CN104600391A - Method for preparing manganese-doped cobalt ferrite magnetostriction material by utilizing spent lithium ion batteries - Google Patents
Method for preparing manganese-doped cobalt ferrite magnetostriction material by utilizing spent lithium ion batteries Download PDFInfo
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- CN104600391A CN104600391A CN201510023800.XA CN201510023800A CN104600391A CN 104600391 A CN104600391 A CN 104600391A CN 201510023800 A CN201510023800 A CN 201510023800A CN 104600391 A CN104600391 A CN 104600391A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N35/00—Magnetostrictive devices
- H10N35/01—Manufacture or treatment
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N35/00—Magnetostrictive devices
- H10N35/80—Constructional details
- H10N35/85—Magnetostrictive active materials
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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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Abstract
The invention discloses a method for preparing a manganese-doped cobalt ferrite magnetostriction material by utilizing spent lithium ion batteries, belonging to the technical fields of spent lithium ion battery recycling and magnetostriction materials. According to the key points of the technical scheme in the invention, the method for preparing the manganese-doped cobalt ferrite magnetostriction material by utilizing spent lithium ion batteries is characterized in that the manganese-doped cobalt ferrite magnetostriction material with high magnetostriction property in a low field is obtained through a sol-gel-hydrothermal coupling method by utilizing the spent lithium ion batteries. According to the method disclosed by the invention, the spent lithium ion batteries are recycled, the energy is saved, the environment is protected, and the prepared manganese-doped cobalt ferrite magnetostriction material has high magnetostriction property in the low field and has obvious applications in pressure sensors, brakes, non-contact type sensors, sonar probes and magnetic force ejection devices.
Description
Technical field
The invention belongs to waste and old lithium ion battery renewable resources and magnetostrictive material preparing technical field, be specifically related to a kind of method utilizing waste and old lithium ion battery to prepare additive Mn Conjugate ferrite magnetostrictive material.
Background technology
Lithium ion battery has a series of premium properties, there is the high and advantage such as to have extended cycle life of high-energy-density, high power density, operating voltage, the fields such as mobile phone, notebook computer and video camera are widely used in, progressively set out to new-energy automobile and electric tool class again now, the market share significantly improves.Current anode material for lithium-ion batteries mainly contains LiMO
2(LiCoO
2, LiNiO
2, LiNi
1/3co
1/3mn
1/3o
2) system, lithium manganese oxide (LiMn
2o
4) system and iron lithium system (LiFePO
4) system.
Waste and old lithium ion battery is a kind of solid waste more common in daily life, along with the progress of life and the develop rapidly of science and technology, discarded amount increases year by year, containing metals such as a large amount of cobalt, lithium and iron in waste and old lithium ion battery, not only can cause severe contamination to the environment such as water source and air, and resource can be caused to waste in a large number.Therefore, be necessary waste and old lithium ion battery renewable resources to utilize.At present, many researchers have done a large amount of work in waste and old lithium ion battery renewable resources, on the one hand, mainly purify with regard to the precious metal separation in waste and old lithium ion battery, again use as the raw material of industry in traditional resource reclaim; On the other hand, leach by acid solution after waste and old lithium ion battery is pulverized, metal wherein is directly utilized and makes the product that some have certain added value, the sulfate, nitrate etc. of such as metal and be reassembled into the composite functional materials such as cobalt acid lithium, and the method utilizing waste and old lithium ion battery to prepare magnetostrictive material has no report.
Summary of the invention
The object of this invention is to provide a kind of method utilizing waste and old lithium ion battery to prepare additive Mn Conjugate ferrite magnetostrictive material, the additive Mn Conjugate ferrite magnetostrictive material that the method be coupled by the sol-gel-hydrothermal low Magnetostriction after the match that utilized waste and old lithium ion battery to obtain is higher.
