step S402, drying the primary product of the iron phosphate after the soft water washing treatment to obtain anhydrous battery-grade iron phosphate;
further, in the step S401, the soft water washing treatment of the iron phosphate primary product specifically includes,
carrying out soft water washing treatment on the iron phosphate primary product within the temperature range of 40-80 ℃;
alternatively, the first and second electrodes may be,
in the step S402, the drying process of the iron phosphate primary product after the soft water washing process specifically includes,
and drying the primary iron phosphate product subjected to the soft water washing treatment at the drying temperature of 400-650 ℃.
Compared with the prior art, the method for producing battery-grade iron phosphate by using the waste lithium iron phosphate positive electrode material comprises the following steps of S1, crushing and screening the lithium iron phosphate positive electrode material to obtain lithium iron phosphate powder meeting specific granularity conditions; step S2, under the specific temperature environment condition, carrying out oxidation and calcination treatment on the lithium iron phosphate powder to remove combustible substances at least containing organic adhesives or carbon powder and obtain lithium iron phosphate oxide powder, and then carrying out acidification reaction and filtration separation treatment on the lithium iron phosphate oxide powder and a dispersing agent under the specific acid environment condition to obtain a reaction product of iron phosphate; step S3, performing specific chemical reaction treatment on the iron phosphate to obtain an iron phosphate primary product; step S4, the primary product of the iron phosphate is refined to obtain the battery-grade iron phosphate, the recovery manufacturing method is different from the prior art that the lithium iron phosphate is subjected to reaction conversion to obtain other lithium salts, the main component iron phosphate in the lithium iron phosphate can be separated independently, and the battery-grade iron phosphate is obtained to be directly used for manufacturing other types of batteries.
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In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the embodiments or technical descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic flow chart of a method for producing battery grade iron phosphate by using a waste lithium iron phosphate positive electrode material according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, a schematic flow chart of a method for producing battery grade iron phosphate by using a waste lithium iron phosphate positive electrode material according to the present invention is shown. The recycling and manufacturing method of the battery grade ferro-phosphorus comprises the following steps:
and step S1, crushing and screening the lithium iron phosphate positive electrode material to obtain lithium iron phosphate powder meeting the specific granularity condition.
Preferably, in step S1, the crushing and screening of the lithium iron phosphate positive electrode material to obtain the lithium iron phosphate powder satisfying the specific particle size condition specifically includes,
step S101, performing primary grinding and crushing treatment on the lithium iron phosphate to obtain primary lithium iron phosphate powder;
step S102, carrying out particle size value detection processing on the lithium iron phosphate primary powder to determine the current average particle size value of the lithium iron phosphate primary powder;
step S103, obtaining a matching relation between the current average particle size value of the lithium iron phosphate primary powder and the specific particle size condition, and performing crushing treatment and/or screening treatment in different modes on the lithium iron phosphate powder according to the matching relation to obtain the lithium iron phosphate powder.
Preferably, in the step S103, before obtaining the matching relationship between the current average particle size value of the lithium iron phosphate primary powder and the specific particle size condition, determining the specific particle size condition, specifically, determining the particle size range corresponding to the specific particle size condition to be 100-200 meshes;
preferably, in the step S103, performing crushing treatment and/or screening treatment in different modes on the lithium iron phosphate powder according to the matching relationship to obtain the lithium iron phosphate powder specifically includes,
step S1031, if the matching relation indicates that the current average particle size value of the primary lithium iron phosphate powder meets the specific particle size condition, screening the processed lithium iron phosphate powder to remove non-lithium iron phosphate solid impurities in the processed lithium iron phosphate powder, so as to obtain the lithium iron phosphate powder;
step S1032, if the matching relationship indicates that the current average particle size of the primary lithium iron phosphate powder does not satisfy the specific particle size condition, performing secondary grinding and crushing on the primary lithium iron phosphate powder to make the average particle size satisfy the specific particle size condition, and performing screening on the processed lithium iron phosphate powder to remove non-lithium iron phosphate solid impurities therein, thereby obtaining the lithium iron phosphate powder.
Step S2, under a specific temperature environment condition, performing an oxidizing calcination process on the lithium iron phosphate powder to remove a combustible substance at least containing an organic binder or carbon powder and obtain a lithium iron phosphate oxide powder, and then performing an acidification reaction and a filtration separation process on the lithium iron phosphate oxide powder and a dispersant under a specific acid environment condition to obtain a reaction product, namely, iron phosphate.
