CN115947321A - High-aluminum high-carbon type iron phosphate waste recovery process and application thereof - Google Patents
High-aluminum high-carbon type iron phosphate waste recovery process and application thereof Download PDFInfo
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- CN115947321A CN115947321A CN202211034103.0A CN202211034103A CN115947321A CN 115947321 A CN115947321 A CN 115947321A CN 202211034103 A CN202211034103 A CN 202211034103A CN 115947321 A CN115947321 A CN 115947321A
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- 239000002699 waste material Substances 0.000 title claims abstract description 49
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 title claims abstract description 48
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 47
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 45
- 229910000398 iron phosphate Inorganic materials 0.000 title claims abstract description 45
- 238000011084 recovery Methods 0.000 title claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 40
- 239000000243 solution Substances 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000012535 impurity Substances 0.000 claims abstract description 20
- 239000007800 oxidant agent Substances 0.000 claims abstract description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007787 solid Substances 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 7
- 238000004064 recycling Methods 0.000 claims abstract 10
- 239000002002 slurry Substances 0.000 claims description 18
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 2
- 239000010926 waste battery Substances 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052802 copper Inorganic materials 0.000 abstract description 4
- 239000010949 copper Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 230000001590 oxidative effect Effects 0.000 abstract description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052804 chromium Inorganic materials 0.000 abstract description 3
- 239000011651 chromium Substances 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- RQMIWLMVTCKXAQ-UHFFFAOYSA-N [AlH3].[C] Chemical compound [AlH3].[C] RQMIWLMVTCKXAQ-UHFFFAOYSA-N 0.000 abstract description 2
- 238000012216 screening Methods 0.000 abstract 2
- 238000005554 pickling Methods 0.000 abstract 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000005955 Ferric phosphate Substances 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 229940032958 ferric phosphate Drugs 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
Classifications
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a high-aluminum high-carbon type iron phosphate waste recovery process, which comprises the following steps: pre-screening the iron phosphate waste, wet screening, testing impurity content, pickling, oxidizing, roasting and crushing to obtain the iron phosphate waste. The method provided by the invention can be used for recycling the high-aluminum high-carbon type iron phosphate waste, and can realize a removal rate of more than 97% of aluminum-carbon elements, and the removal rate is high. And 3mol/L H is adopted by adjusting the solid content of the wet material to be 25 percent 2 SO 4 The aqueous solution acid cleaning can greatly improve the removal rate of aluminum and carbon impurities in the high-aluminum high-carbon waste iron phosphate, and the acid solution has low use concentration and low environmental protection pressure. Meanwhile, oxidizing by using a low-concentration oxidant, roasting at 700 ℃, and keeping the temperature for 4 hours, so that the removal rate of impurity metal elements in the system can be further improved, especially for copper, chromium and other elementsAnd (4) element.
Description
Technical Field
The invention relates to a high-aluminum high-carbon type iron phosphate waste recovery process and application thereof, relates to C01B25, and particularly relates to the field of phosphate-containing material treatment.
Background
Along with the development of science and technology, the use level of new energy electric energy is higher and higher, the synthesis process of the lithium iron phosphate battery is very perfect, and the lithium iron phosphate battery is widely loved by people due to the characteristics of high energy density, good safety performance, stable chemical performance and long cycle life. Lithium iron phosphate batteries are widely used in electric energy products, and the scrappage of lithium iron phosphate batteries is rapidly increased. If the waste lithium iron phosphate batteries are not treated, fluoride and heavy metal in the waste lithium iron phosphate batteries enter the environment, the environment can be greatly damaged, and the natural environment and the human health are greatly harmed. After lithium is removed from the waste lithium iron phosphate batteries, the waste lithium iron phosphate is purified, so that the regeneration of the lithium iron phosphate can be realized, and the method has great economic benefit.
Chinese invention patent CN202111318598.5 discloses a method for treating high-impurity lithium iron phosphate waste powder by low-consumption phosphoric acid, which comprises the steps of pre-removing aluminum from the calcined lithium iron phosphate waste powder in an alkaline system, leaching with phosphoric acid and hydrogen peroxide, and purifying FePO4 leaching residue by using excessive phosphoric acid. The Chinese patent of invention CN202110976026.X discloses a method for recovering waste lithium iron phosphate battery powder, which comprises the steps of subjecting mixed powder of a positive electrode and a negative electrode to an alkaline boiling method to obtain powder of the positive electrode and the negative electrode after aluminum removal, adding inorganic acid to leach lithium, iron, phosphate radical and copper elements, filtering to obtain filtrate and graphite, and recovering the graphite after purification.