For achieving the above object, the present invention adopts following technical scheme, utilizes waste and old lithium ion battery to prepare the method for additive Mn Conjugate ferrite magnetostrictive material, it is characterized in that comprising the following steps:
(1) select with cobalt acid lithium and the LiFePO4 waste and old lithium ion battery that is positive electrode, waste and old lithium ion battery is split the positive electrode active materials obtained and sulfuric acid/hydrogen peroxide mixed solution leaches by solid-to-liquid ratio 1:2-6g/mL, pH=9-10 is regulated with NaOH, the Fe in complete precipitation filtrates after being filtered by leaching liquid
3+and Co
2+, filter and use washed with de-ionized water filter residue, then with nitric acid dissolve and elimination is not tolerant;
(2) Fe in the nitric acid dissolve liquid after filtering is measured with atomic absorption spectrophotometer
3+and Co
2+content, and with Co (NO
3)
26H
2o and Co (NO
3)
26H
2o or Fe (NO
3)
39H
2o regulates Fe in lysate
3+with Co
2+and Mn
2+the mol ratio of integral molar quantity is 2:1, Mn
2+with Co
2+mol ratio be X:1-X, X=0.1-0.4, then in 80 DEG C of heating water baths, in lysate, add citric acid, wherein citric acid and Fe
3+, Co
2+and Mn
2+the mol ratio of integral molar quantity is 1:1, regulate the pH=5-7 of solution, in 80 DEG C of water-baths, be heated to lysate is gel, presoma is obtained at 200 DEG C of self-propagating process 2h after gel is dried to xerogel in 120 DEG C, presoma is put into reactor and adds deionized water, in 140-200 DEG C of hydro-thermal reaction, product filtration, washing, drying obtain additive Mn cobalt ferrite powder;
(3) mass concentration dripping additive Mn cobalt ferrite powder quality 3%-5% in additive Mn cobalt ferrite powder is the polyvinyl alcohol adhesive of 8%-10%, grinding makes additive Mn cobalt ferrite powder mix with polyvinyl alcohol adhesive, then the granulation of 80-120 mesh sieve is crossed, mixture after granulation being added to diameter is in the mould of 10mm, makes the cylindrical sample base substrate of 10mm*20mm in the pressure of 10-15MPa;
(4) cylindrical sample base substrate is naturally cooled to room temperature after 100 DEG C of insulation 60min remove moisture, then in Muffle furnace, be warming up to 600-650 DEG C with the heating rate of 5 DEG C/min and be incubated after 360min removes polyvinyl alcohol adhesive and be down to room temperature with furnace temperature, finally in high temperature furnace, be warming up to 1300-1500 DEG C with the heating rate of 5 DEG C/min and be incubated 10-60min calcining, being down to the room temperature additive Mn Conjugate ferrite magnetostrictive material that namely obtained smooth surface is smooth with furnace temperature.
Further preferably, in step (1) sulfuric acid/hydrogen peroxide mixed solution, the molar concentration of sulfuric acid is 2-4mol/L, and mass concentration is the volume of the hydrogen peroxide of 30% and the mass ratio of positive electrode active materials is 0.5-1.5:1mL/g.PH=9.5 is regulated with NaOH after being filtered by leaching liquid in step (1).
The present invention has following beneficial effect: (1) waste and old lithium ion battery renewable resources, not only energy savings but also protection of the environment; (2) obtained additive Mn Conjugate ferrite magnetostrictive material have higher Magnetostriction after the match low, explore and have in magnetic force catapult-launching gear apply comparatively significantly at pressure sensor, brake, noncontacting proximity sensor, sonar.
Embodiment
Be described in further details foregoing of the present invention by the following examples, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
(1) select with cobalt acid lithium and the LiFePO4 waste and old lithium ion battery that is positive electrode, waste and old lithium ion battery is split the positive electrode active materials obtained and sulfuric acid/hydrogen peroxide mixed solution leaches by solid-to-liquid ratio 1:4g/mL, pH=9.5 is regulated with NaOH, the Fe in complete precipitation filtrates after being filtered by leaching liquid
3+and Co
2+, filter and use washed with de-ionized water filter residue, then with nitric acid dissolve and elimination is not tolerant, in sulfuric acid/hydrogen peroxide mixed solution, the molar concentration of sulfuric acid is 3mol/L, and mass concentration is the volume of the hydrogen peroxide of 30% and the mass ratio of positive electrode active materials is 1:1mL/g;
(2) Fe in the nitric acid dissolve liquid after filtering is measured with atomic absorption spectrophotometer
3+and Co
2+content, and with Co (NO
3)
26H
2o and Co (NO
3)
26H
2o or Fe (NO
3)
39H
2o regulates Fe in lysate
3+with Co
2+and Mn
2+the mol ratio of integral molar quantity is 2:1, Mn
2+with Co
2+mol ratio be 3:7, then in 80 DEG C of heating water baths, in lysate, add citric acid, wherein citric acid and Fe
3+, Co
2+and Mn
2+the mol ratio of integral molar quantity is 1:1, regulate the pH=6 of solution, in 80 DEG C of water-baths, be heated to lysate is gel, presoma is obtained at 200 DEG C of self-propagating process 2h after gel is dried to xerogel in 120 DEG C, presoma is put into reactor and adds deionized water, in 180 DEG C of hydro-thermal reactions, product filtration, washing, drying obtain additive Mn cobalt ferrite powder;
(3) mass concentration dripping additive Mn cobalt ferrite powder quality 4% in additive Mn cobalt ferrite powder is the polyvinyl alcohol adhesive of 9%, grinding makes additive Mn cobalt ferrite powder mix with polyvinyl alcohol adhesive, then 100 mesh sieve granulations are crossed, mixture after granulation being added to diameter is in the mould of 10mm, makes the cylindrical sample base substrate of 10mm*20mm in the pressure of 12MPa;
(4) cylindrical sample base substrate is naturally cooled to room temperature after 100 DEG C of insulation 60min remove moisture, then in Muffle furnace, be warming up to 620 DEG C with the heating rate of 5 DEG C/min and be incubated after 360min removes polyvinyl alcohol adhesive and be down to room temperature with furnace temperature, finally in high temperature furnace, be warming up to 1400 DEG C with the heating rate of 5 DEG C/min and be incubated 30min calcining, being down to the room temperature additive Mn Conjugate ferrite magnetostrictive material that namely obtained smooth surface is smooth with furnace temperature.
