CN115947379A - Paramagnetic micron material and preparation method thereof - Google Patents
Paramagnetic micron material and preparation method thereof Download PDFInfo
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- CN115947379A CN115947379A CN202211723150.6A CN202211723150A CN115947379A CN 115947379 A CN115947379 A CN 115947379A CN 202211723150 A CN202211723150 A CN 202211723150A CN 115947379 A CN115947379 A CN 115947379A
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- 239000000463 material Substances 0.000 title claims abstract description 58
- 230000005298 paramagnetic effect Effects 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 239000000203 mixture Substances 0.000 claims abstract description 26
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims abstract description 24
- 239000002699 waste material Substances 0.000 claims abstract description 17
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 230000005291 magnetic effect Effects 0.000 claims abstract description 13
- 239000000706 filtrate Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 35
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052744 lithium Inorganic materials 0.000 claims description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 15
- 238000003912 environmental pollution Methods 0.000 abstract description 7
- 150000003839 salts Chemical class 0.000 abstract description 7
- 239000002351 wastewater Substances 0.000 abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 239000007774 positive electrode material Substances 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 description 6
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000010405 anode material Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000005408 paramagnetism Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000010891 toxic waste Substances 0.000 description 1
- 239000010926 waste battery Substances 0.000 description 1
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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
Abstract
The invention provides a paramagnetic micron material and a preparation method thereof, which relate to the technical field of power batteries and comprise the following steps: s1: putting the anode of the waste lithium iron phosphate battery into alkali liquor, and stirring on a constant-temperature magnetic stirrer to obtain a mixture; s2: filtering the mixture to obtain filter residue and filtrate; s3: and drying the filter residue, and calcining at 400-600 ℃ to obtain the paramagnetic micron material. The invention provides a method for preparing a paramagnetic micron material, which takes a positive electrode material of a waste lithium iron phosphate battery as a raw material, and directly converts Fe and O in lithium iron phosphate into micron-sized paramagnetic Fe through stirring and calcining by a constant-temperature magnetic stirrer 3 O 4 The method has the advantages of simple operation and low preparation cost, does not need to consume a large amount of chemical reagents, does not discharge a large amount of salt-containing wastewater, and is not easy to cause environmental pollution.
Description
Technical Field
The invention relates to the technical field of power batteries, in particular to a paramagnetic micron material and a preparation method thereof.
Background
Lithium ion batteries have the characteristics of high energy density, high power, long service life and the like, are known as novel energy storage and conversion devices of electric automobiles, and are beneficial to protecting the environment and solving the energy problem. Among various lithium ion batteries, lithium iron phosphate has a large share in the lithium ion battery market due to the advantages of safety, thermal stability, non-toxicity, long service life and the like. Meanwhile, a large amount of waste lithium iron phosphate batteries are generated, and the waste batteries need to be recycled by an environment-friendly, economical and feasible method so as to suppress toxic waste in the waste lithium ion environment and suppress the exhaustion of residual lithium resources. At present, the recycling method and process route of the waste lithium ion battery are widely developed, and the hydrometallurgical method is the most common method for recycling the waste lithium iron phosphate, namely, transferring metal ions from an electrode material into a leaching solution by using an acid or alkali solution, and then selectively separating Li, fe and P in the form of salt. In the hydrometallurgy process, need consume a large amount of chemical reagent, discharge a large amount of salt waste water, organic electrolyte can not recovery processing well moreover, easily causes environmental pollution, and these shortcomings have greatly hindered the effective recycle of useless lithium iron phosphate.
In view of the above, it is imperative to develop a new method for recycling waste lithium iron phosphate batteries.
Disclosure of Invention
The invention solves the problem that the existing lithium iron phosphate recovery method is easy to cause environmental pollution.