Disclosure of Invention
In order to solve the problem of low impurity removal efficiency in the high-aluminum high-carbon type iron phosphate waste and ensure high safety and environmental protection in the impurity removal treatment process, the invention provides a high-aluminum high-carbon type iron phosphate waste recovery process, which comprises the following steps:
(1) Drying the iron phosphate waste wet material, crushing and sieving to obtain a material 1;
(2) Adding water into the material 1 obtained in the step 1 to prepare slurry with proper solid content, and sieving by a wet method to obtain physically impurity-removed slurry;
(3) Drying the slurry obtained in the step 2, then testing the content of impurities, then adding an acid solution into a storage tank, stirring for a period of time, adding an oxidizing substance, stirring for reaction, then performing filter pressing, and drying to obtain a material 2 after impurity removal;
(4) And (4) roasting the material 2 obtained in the step (3) in a rotary kiln, preserving heat for a period of time, and crushing to obtain the purified iron phosphate material.
In a preferred embodiment, the iron phosphate waste is high-aluminum high-carbon iron phosphate waste, wherein the aluminum content is more than 30000ppm, and the carbon content is more than 60000ppm.
As a preferred embodiment, the crushing and sieving in the step 1 have a mesh size of 20-100 meshes.
As a preferred embodiment, the wet sieving in step 2 has a mesh size of 200-800 meshes.
The treated iron phosphate waste is a high-aluminum high-carbon type iron phosphate product, the aluminum content reaches 37000ppm and the carbon content reaches 68000ppm in an element test. The applicant finds that when the recycled raw material iron phosphate waste contains high-concentration aluminum elements and carbon elements, the aluminum elements and the carbon elements cannot be removed completely by adopting a conventional acid dissolution method, the residual quantity of the aluminum and the carbon in the recycled material is high, and an iron phosphate finished product with high purity cannot be obtained.
As a preferred embodiment, the solid content of the slurry formed by adding water to the material 1 in the step 2 is 20-45%.
As a preferred embodiment, the solid content of the slurry formed by adding water to the material 1 in the step 2 is 25-40%.
As a preferred embodiment, the solid content of the slurry formed by adding water to the material 1 in the step 2 is 25%.
As a preferred embodiment, the acid solution is selected from one or a combination of strong acid solution, medium strong acid solution and weak acid solution.
As a preferred embodiment, the strong acid solution is selected from HClO 4 、HI、H 2 SO 4 、HCI、HBr、HNO 3 、HIO 3 One or a combination of several of them.
As a preferred embodiment, the medium strong acid solution is selected from H 2 C 2 O 4 、H 3 PO 4 、HNO 2 、C 3 H 4 O 3 One or a combination of several of them.
As a preferred embodiment, said weak acid solution is selected from C 6 H 8 O 7 And malic acid or a combination of several of the above.
As a preferred embodiment, the acid solution is H 2 SO 4 An aqueous solution.
In a preferred embodiment, the strong acid solution is a mixed solution of an acidic substance and water, the concentration of the strong acid solution is 1.0mol/L-4.5mol/L, and the stirring time is 2-8h after the acid solution is added in the step 3.
In a preferred embodiment, the strong acid solution is a mixed solution of an acidic substance and water, the concentration of the strong acid solution is 2mol/L-3mol/L, and the stirring time is 3-6h after the acid solution is added in the step 3.
In a preferred embodiment, the strong acid solution is a mixed solution of an acidic substance and water, the concentration of the strong acid solution is 3mol/L, and the stirring time is 5h after the acid solution is added in the step 3.
The Applicant has further found that by adjusting the solids content of the wet mass to 25%, 3mol/L of H are used 2 SO 4 The acid washing with aqueous solution can be greatly improvedThe removal rate of aluminum and carbon impurities in the high-aluminum high-carbon waste iron phosphate. The possible reasons for guessing are: h 2 SO 4 The aqueous solution contains higher hydrogen ion concentration, which can improve the acid cleaning efficiency of metal impurities, but when H is used 2 SO 4 When the concentration of the aqueous solution is too high, passivation of the surface of the aluminum metal element may occur, which may reduce the removal efficiency of the metal element, and thus high purity of the high-aluminum high-carbon type iron phosphate waste cannot be achieved.