Embodiment 2
(1) select with cobalt acid lithium and the LiFePO4 waste and old lithium ion battery that is positive electrode, waste and old lithium ion battery is split the positive electrode active materials obtained and sulfuric acid/hydrogen peroxide mixed solution leaches by solid-to-liquid ratio 1:2g/mL, pH=9 is regulated with NaOH, the Fe in complete precipitation filtrates after being filtered by leaching liquid
3+and Co
2+, filter and use washed with de-ionized water filter residue, then with nitric acid dissolve and elimination is not tolerant, in sulfuric acid/hydrogen peroxide mixed solution, the molar concentration of sulfuric acid is 2mol/L, and mass concentration is the volume of the hydrogen peroxide of 30% and the mass ratio of positive electrode active materials is 0.5:1mL/g;
(2) Fe in the nitric acid dissolve liquid after filtering is measured with atomic absorption spectrophotometer
3+and Co
2+content, and with Co (NO
3)
26H
2o and Co (NO
3)
26H
2o or Fe (NO
3)
39H
2o regulates Fe in lysate
3+with Co
2+and Mn
2+the mol ratio of integral molar quantity is 2:1, Mn
2+with Co
2+mol ratio be 1:9, then in 80 DEG C of heating water baths, in lysate, add citric acid, wherein citric acid and Fe
3+, Co
2+and Mn
2+the mol ratio of integral molar quantity is 1:1, regulate the pH=5 of solution, in 80 DEG C of water-baths, be heated to lysate is gel, presoma is obtained at 200 DEG C of self-propagating process 2h after gel is dried to xerogel in 120 DEG C, presoma is put into reactor and adds deionized water, in 140 DEG C of hydro-thermal reactions, product filtration, washing, drying obtain additive Mn cobalt ferrite powder;
(3) mass concentration dripping additive Mn cobalt ferrite powder quality 3% in additive Mn cobalt ferrite powder is the polyvinyl alcohol adhesive of 8%, grinding makes additive Mn cobalt ferrite powder mix with polyvinyl alcohol adhesive, then 80 mesh sieve granulations are crossed, mixture after granulation being added to diameter is in the mould of 10mm, makes the cylindrical sample base substrate of 10mm*20mm in the pressure of 10MPa;
(4) cylindrical sample base substrate is naturally cooled to room temperature after 100 DEG C of insulation 60min remove moisture, then in Muffle furnace, be warming up to 600 DEG C with the heating rate of 5 DEG C/min and be incubated after 360min removes polyvinyl alcohol adhesive and be down to room temperature with furnace temperature, finally in high temperature furnace, be warming up to 1300 DEG C with the heating rate of 5 DEG C/min and be incubated 10min calcining, being down to the room temperature additive Mn Conjugate ferrite magnetostrictive material that namely obtained smooth surface is smooth with furnace temperature.