In order to solve the above problems, the present invention provides a method for preparing a paramagnetic micron material, comprising the following steps:
s1: putting the positive electrode of the waste lithium iron phosphate battery into alkali liquor, and stirring on a constant-temperature magnetic stirrer to obtain a mixture;
s2: filtering the mixture to obtain filter residue and filtrate;
s3: and drying the filter residue, and calcining at 400-600 ℃ to obtain the paramagnetic micron material.
Optionally, the temperature range of the constant temperature magnetic stirring is 15-60 ℃.
Optionally, the rotation speed of the constant temperature magnetic stirring is 250rpm.
Alternatively, the calcination time in step S3 is 1-5h.
Optionally, the lye is a NaOH solution.
Alternatively, the concentration of the NaOH solution ranges from 0.2mol/L to 1mol/L.
Optionally, the method further comprises: s4: and recovering lithium and aluminum in the filtrate.
Another object of the present invention is to provide a paramagnetic micro-material, which is prepared by the method for preparing a paramagnetic micro-material as described above.
Compared with the prior art, the preparation method of the paramagnetic micron material provided by the invention has the following advantages:
the invention provides a method for preparing a paramagnetic micron material, which takes a positive electrode material of a waste lithium iron phosphate battery as a raw material, and directly converts Fe and O in lithium iron phosphate into micron-sized paramagnetic Fe through stirring and calcining by a constant-temperature magnetic stirrer 3 O 4 The method has the advantages of simple operation and low preparation cost, does not need to consume a large amount of chemical reagents, does not discharge a large amount of salt-containing wastewater, and is not easy to cause environmental pollution.
Drawings
Fig. 1 is an XRD pattern of paramagnetic micron material prepared in example 1 of the present invention;
FIG. 2 is a SEM image of a paramagnetic micron material prepared in example 2 of the present invention;
FIG. 3 is a hysteresis loop of paramagnetic micron material prepared in example 3 of the present invention.
Detailed Description
Reference will now be made in detail to the embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the drawings are exemplary intended to explain the present invention and should not be construed as limiting the present invention, and all other embodiments that can be obtained by one skilled in the art without inventive effort based on the embodiments of the present invention are within the scope of protection of the present invention.
In order to solve the problem that the existing lithium iron phosphate recovery method is easy to cause environmental pollution, the invention provides a preparation method of a paramagnetic micron material, which comprises the following steps:
s1: putting the anode of the waste lithium iron phosphate battery into alkali liquor, and stirring on a constant-temperature magnetic stirrer to obtain a mixture;
s2: filtering the mixture to obtain filter residue and filtrate;
s3: and drying the filter residue, and calcining at 400-600 ℃ to obtain the paramagnetic micron material.
In particular, the present invention will preferably be LiFePO 4 Cutting the leftover materials of the positive electrode into small pieces of 1cm multiplied by 1cm, and stirring on a constant-temperature magnetic stirrer until the aluminum of the current collector is completely dissolved to obtain a mixture; through the stirring effect of the constant-temperature magnetic stirrer, the iron element is paramagnetic based on the principle of magnetic stirring while the lithium iron phosphate is fully dissolved by fully stirring; and further drying and calcining filter residues in the mixture to obtain the paramagnetic micron material.
The invention provides a method for preparing a paramagnetic micron material, which takes a positive electrode material of a waste lithium iron phosphate battery as a raw material, and directly converts Fe and O in lithium iron phosphate into micron-sized paramagnetic Fe through stirring and calcining by a constant-temperature magnetic stirrer 3 O 4 The method has the advantages of simple operation and low preparation cost, does not need to consume a large amount of chemical reagents, does not discharge a large amount of salt-containing wastewater, and is not easy to cause environmental pollution.
Specifically, the temperature range of the constant-temperature magnetic stirring is preferably 15-60 ℃, and the rotating speed is 250rpm; the calcination time in step S3 is preferably 1 to 5 hours.
The alkali liquor can be NaOH solution or KOH solution, the alkali liquor is preferably NaOH solution in the invention, and the concentration range of NaOH solution is further preferably 0.2mol/L-1mol/L.