Preferably, in the step S2, the step of subjecting the lithium iron phosphate oxide powder and the dispersant to an acidification reaction and a filtering separation treatment under a specific acid environment condition to obtain the reaction product iron phosphate specifically includes,
step S201, preparing an acid solution with a liquid-solid ratio and/or an acidity value meeting the specific acid environmental condition;
step S202, dissolving the lithium iron phosphate oxide powder in the acid solution to obtain an oxidized lithium iron phosphate acid solution, and adding the dispersing agent into the oxidized lithium iron phosphate solution to fully mix for carrying out the acidification reaction;
step S203, the filtration separation treatment is performed on the oxidized lithium iron phosphate acidic solution to remove insoluble impurities in the oxidized lithium iron phosphate acidic solution.
Preferably, in step S201, the acid solution configured such that the liquid-solid ratio and/or the acidity value satisfies the specific acid environment condition specifically includes,
preparing an acid solution which meets the requirements that the liquid-solid ratio is 2-10 and/or the acidity value is 30-150 g/l;
preferably, step S204 is further included after step S203, and step S204 specifically includes,
carrying out pH value adjustment treatment on the oxidized lithium iron phosphate filtrate to adjust the pH value of the oxidized lithium iron phosphate filtrate to 0.5-2.5;
preferably, in the step S202, adding the dispersant to the oxidized lithium iron phosphate solution and sufficiently mixing to perform the acidification reaction specifically includes,
step S2021, adding a CTAB dispersant to the oxidized lithium iron phosphate solution, and maintaining the temperature of the oxidized lithium iron phosphate solution within a predetermined temperature range;
step S2022, adding ferrous oxide ions into the oxidized lithium iron phosphate solution, and simultaneously carrying out the acidification reaction of the ferrous oxide ions in the lithium iron phosphate solution for a predetermined time;
preferably, in step S2021, adding a CTAB dispersant to the oxidized lithium iron phosphate solution specifically includes,
adding a CTAB dispersing agent with the ferric salt content of 0.5-2.5% into the oxidized lithium iron phosphate solution;
preferably, in the step S2021, maintaining the temperature of the oxidized lithium iron phosphate solution in the predetermined temperature range specifically includes,
maintaining the temperature of the oxidized lithium iron phosphate solution at 50-90 ℃;
preferably, in step S2022, the adding of the oxidized divalent iron ions to the oxidized lithium iron phosphate solution specifically includes,
adding 3-20% of hydrogen peroxide into the oxidized lithium iron phosphate solution to oxidize ferrous ions;
preferably, in the step S2022, the acidifying reaction of the divalent iron oxide ions in the lithium iron phosphate solution for a predetermined period of time specifically includes,
so that the reaction time of the ferrous oxide ions in the ferric oxide phosphate lithium solution is 0.5-5 h.
And step S3, performing specific chemical reaction treatment on the iron phosphate to obtain an iron phosphate primary product.
And step S4, refining the iron phosphate primary product to obtain battery-grade iron phosphate.
Preferably, in the step S4, refining the primary iron phosphate product to obtain battery-grade iron phosphate specifically includes,
step S401, performing soft water washing treatment on the primary ferric phosphate product to reduce the impurity content of the primary ferric phosphate product;
step S402, drying the primary product of iron phosphate after the soft water washing treatment to obtain anhydrous battery-grade iron phosphate.
Preferably, in the step S401, the soft water washing treatment of the iron phosphate primary product specifically includes,
carrying out soft water washing treatment on the iron phosphate primary product within the temperature range of 40-80 ℃;
preferably, in the step S402, the drying process of the iron phosphate primary product after the soft water washing process specifically includes,
and drying the primary iron phosphate product subjected to the soft water washing treatment at the drying temperature of 400-650 ℃.
From the content of the embodiment, the method is different from the prior art that lithium iron phosphate is subjected to reaction conversion to obtain other lithium salts, and the iron phosphate contained in the lithium iron phosphate is separated separately through different processes such as acid dissolution, impurity filtration, dispersing agent dispersion treatment, iron ion oxidation, water washing and drying, so that battery-grade iron phosphate is obtained to be directly used for manufacturing other types of batteries, the recycling manufacturing method can solve the problem of high waste residue rate in the recycling and generating process of the conventional lithium iron phosphate positive electrode material, the yield of corresponding solid waste residues is reduced by more than 90%, the recycling and production cost can be reduced, and battery-grade iron phosphate products with high added values can be generated, so that the effects of improving the recycling economic benefit of the lithium iron phosphate, reducing the recycling and production cost and waste residue treatment cost, and reducing environmental pollution are achieved; in addition, the recovery manufacturing method does not involve the formation of other iron salts or lithium salts and other intermediate products in the process of recovering and generating the lithium iron phosphate, and only separates and refines the iron phosphate, so that the recovery manufacturing method does not generate a large amount of waste, thereby effectively improving the recovery efficiency of the iron phosphate, reducing the recovery cost and reducing the waste output.