Embodiment 3
(1) select with cobalt acid lithium and the LiFePO4 waste and old lithium ion battery that is positive electrode, waste and old lithium ion battery is split the positive electrode active materials obtained and sulfuric acid/hydrogen peroxide mixed solution leaches by solid-to-liquid ratio 1:6g/mL, pH=10 is regulated with NaOH, the Fe in complete precipitation filtrates after being filtered by leaching liquid
3+and Co
2+, filter and use washed with de-ionized water filter residue, then with nitric acid dissolve and elimination is not tolerant, in sulfuric acid/hydrogen peroxide mixed solution, the molar concentration of sulfuric acid is 4mol/L, and mass concentration is the volume of the hydrogen peroxide of 30% and the mass ratio of positive electrode active materials is 1.5:1mL/g;
(2) Fe in the nitric acid dissolve liquid after filtering is measured with atomic absorption spectrophotometer
3+and Co
2+content, and with Co (NO
3)
26H
2o and Co (NO
3)
26H
2o or Fe (NO
3)
39H
2o regulates Fe in lysate
3+with Co
2+and Mn
2+the mol ratio of integral molar quantity is 2:1, Mn
2+with Co
2+mol ratio be 2:3, then in 80 DEG C of heating water baths, in lysate, add citric acid, wherein citric acid and Fe
3+, Co
2+and Mn
2+the mol ratio of integral molar quantity is 1:1, regulate the pH=7 of solution, in 80 DEG C of water-baths, be heated to lysate is gel, presoma is obtained at 200 DEG C of self-propagating process 2h after gel is dried to xerogel in 120 DEG C, presoma is put into reactor and adds deionized water, in 200 DEG C of hydro-thermal reactions, product filtration, washing, drying obtain additive Mn cobalt ferrite powder;
(3) mass concentration dripping additive Mn cobalt ferrite powder quality 5% in additive Mn cobalt ferrite powder is the polyvinyl alcohol adhesive of 10%, grinding makes additive Mn cobalt ferrite powder mix with polyvinyl alcohol adhesive, then 120 mesh sieve granulations are crossed, mixture after granulation being added to diameter is in the mould of 10mm, makes the cylindrical sample base substrate of 10mm*20mm in the pressure of 15MPa;
(4) cylindrical sample base substrate is naturally cooled to room temperature after 100 DEG C of insulation 60min remove moisture, then in Muffle furnace, be warming up to 650 DEG C with the heating rate of 5 DEG C/min and be incubated after 360min removes polyvinyl alcohol adhesive and be down to room temperature with furnace temperature, finally in high temperature furnace, be warming up to 1500 DEG C with the heating rate of 5 DEG C/min and be incubated 60min calcining, being down to the room temperature additive Mn Conjugate ferrite magnetostrictive material that namely obtained smooth surface is smooth with furnace temperature.
Embodiment above describes general principle of the present invention, principal character and advantage.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification just illustrates principle of the present invention; under the scope not departing from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.
Claims (3)
1. utilize waste and old lithium ion battery to prepare the method for additive Mn Conjugate ferrite magnetostrictive material, it is characterized in that comprising the following steps:
(1) select with cobalt acid lithium and the LiFePO4 waste and old lithium ion battery that is positive electrode, waste and old lithium ion battery is split the positive electrode active materials obtained and sulfuric acid/hydrogen peroxide mixed solution leaches by solid-to-liquid ratio 1:2-6g/mL, pH=9-10 is regulated with NaOH, the Fe in complete precipitation filtrates after being filtered by leaching liquid
3+and Co
2+, filter and use washed with de-ionized water filter residue, then with nitric acid dissolve and elimination is not tolerant;
(2) Fe in the nitric acid dissolve liquid after filtering is measured with atomic absorption spectrophotometer
3+and Co
2+content, and with Co (NO
3)
26H
2o and Co (NO
3)
26H
2o or Fe (NO
3)
39H
2o regulates Fe in lysate
3+with Co
2+and Mn
2+the mol ratio of integral molar quantity is 2:1, Mn
2+with Co
2+mol ratio be X:1-X, X=0.1-0.4, then in 80 DEG C of heating water baths, in lysate, add citric acid, wherein citric acid and Fe
3+, Co
2+and Mn
2+the mol ratio of integral molar quantity is 1:1, regulate the pH=5-7 of solution, in 80 DEG C of water-baths, be heated to lysate is gel, presoma is obtained at 200 DEG C of self-propagating process 2h after gel is dried to xerogel in 120 DEG C, presoma is put into reactor and adds deionized water, in 140-200 DEG C of hydro-thermal reaction, product filtration, washing, drying obtain additive Mn cobalt ferrite powder;
(3) mass concentration dripping additive Mn cobalt ferrite powder quality 3%-5% in additive Mn cobalt ferrite powder is the polyvinyl alcohol adhesive of 8%-10%, grinding makes additive Mn cobalt ferrite powder mix with polyvinyl alcohol adhesive, then the granulation of 80-120 mesh sieve is crossed, mixture after granulation being added to diameter is in the mould of 10mm, makes the cylindrical sample base substrate of 10mm*20mm in the pressure of 10-15MPa;
(4) cylindrical sample base substrate is naturally cooled to room temperature after 100 DEG C of insulation 60min remove moisture, then in Muffle furnace, be warming up to 600-650 DEG C with the heating rate of 5 DEG C/min and be incubated after 360min removes polyvinyl alcohol adhesive and be down to room temperature with furnace temperature, finally in high temperature furnace, be warming up to 1300-1500 DEG C with the heating rate of 5 DEG C/min and be incubated 10-60min calcining, being down to the room temperature additive Mn Conjugate ferrite magnetostrictive material that namely obtained smooth surface is smooth with furnace temperature.