Further, the preparation method of the paramagnetic micron material provided by the invention further comprises the following steps: s4: and recovering lithium and aluminum in the filtrate.
The specific method for recovering lithium and aluminum in the filtrate can be related methods in the prior art; the present application does not limit the specific recovery method of lithium and aluminum.
Another object of the present invention is to provide a paramagnetic micro-material prepared by the method for preparing a paramagnetic micro-material as described above.
The paramagnetic micron material provided by the invention is prepared by taking the anode material of a waste lithium iron phosphate battery as a raw material, and in the preparation process, fe and O in lithium iron phosphate are directly converted into micron-sized paramagnetic Fe through stirring and calcining by a constant-temperature magnetic stirrer 3 O 4 The method has the advantages of simple operation, low preparation cost, no need of consuming a large amount of chemical reagents, no discharge of a large amount of salt-containing wastewater, and no easy environmental pollution.
Fe due to paramagnetism 3 O 4 Compared with common Fe 3 O 4 The preparation method of the paramagnetic micron material provided by the invention has wider application prospect in the fields of biomedicine, immunity, environmental science and the like, and the paramagnetic Fe is prepared by taking the anode material of the waste lithium iron phosphate battery as a raw material 3 O 4 The method not only realizes effective recycling of the waste lithium iron phosphate, reduces the discharge amount of salt-containing wastewater in the recycling process, but also improves the additional value of the waste lithium iron phosphate battery recycling product and improves the utilization rate.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
The invention provides a method for preparing a paramagnetic micron material, which comprises the following steps:
s1: mixing LiFePO 4 Positive pole cornerCutting the material into small pieces with the size of 1cm multiplied by 1cm, putting 1g of the material into a beaker containing 100ml of 0.5mol/L NaOH solution, placing the beaker on a constant-temperature magnetic stirrer and stirring the mixture at the stirring temperature of 25 ℃ and the stirring speed of 250rpm, and stirring the mixture for reaction until aluminum in a current collector is completely dissolved to obtain a mixture;
s2: filtering the mixture, and washing the mixture for several times by using deionized water to obtain filter residue and filtrate;
s3: drying the filter residue, moving the filter residue into a tube furnace, introducing air, and calcining the filter residue for 2 hours at 550 ℃ to obtain a sample, namely the sample containing micron-sized Fe 3 O 4 Sample, i.e. paramagnetic micro material.
Detecting the prepared paramagnetic micron material, as shown in figure 1, and comparing with a standard map, the paramagnetic micron material is Fe with JCPDS:019-0629 3 O 4 And (3) sampling.
Example 2
The invention provides a method for preparing a paramagnetic micron material, which comprises the following steps:
s1: mixing LiFePO 4 Cutting the positive leftover materials into small pieces of 1cm multiplied by 1cm, putting 2g of the positive leftover materials into a beaker containing 100ml of a 1mol/L NaOH solution, placing the beaker on a constant-temperature magnetic stirrer and stirring at the stirring temperature of 35 ℃ and the stirring speed of 300rpm, and stirring for reaction until aluminum of a current collector is completely dissolved to obtain a mixture;
s2: filtering the mixture, and washing the mixture for several times by using deionized water to obtain filter residue and filtrate;
s3: drying the filter residue, moving the filter residue into a tube furnace, introducing air, and calcining the filter residue for 4 hours at 550 ℃ to obtain a sample, namely the sample containing micron-sized Fe 3 O 4 Sample, i.e. paramagnetic micro material.
The prepared paramagnetic micron material is detected, and as shown in fig. 2, the paramagnetic micron material prepared in this example is in an irregular powder shape, and the size is in the micron order.
