CN112047384B - Method for preparing nano iron oxide negative electrode material for lithium ion battery by using tin ore tailing sulfuric acid leaching solution - Google Patents
Method for preparing nano iron oxide negative electrode material for lithium ion battery by using tin ore tailing sulfuric acid leaching solution Download PDFInfo
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 57
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 52
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002386 leaching Methods 0.000 title claims abstract description 27
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 20
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052742 iron Inorganic materials 0.000 claims abstract description 14
- 239000010406 cathode material Substances 0.000 claims abstract description 6
- 238000004108 freeze drying Methods 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims abstract description 6
- 239000002243 precursor Substances 0.000 claims description 25
- 239000000126 substance Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- -1 iron ion Chemical class 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000012716 precipitator Substances 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 48
- 239000000463 material Substances 0.000 description 5
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 4
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000000349 field-emission scanning electron micrograph Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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Abstract
The invention discloses a method for preparing a nano iron oxide cathode material for a lithium ion battery by using a tin ore tailing sulfuric acid leaching solution. Directly taking a tin ore tailing sulfuric acid leaching solution as a raw material, controlling the concentration and the pH value of the leaching solution and the pH value at the end of precipitation, and combining freeze drying and sintering technologies to prepare the iron oxide negative electrode material with mutually bridged nanoparticles. The invention provides a new way for high-value utilization of iron resources in the sulfuric acid leaching solution of tin ore tailings, improves the utilization rate of the tin ore tailings resources and reduces the environmental pollution. Meanwhile, the preparation method is simple, the conditions are easy to control, the cost is low, the method is suitable for large-scale production, and the prepared nano iron oxide serving as the lithium ion battery cathode material has good cycle stability and rate capability.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a method for preparing a nano iron oxide cathode material for a lithium ion battery by using a tin ore tailing sulfuric acid leaching solution.
Background
Certain tin ore is mined underground to produce a large amount of tailings. Tin ore tailings, which is one of industrial solid wastes, mainly consists of oxides of iron, silicon, aluminum and calcium. Iron in the tailings cannot meet the iron-making requirement, and the recovery value is low, so that a large amount of tin ore tailings are stacked for a long time, land resources are occupied, and simultaneously, the waste of valuable resources and the serious environmental pollution are caused. In recent years, leaching slag or tailings and recovering valuable metals from the leaching solution are becoming an important method for resource utilization of slag or tailings. However, related researches on resource utilization of tin ore tailing leachate are only reported, and therefore, the invention provides a method for preparing a nano iron oxide negative electrode material for a high-performance lithium ion battery by directly using tin ore tailing sulfuric acid leachate as a raw material.
Disclosure of Invention
The invention aims to provide a method for preparing a nano iron oxide negative electrode material for a lithium ion battery by using a tin ore tailing sulfuric acid leaching solution.
The method comprises the following specific steps:
(1) And measuring the quantity concentration of total iron ion substances in the tin ore tailing sulfuric acid leaching solution and the pH value of the solution, and adjusting the quantity concentration of the total iron ion substances in the solution to be 0.65 mol/L and the pH value of the solution to be 0.44 according to the measurement result.
(2) And (3) putting 100 mL of deionized water into a 500 mL beaker, adding 30 mL of the solution obtained in the step (1) into the beaker, and uniformly stirring to obtain the tin ore tailing sulfuric acid leaching solution diluted solution.
(3) Placing the beaker containing the diluted solution of the sulfuric acid leaching solution of the tin ore tailings in the step (2) on a constant-temperature heating magnetic stirrer, and dropwise adding a precipitator with the concentration of 1 mol/L into the beaker through a constant-pressure separating funnel under the magnetic stirring at the stirring speed of 350 revolutions per minute at the temperature of 25 ℃ until the pH value of the solution is 4; and after the dropwise addition is finished, continuously stirring for 3 hours, standing and aging for 12 hours, filtering and washing after aging until the filtrate is neutral, and collecting a filter cake.
(4) And (4) freeze-drying the filter cake obtained in the step (3) for 3 days to obtain a precursor.
(5) And (3) placing the precursor obtained in the step (4) into a muffle furnace, heating the precursor from room temperature to 800 ℃ at the heating rate of 5 ℃/min in the air atmosphere, sintering the precursor at the constant temperature of 800 ℃ for 2 hours, and cooling the sintered precursor to room temperature along with the furnace to obtain the nano iron oxide cathode material for the lithium ion battery.
And (3) the precipitator in the step (3) is one of sodium carbonate, sodium hydroxide and ammonia water.