As a preferred embodiment, the oxidizing substance is selected from H 2 O 2 、O 2 、O 3 、CH 3 COOOH or a combination of several COOOH.
In a preferred embodiment, the oxidizing substance is H 2 O 2 。
In a preferred embodiment, the molar concentration of the oxidizing substance is 0.05 to 0.15mol/L.
In a preferred embodiment, the molar concentration of the oxidizing substance is 0.05 to 0.1mol/L.
In a preferred embodiment, the molar concentration of the oxidizing substance is 0.05mol/L.
In a preferred embodiment, the roasting temperature of the rotary kiln in the step 4 is 650-950 ℃, and the holding time is 3-12h.
In a preferred embodiment, the roasting temperature of the rotary kiln in the step 4 is 700-750 ℃, and the holding time is 4-6h.
In a preferred embodiment, the roasting temperature of the rotary kiln in the step 4 is 700 ℃, and the holding time is 4 hours.
The second aspect of the invention provides application of a high-aluminum high-carbon type ferric phosphate waste recovery process, which is applied to treatment of crushed lithium iron phosphate waste batteries and treatment of lithium iron phosphate positive plates after lithium extraction.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the recovery process of the high-aluminum high-carbon type iron phosphate waste, the high-aluminum high-carbon type iron phosphate waste with the aluminum content of 37000ppm and the carbon content of 68000ppm is recovered, the removal rate of more than 97% of aluminum carbon elements can be realized, and the removal rate is high.
(2) According to the high-aluminum high-carbon type ferric phosphate waste recovery process, the solid content of wet materials is adjusted to be 25%, and 3mol/L H is adopted 2 SO 4 The aqueous solution acid cleaning can greatly improve the removal rate of aluminum and carbon impurities in the high-aluminum high-carbon waste iron phosphate, and the acid solution has low use concentration and low environmental protection pressure.
(3) The high-aluminum high-carbon type iron phosphate waste recovery process provided by the invention adopts a low-concentration oxidant for oxidation, and roasting and heat preservation are carried out for 4 hours at 700 ℃, so that the removal rate of impurity metal elements in a system can be further improved, especially for elements such as copper and chromium.
Drawings
Fig. 1 is a schematic flow diagram of the high-aluminum high-carbon type iron phosphate waste recovery process of the invention.
Detailed Description
Example 1
The flow of the steps is shown in figure 1: a high-aluminum high-carbon type iron phosphate waste recovery process comprises the following steps:
(1) Drying the iron phosphate waste wet material, crushing and sieving to obtain a material 1;
(2) Adding water into the material 1 in the step 1 to prepare slurry with proper solid content, and sieving by a wet method to obtain physically impurity-removed slurry;
(3) Drying the slurry obtained in the step 2, then testing the content of impurities, then adding an acid solution into a storage tank, stirring for a period of time, adding an oxidizing substance, stirring for reaction, then performing filter pressing, and drying to obtain a material 2 after impurity removal;
(4) And (4) roasting the material 2 obtained in the step (3) in a rotary kiln, preserving heat for a period of time, and crushing to obtain a purified iron phosphate material.
And (3) crushing and sieving in the step (1), wherein the mesh size is 80 meshes.
And (3) performing wet sieving in the step (2), wherein the mesh size is 500 meshes.
In the step 2, the solid content of the slurry formed by adding water to the material 1 is 40%.
The acid solution is H 2 SO 4 An aqueous solution. The concentration of the strong acid solution is 2mol/L, and the stirring time is 5h after the acid solution is added in the step 3.
The oxidizing substance is H 2 O 2 The solvent is water, and the molar concentration of the oxidizing substance is 0.1mol/L. And (4) after the oxidizing substance is added in the step (3), stirring for 1h.
In the step 4, the roasting temperature of the rotary kiln is 700 ℃, and the heat preservation time is 4 hours.
Example 2
The specific steps of the process for recovering high-aluminum high-carbon type iron phosphate waste are the same as those in example 1, and the difference is that in the step 2, the solid content of slurry formed by adding water to the material 1 is 25%, the concentration of the strong acid solution is 3mol/L, and the molar concentration of the oxidizing substance is 0.05mol/L.