Example 3
The invention provides a method for preparing a paramagnetic micron material, which comprises the following steps:
s1: mixing LiFePO 4 Cutting the leftover material of the positive electrode into small pieces of 1cm multiplied by 1cm, taking 1g and putting into 100ml 0.75mol/L NaOH solutionPlacing the beaker on a constant-temperature magnetic stirrer and stirring, wherein the stirring temperature is 25 ℃, the stirring speed is 300rpm, and stirring for reaction until the aluminum of the current collector is completely dissolved to obtain a mixture;
s2: filtering the mixture, and washing the mixture for a plurality of times by using deionized water to obtain filter residues and filtrate;
s3: drying the filter residue, moving the filter residue into a tube furnace, introducing air, and calcining the filter residue for 4 hours at 550 ℃ to obtain a sample, namely the sample containing micron-sized Fe 3 O 4 Sample, i.e. paramagnetic micro material.
The prepared paramagnetic micron material is detected, and as shown in fig. 3, the saturation magnetization of the paramagnetic micron material prepared in this example is 11.19emu/g, and has certain magnetism, and the hysteresis loops are basically overlapped, which indicates that the material is paramagnetic.
Comparative example 1
The comparative example provides a method for recovering waste lithium iron phosphate, which comprises the following steps:
s1: mixing LiFePO 4 Cutting the leftover materials of the positive electrode into small pieces with the size of 1cm multiplied by 1cm, putting 2g of the leftover materials into a beaker containing 100ml of 0.5mol/L NaOH solution, stirring the mixture by a stirrer at the stirring temperature of 40 ℃ and the stirring speed of 250rpm, and stirring the mixture for reaction until aluminum of a current collector is completely dissolved to obtain a mixture;
s2: filtering the mixture, and washing the mixture for several times by using deionized water to obtain filter residue and filtrate;
s3: and drying the filter residue, moving the filter residue into a tubular furnace, and introducing air to calcine the filter residue for 2 hours at 550 ℃ to obtain the micron material.
Paramagnetic performance of the micron material prepared by the comparative example is detected, and the detection process is the same as that of the example 3; according to the detection result, the micron material does not have paramagnetism.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present disclosure, and such changes and modifications will fall within the scope of the present invention.
Claims (8)
1. A method for preparing paramagnetic micron materials is characterized by comprising the following steps:
s1: putting the anode of the waste lithium iron phosphate battery into alkali liquor, and stirring on a constant-temperature magnetic stirrer to obtain a mixture;
s2: filtering the mixture to obtain filter residue and filtrate;
s3: and drying the filter residue, and calcining at 400-600 ℃ to obtain the paramagnetic micron material.
2. The method for preparing paramagnetic micron material according to claim 1, wherein the temperature range of the constant temperature magnetic stirring is 15-60 ℃.
3. The method for preparing paramagnetic micron material according to claim 1, wherein the rotation speed of the constant temperature magnetic stirring is 250rpm.
4. The method for preparing paramagnetic micro material according to claim 1, wherein the calcination time in step S3 is 1-5h.
5. The method for preparing paramagnetic micro material according to claim 1, wherein the alkali solution is NaOH solution.
6. The method for preparing paramagnetic micro material according to claim 5, wherein the concentration of NaOH solution is in the range of 0.2mol/L to 1mol/L.
7. The method of preparing a paramagnetic micron material according to claims 1 to 6, further comprising: s4: and recovering lithium and aluminum in the filtrate.
8. A paramagnetic micro-material prepared by the method of preparing a paramagnetic micro-material according to any one of claims 1 to 7.
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| CN202211723150.6A CN115947379A (en) | 2022-12-30 | 2022-12-30 | Paramagnetic micron material and preparation method thereof |
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| CN202211723150.6A CN115947379A (en) | 2022-12-30 | 2022-12-30 | Paramagnetic micron material and preparation method thereof |
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| CN101172664A (en) * | 2006-11-01 | 2008-05-07 | 中国民航大学 | Ultrasound wave auxiliary hydrothermal synthesis technique for magnetic magnetic iron oxide nano ultra-tiny grain |
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