The invention has the advantages that: the invention provides a new way for high-value utilization of iron resources in the sulfuric acid leaching solution of tin ore tailings, improves the utilization rate of the tin ore tailings resources and reduces the environmental pollution. Meanwhile, the method disclosed by the invention is simple in preparation method, easy in condition control, low in cost and suitable for large-scale production, and the prepared nano iron oxide negative electrode material for the lithium ion battery has better cycling stability and rate capability.
Drawings
FIG. 1 is an XRD spectrum of the nano iron oxide negative electrode materials for lithium ion batteries prepared in examples 1 to 3.
FIG. 2 is an FESEM image of the nano iron oxide negative electrode materials for lithium ion batteries prepared in examples 1 to 3.
FIG. 3 is a diagram showing cycle characteristics of the nano iron oxide negative electrode materials for lithium ion batteries prepared in examples 1 to 3.
FIG. 4 is a graph showing rate capability of the nano iron oxide negative electrode materials for lithium ion batteries prepared in examples 1 to 3.
Detailed Description
The present invention is further described with reference to the following examples, which are intended to enable those skilled in the art to better understand the present invention without limiting the scope of the present invention, and which are intended to be modified and adapted by the skilled in the art.
Example 1:
(1) Measuring the quantity concentration of total iron ion substances in the tin ore tailing sulfuric acid leaching solution and the pH value of the solution to obtain the quantity concentration of the total iron ion substances in the solution of 0.65 mol/L, wherein the Fe content is 3+ The amount concentration of the substance(s) is 0.37 mol/L, fe 2+ The amount concentration of the substance (2) was 0.28 mol/L, and the pH of the solution was 0.44.
(2) And (2) putting 100 mL of deionized water into a 500 mL beaker, slowly adding 30 mL of the solution obtained in the step (1) into the beaker, and uniformly stirring to obtain the tin ore tailing sulfuric acid leaching solution diluted solution.
(3) And (3) placing the beaker filled with the diluted solution of the sulfuric acid leaching solution of the tin ore tailings in the step (2) on a constant-temperature heating magnetic stirrer, and dropwise adding a sodium carbonate solution with the concentration of 1 mol/L into the beaker through a constant-pressure separating funnel under the condition of magnetic stirring at the temperature of 25 ℃ (the stirring speed is 350 r/min) until the pH value of the solution is 4. And after the dropwise addition is finished, stirring is continuously carried out for 3 hours, then standing and aging are carried out for 12 hours, filtering and washing operations are carried out after aging until the filtrate is neutral, and a filter cake is collected.
(4) And (4) freeze-drying the filter cake obtained in the step (3) for 3 days to obtain a precursor.
(5) And (5) placing the precursor obtained in the step (4) in a muffle furnace, heating the precursor to 800 ℃ from room temperature in an air atmosphere (the heating rate is 5 ℃/min), sintering the precursor at the constant temperature of 800 ℃ for 2 hours, and cooling the sintered precursor to room temperature along with the furnace to obtain the nano ferric oxide negative electrode material for the lithium ion battery.
Example 2:
(1) Measuring the quantity concentration of total iron ion substances in the tin ore tailing sulfuric acid leaching solution and the pH value of the solution to obtain the quantity concentration of the total iron ion substances in the solution of 0.65 mol/L, wherein the Fe content is 3+ The amount concentration of the substance(s) is 0.37 mol/L, fe 2+ The amount concentration of the substance (2) was 0.28 mol/L, and the pH of the solution was 0.44.
(2) And (2) putting 100 mL of deionized water into a 500 mL beaker, slowly adding 30 mL of the solution obtained in the step (1) into the beaker, and uniformly stirring to obtain the tin ore tailing sulfuric acid leaching solution diluted solution.
(3) And (3) placing the beaker containing the diluted solution of the sulfuric acid leaching solution of the tin ore tailings in the step (2) on a constant-temperature heating magnetic stirrer, and dropwise adding a sodium hydroxide solution with the concentration of 1 mol/L into the beaker through a constant-pressure separating funnel under the condition of magnetic stirring at the temperature of 25 ℃ (the stirring speed is 350 r/min) until the pH value of the solution is 4. And after the dropwise addition is finished, stirring is continuously carried out for 3 hours, then standing and aging are carried out for 12 hours, filtering and washing operations are carried out after aging until the filtrate is neutral, and a filter cake is collected.
(4) And (4) freeze-drying the filter cake obtained in the step (3) for 3 days to obtain a precursor.