Claims (10)

1. A method for producing battery-grade ferric phosphate by using a waste lithium iron phosphate positive electrode material is characterized in that the method for recycling and manufacturing the battery-grade ferrophosphorus comprises the following steps:
step S1, crushing and screening the lithium iron phosphate positive electrode material to obtain lithium iron phosphate powder meeting the specific granularity condition;
step S2, under a specific temperature environment condition, carrying out oxidation and calcination treatment on the lithium iron phosphate powder to remove combustible substances at least containing organic adhesives or carbon powder and obtain lithium iron phosphate oxide powder, and then carrying out acidification reaction and filtration separation treatment on the lithium iron phosphate oxide powder and a dispersing agent under a specific acid environment condition to obtain a reaction product of iron phosphate;
step S3, performing specific chemical reaction treatment on the iron phosphate to obtain an iron phosphate primary product;
and step S4, refining the iron phosphate primary product to obtain battery-grade iron phosphate.
2. The method for producing battery grade iron phosphate by using the waste lithium iron phosphate cathode material as claimed in claim 1, wherein:
in step S1, the crushing and screening of the lithium iron phosphate positive electrode material to obtain lithium iron phosphate powder satisfying the specific particle size condition specifically includes,
step S101, performing primary grinding and crushing treatment on the lithium iron phosphate to obtain primary lithium iron phosphate powder;
step S102, performing particle size value detection processing on the lithium iron phosphate primary powder to determine the current average particle size value of the lithium iron phosphate primary powder;
step S103, obtaining a matching relation between the current average particle size value of the lithium iron phosphate primary powder and the specific particle size condition, and performing crushing treatment and/or screening treatment in different modes on the lithium iron phosphate powder according to the matching relation to obtain the lithium iron phosphate powder.
3. The method for producing battery grade iron phosphate by using the waste lithium iron phosphate positive electrode material as claimed in claim 2, wherein:
in step S103, before obtaining the matching relationship between the current average particle size value of the lithium iron phosphate primary powder and the specific particle size condition, determining the specific particle size condition, specifically, determining a particle size range corresponding to the specific particle size condition as 100-200 meshes;
alternatively, the first and second electrodes may be,
in the step S103, performing crushing processing and/or screening processing in different modes on the lithium iron phosphate powder according to the matching relationship to obtain the lithium iron phosphate powder specifically includes,
step S1031, if the matching relation indicates that the current average particle size value of the lithium iron phosphate primary powder meets the specific particle size condition, screening the lithium iron phosphate treated powder to remove non-lithium iron phosphate solid impurities in the lithium iron phosphate treated powder, so as to obtain the lithium iron phosphate powder;
step S1032, if the matching relation indicates that the current average particle size value of the lithium iron phosphate primary powder does not meet the specific particle size condition, performing secondary grinding and crushing treatment on the lithium iron phosphate primary powder so that the average particle size value meets the specific particle size condition, and performing screening treatment on the lithium iron phosphate treated powder so as to remove non-lithium iron phosphate solid impurities in the lithium iron phosphate treated powder, thereby obtaining the lithium iron phosphate powder.
4. The method for producing battery grade iron phosphate by using the waste lithium iron phosphate cathode material as claimed in claim 1, wherein:
in the step S2, the step of performing an acidification reaction and a filtration separation treatment on the lithium iron phosphate oxide powder and the dispersant under a specific acid environment condition to obtain a reaction product of iron phosphate specifically includes,
step S201, preparing an acid solution with a liquid-solid ratio and/or an acidity value meeting the specific acid environmental conditions;
step S202, dissolving the lithium iron phosphate oxide powder in the acid solution to obtain an oxidized lithium iron phosphate acid solution, and adding the dispersing agent to the oxidized lithium iron phosphate solution to fully mix for the acidification reaction;
step S203, performing the filtration separation treatment on the oxidized lithium iron phosphate acid solution to remove insoluble impurities in the oxidized lithium iron phosphate acid solution.