Example 3
The specific steps of the process for recovering the high-aluminum high-carbon type iron phosphate waste material are the same as those in example 1, and the difference is that the solid content of slurry formed by adding water into the material 1 in the step 2 is 25%, the molar concentration of the oxidizing substance is 0.05mol/L, the roasting temperature of the rotary kiln in the step 4 is 750 ℃, and the heat preservation time is 6 hours.
Comparative example 1
The specific steps of the process for recovering the high-aluminum high-carbon type iron phosphate waste material are the same as those in example 1, and the difference is that the solid content of slurry formed by adding water to the material 1 in the step 2 is 25%, and the molar concentration of the oxidizing substance is 0.05mol/L.
Performance test
And (3) testing the impurity content of the dried slurry obtained in the step (2) before adding the oxidizing substance without adding acid in the step (3), wherein the ICP impurity element content test comprises the following steps: aluminum: 37450ppm, carbon: 68500ppm, copper: 1150ppm, zinc: 65ppm, chromium: 81ppm. The impurity content and the impurity removal rate after treatment are shown in table 1.
TABLE 1
Claims (10)
1. The high-aluminum high-carbon type iron phosphate waste recycling process is characterized by comprising the following steps of:
(1) Drying, crushing and sieving the wet iron phosphate waste to obtain a material 1;
(2) Adding water into the material 1 in the step 1 to prepare slurry with proper solid content, and sieving by a wet method to obtain physically impurity-removed slurry;
(3) Drying the slurry obtained in the step 2, then testing the content of impurities, then adding an acid solution into a storage tank, stirring for a period of time, adding an oxidizing substance, stirring for reaction, then performing filter pressing, and drying to obtain a material 2 after impurity removal;
(4) And (4) roasting the material 2 obtained in the step (3) in a rotary kiln, preserving heat for a period of time, and crushing to obtain the purified iron phosphate material.
2. The recycling process of the high-aluminum high-carbon type iron phosphate waste material according to claim 1, wherein the iron phosphate waste material is high-aluminum high-carbon type iron phosphate waste material, and the aluminum content is more than 30000ppm, and the carbon content is more than 60000ppm.
3. The recycling process of high-aluminum high-carbon type iron phosphate waste material according to claim 1, wherein the crushing and sieving in the step 1 have a mesh size of 20-100 meshes.
4. The process for recycling the high-aluminum high-carbon type iron phosphate waste material according to claim 1, wherein the solid content of the slurry formed by adding water to the material 1 in the step 2 is 20-45%.
5. The high-aluminum high-carbon type iron phosphate waste recovery process according to claim 1, wherein the acid solution is selected from one or more of strong acid solution, medium-strong acid solution and weak acid solution.
6. The recycling process of high-aluminum high-carbon type iron phosphate waste material according to claim 5, wherein the strong acid solution is selected from HClO 4 、HI、H 2 SO 4 、HCI、HBr、HNO 3 、HIO 3 One or a combination of several of them.
7. The recycling process of high-aluminum high-carbon type iron phosphate waste material according to claim 5, wherein the strong acid solution is a mixed solution of an acidic substance and water, the concentration of the strong acid solution is 1.0mol/L-4.5mol/L, and the stirring time is 2-8h after the acid solution is added in the step 3.
8. The process for recycling the high-aluminum high-carbon type iron phosphate waste material according to claim 1, wherein the oxidizing substance is selected from H 2 O 2 、O 2 、O 3 、CH 3 COOOH or a combination of several COOOH.
9. The recycling process of the high-aluminum high-carbon type iron phosphate waste material according to claim 1, wherein the molar concentration of the oxidizing substance is 0.05-0.15mol/L.
10. The application of the process for recycling the high-aluminum high-carbon type iron phosphate waste material according to any one of claims 1 to 9 is characterized by being applied to the treatment of crushed lithium iron phosphate waste batteries and the treatment of lithium iron phosphate positive plates after lithium extraction.
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- 2022-08-26 CN CN202211034103.0A patent/CN115947321A/en active Pending
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| CN102709620A (en) * | 2012-05-23 | 2012-10-03 | 浙江大学 | Method for recycling positive material of waste lithium iron phosphate battery |
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