(5) And (3) placing the precursor obtained in the step (4) in a muffle furnace, heating the precursor to 800 ℃ from room temperature in an air atmosphere, sintering the precursor at the constant temperature of 800 ℃ for 2 hours, and cooling the precursor to room temperature along with the furnace to obtain the nano ferric oxide negative electrode material for the lithium ion battery.
Example 3:
(1) Measuring the quantity concentration of total iron ion substances in the tin ore tailing sulfuric acid leaching solution and the pH value of the solution to obtain the quantity concentration of the total iron ion substances in the solution of 0.65 mol/L, wherein the Fe 3+ The amount concentration of the substance(s) is 0.37 mol/L, fe 2+ The amount concentration of the substance (2) was 0.28 mol/L, and the pH of the solution was 0.44.
(2) And (3) putting 100 mL of deionized water into a 500 mL beaker, slowly adding 30 mL of the solution obtained in the step (1) into the beaker, and uniformly stirring to obtain the tin ore tailing sulfuric acid leaching solution diluted solution.
(3) And (3) placing the beaker filled with the diluted solution of the sulfuric acid leaching solution of the tin ore tailings in the step (2) on a constant-temperature heating magnetic stirrer, and dropwise adding an ammonia water solution with the concentration of 1 mol/L into the beaker through a constant-pressure separating funnel under the condition of magnetic stirring at the temperature of 25 ℃ (the stirring speed is 350 r/min) until the pH value of the solution is 4. And after the dropwise addition is finished, stirring is continuously carried out for 3 hours, then standing and aging are carried out for 12 hours, filtering and washing operations are carried out after aging until the filtrate is neutral, and a filter cake is collected.
(4) And (4) freeze-drying the filter cake obtained in the step (3) for 3 days to obtain a precursor.
(5) And (5) placing the precursor obtained in the step (4) in a muffle furnace, heating the precursor to 800 ℃ from room temperature in an air atmosphere (the heating rate is 5 ℃/min), sintering the precursor at the constant temperature of 800 ℃ for 2 hours, and cooling the sintered precursor to room temperature along with the furnace to obtain the nano ferric oxide negative electrode material for the lithium ion battery.
The sulfuric acid leachate of tin ore tailings used in examples 1 to 3 are only examples, and are not intended to limit the present invention in any way, so as to enable those skilled in the art to better understand the present invention.
And (3) electrochemical performance testing: the nano iron oxide negative electrode material for the lithium ion battery prepared in the examples 1 to 3 is used as an active material, conductive carbon black (Super P) is used as a conductive agent, polyvinylidene fluoride (PVDF) is used as a binder, the materials are mixed and uniformly ground according to the mass ratio of 7. Taking an iron oxide electrode plate as a working electrode, a metal lithium plate as a counter electrode, a polypropylene porous membrane (Celgard 2400) as a diaphragm and 1 mol/L LiPF 6 A mixed solution of Ethylene Carbonate (EC), dimethyl carbonate (DMC) and diethyl carbonate (DEC) (volume ratio, v (EC): v (DMC) = v (DEC) = 1) as an electrolyte solution, and assembled into a CR2016 type button half cell in a glove box filled with argon gas. Constant current charge and discharge tester for testing battery by adopting BTS-5V/10 mA type multichannel charge and discharge tester of Shenzhen Xinwei corporationThe electrical property, the charging and discharging voltage range is 0.01 to 3.0V, the cycle performance test is firstly carried out at 0.2A g -1 Cycling at current density for 10 cycles, then at 0.5A g -1 The current density cycles 290 turns. The current density of the multiplying power performance test is 0.2A g respectively -1 、0.5 A g -1 、1 A g -1 、2 A g -1 、3 A g -1 、4 A g -1 。
As shown in FIG. 1, XRD patterns of the materials prepared in examples 1 to 3 were obtained. As can be seen from the figure, the material prepared by the invention is ferric oxide (alpha-Fe) 2 O 3 ) And (3) a negative electrode material.
As shown in fig. 2, FESEM images of the iron oxide negative electrode materials prepared in examples 1 to 3 were obtained. As can be seen from the figure, the iron oxide cathode material prepared by the invention is composed of nanometer spheroidal particles which are mutually bridged.