5. The method for producing battery grade iron phosphate by using the waste lithium iron phosphate cathode material as claimed in claim 4, wherein the method comprises the following steps:
in the step S201, the acid solution configured such that the liquid-solid ratio and/or the acidity value satisfies the specific acid environment condition specifically includes,
preparing acid solution with liquid-solid ratio of 2-10 and/or acidity value of 30-150 g/l.
6. The method for producing battery grade iron phosphate by using the waste lithium iron phosphate cathode material as claimed in claim 4, wherein the method comprises the following steps:
step S204 is further included after step S203, where step S204 specifically includes performing PH adjustment processing on the oxidized lithium iron phosphate filtrate to adjust the PH of the oxidized lithium iron phosphate filtrate to 0.5-2.5.
7. The method for producing battery grade iron phosphate by using the waste lithium iron phosphate cathode material as claimed in claim 4, wherein the method comprises the following steps:
in the step S202, adding the dispersant to the oxidized lithium iron phosphate solution and sufficiently mixing to perform the acidification reaction specifically includes,
step S2021, adding a CTAB dispersant to the oxidized lithium iron phosphate solution, and maintaining the temperature of the oxidized lithium iron phosphate solution within a predetermined temperature range;
step S2022, adding divalent iron oxide ions to the oxidized lithium iron phosphate solution, and simultaneously performing the acidification reaction of the divalent iron oxide ions in the lithium iron phosphate solution for a predetermined period of time.
8. The method for producing battery grade iron phosphate by using the waste lithium iron phosphate cathode material as claimed in claim 7, wherein the method comprises the following steps:
in the step S2021, adding a CTAB dispersant to the oxidized lithium iron phosphate solution specifically includes,
adding a CTAB dispersing agent with the ferric salt content of 0.5-2.5% into the oxidized lithium iron phosphate solution;
alternatively, the first and second electrodes may be,
specifically, the step S2021 of maintaining the temperature of the oxidized lithium iron phosphate solution in the predetermined temperature range includes,
maintaining the temperature of the oxidized lithium iron phosphate solution at 50-90 ℃;
alternatively, the first and second electrodes may be,
in the step S2022, the adding of the oxidized divalent iron ions to the oxidized lithium iron phosphate solution specifically includes,
adding 3-20% of hydrogen peroxide into the oxidized lithium iron phosphate solution to oxidize ferrous ions;
alternatively, the first and second electrodes may be,
in the step S2022, the step of allowing the ferrous oxide ions to perform the acidification reaction in the lithium iron phosphate solution for a predetermined period of time specifically includes,
and carrying out an acidification reaction on the oxidized ferrous iron ions in the oxidized lithium iron phosphate solution for 0.5-5 h.
9. The method for producing battery grade iron phosphate by using the waste lithium iron phosphate cathode material as claimed in claim 1, wherein:
in step S4, refining the primary iron phosphate product to obtain battery-grade iron phosphate specifically includes,
step S401, performing soft water washing treatment on the primary ferric phosphate product to reduce the impurity content of the primary ferric phosphate product;
step S402, drying the primary product of the iron phosphate after the soft water washing treatment to obtain anhydrous battery grade iron phosphate.
10. The method for producing battery grade iron phosphate from waste lithium iron phosphate positive electrode material according to claim 9, characterized in that:
in the step S401, the soft water washing treatment of the iron phosphate primary product specifically includes,
carrying out soft water washing treatment on the iron phosphate primary product within the temperature range of 40-80 ℃;
alternatively, the first and second electrodes may be,
in the step S402, the drying process of the iron phosphate primary product after the soft water washing process specifically includes,
and drying the primary iron phosphate product subjected to the soft water washing treatment at the drying temperature of 400-650 ℃.
CN201911014850.6A 2019-10-24 2019-10-24 Method for producing battery-grade iron phosphate by using waste lithium iron phosphate cathode material Pending CN110668413A (en)

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CN111792635A (en) * 2020-06-23 2020-10-20 湖南邦普循环科技有限公司 Preparation method of anhydrous iron phosphate
CN114132911A (en) * 2021-11-29 2022-03-04 材料科学姑苏实验室 Doping regeneration ferric phosphate lithium material and preparation method and application thereof
CN114132909A (en) * 2021-12-07 2022-03-04 自贡同发荣新材料有限公司 Method for recycling pure metal salt from retired manganese iron phosphate lithium battery waste

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