2. the method utilizing waste and old lithium ion battery to prepare additive Mn Conjugate ferrite magnetostrictive material according to claim 1, it is characterized in that: in step (1) sulfuric acid/hydrogen peroxide mixed solution, the molar concentration of sulfuric acid is 2-4mol/L, mass concentration is the volume of the hydrogen peroxide of 30% and the mass ratio of positive electrode active materials is 0.5-1.5:1mL/g.
3. the method utilizing waste and old lithium ion battery to prepare additive Mn Conjugate ferrite magnetostrictive material according to claim 1, is characterized in that: regulate pH=9.5 with NaOH after being filtered by leaching liquid in step (1).
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Cited By (7)
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|---|---|---|---|---|
| CN106938927A (en) * | 2017-04-05 | 2017-07-11 | 河南师范大学 | The method for preparing Ni-Co ferrite magnetostriction materials using waste and old lithium ion battery doping nickel |
| CN107093779A (en) * | 2017-04-27 | 2017-08-25 | 河南师范大学 | The method that rear-earth-doped Conjugate ferrite magnetostriction materials are prepared using waste and old lithium ion battery |
| CN107331913A (en) * | 2017-07-17 | 2017-11-07 | 河南师范大学 | The method that double rear-earth-doped Conjugate ferrite magnetostriction materials are prepared using waste and old lithium ion battery |
| CN107331914A (en) * | 2017-07-17 | 2017-11-07 | 河南师范大学 | The method that the rare earth doped Conjugate ferrite magnetostriction materials of transiting state metal are prepared using waste and old lithium ion battery |
| CN107673321A (en) * | 2017-11-16 | 2018-02-09 | 海南医学院 | A kind of cadmium phosphate lithium material and its synthetic method |
| CN108258353A (en) * | 2017-12-25 | 2018-07-06 | 河南师范大学 | The method that low field intensity high-performance gallium cation doping ferrite magnetostriction materials are prepared using waste and old lithium ion battery |
| CN108258354A (en) * | 2017-12-25 | 2018-07-06 | 河南师范大学 | The method that zinc doping Conjugate ferrite magnetostriction materials are prepared using waste and old lithium ion battery |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106938927A (en) * | 2017-04-05 | 2017-07-11 | 河南师范大学 | The method for preparing Ni-Co ferrite magnetostriction materials using waste and old lithium ion battery doping nickel |
| CN107093779A (en) * | 2017-04-27 | 2017-08-25 | 河南师范大学 | The method that rear-earth-doped Conjugate ferrite magnetostriction materials are prepared using waste and old lithium ion battery |
| CN107331913A (en) * | 2017-07-17 | 2017-11-07 | 河南师范大学 | The method that double rear-earth-doped Conjugate ferrite magnetostriction materials are prepared using waste and old lithium ion battery |
| CN107331914A (en) * | 2017-07-17 | 2017-11-07 | 河南师范大学 | The method that the rare earth doped Conjugate ferrite magnetostriction materials of transiting state metal are prepared using waste and old lithium ion battery |
| CN107673321A (en) * | 2017-11-16 | 2018-02-09 | 海南医学院 | A kind of cadmium phosphate lithium material and its synthetic method |
| CN107673321B (en) * | 2017-11-16 | 2019-05-03 | 海南医学院 | A kind of cadmium phosphate lithium material and its synthetic method |
| CN108258353A (en) * | 2017-12-25 | 2018-07-06 | 河南师范大学 | The method that low field intensity high-performance gallium cation doping ferrite magnetostriction materials are prepared using waste and old lithium ion battery |
| CN108258354A (en) * | 2017-12-25 | 2018-07-06 | 河南师范大学 | The method that zinc doping Conjugate ferrite magnetostriction materials are prepared using waste and old lithium ion battery |
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