As shown in FIG. 3, the weight of the nano iron oxide negative electrode materials prepared in examples 1 to 3 was 0.2A g -1 Circulating for 10 circles under the current density and then 0.5A g -1 Cycling performance curve for 290 cycles at current density. As can be seen from the figures, the electrode materials prepared in examples 1 to 3 have better cycle stability. Among them, the nano iron oxide electrode prepared in example 1 has relatively best cycle performance, followed by the nano iron oxide electrodes prepared in examples 2 and 3. The electrode material prepared in example 1 was at 0.2 ag -1 Circulating for 10 circles under the current density and then 0.5A g -1 After 290 circles of circulation under the current density, the discharge specific capacity and the charge specific capacity can still respectively reach 1146 mAh g and 1129 mAh g -1 The coulomb efficiency was 98.5%.
As shown in FIG. 4, the nano-iron oxide electrodes prepared in examples 1 to 3 were used at different current densities (0.2, 0.5, 1, 2, 3, 4 Ag) -1 ) Rate performance curve below. As can be seen from the figure, the nano iron oxide electrodes prepared in the examples 1 to 3 have better rate capability. Among them, the rate capability of the nano iron oxide electrode prepared in example 1 is the best, followed by the nano iron oxide electrodes prepared in examples 2 and 3. At 0.2, 0.5, 1, 2, 3, 4 ag -1 The specific discharge/charge capacities of the electrodes of the material prepared in example 1 at current densities were 755/705, respectively578/558, 454/441, 342/333, 280/274 and 236/233 mAh g -1 . When the current density returns to 0.2 ag -1 After 50 cycles, the discharge/charge specific capacity of the electrode made of the material prepared in the example 1 can be recovered to 621/617 mAh g -1 (ii) a When the current density is again from 0.5 ag -1 Gradually increases to 4 Ag -1 The specific discharge/charge capacities are respectively restored to 559/555, 508/505, 449/447, 410/408 and 377/374 mAh g -1 。
Claims (1)
1. A method for preparing a nano iron oxide negative electrode material for a lithium ion battery by using a tin ore tailing sulfuric acid leaching solution is characterized by comprising the following specific steps:
(1) Measuring the quantity concentration of total iron ion substances in the tin ore tailing sulfuric acid leaching solution and the pH value of the solution, and adjusting the quantity concentration of the total iron ion substances in the solution to be 0.65 mol/L and the pH value of the solution to be 0.44 according to the measurement result;
(2) Putting 100 mL of deionized water into a 500 mL beaker, adding 30 mL of the solution obtained in the step (1) into the beaker, and uniformly stirring to obtain a tin ore tailing sulfuric acid leaching solution diluted solution;
(3) Placing the beaker containing the diluted solution of the sulfuric acid leaching solution of the tin ore tailings in the step (2) on a constant-temperature heating magnetic stirrer, and dropwise adding a precipitator with the concentration of 1 mol/L into the beaker through a constant-pressure separating funnel under the magnetic stirring at the stirring speed of 350 revolutions per minute at the temperature of 25 ℃ until the pH value of the solution is 4; after the dropwise adding is finished, continuously stirring for 3 hours, then standing and aging for 12 hours, filtering and washing the mixture after aging until the filtrate is neutral, and collecting a filter cake;
(4) Freeze-drying the filter cake obtained in the step (3) for 3 days to obtain a precursor;
(5) Placing the precursor obtained in the step (4) in a muffle furnace, heating the precursor from room temperature to 800 ℃ at a heating rate of 5 ℃/min in the air atmosphere, sintering the precursor at the constant temperature of 800 ℃ for 2 hours, and cooling the precursor to room temperature along with the furnace to obtain the nano iron oxide cathode material for the lithium ion battery;
and (4) the precipitator in the step (3) is one of sodium carbonate, sodium hydroxide and ammonia water.
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Application publication date: 20201208 Assignee: GUANGXI JISHUN ENERGY TECHNOLOGY Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980045027 Denomination of invention: Method for preparing nano iron oxide negative electrode materials for lithium-ion batteries using sulfuric acid leaching solution from tin ore tailings Granted publication date: 20221111 License type: Common License Record date: 20231101 Application publication date: 20201208 Assignee: GUANGXI BINYANG COUNTY RONGLIANG AGRICULTURAL TECHNOLOGY CO.,LTD. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044910 Denomination of invention: Method for preparing nano iron oxide negative electrode materials for lithium-ion batteries using sulfuric acid leaching solution from tin ore tailings Granted publication date: 20221111 License type: Common License Record date: 20231101 |
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Application publication date: 20201208 Assignee: Guilin Xing GUI Electrical Appliance Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044499 Denomination of invention: Method for preparing nano iron oxide negative electrode materials for lithium-ion batteries using sulfuric acid leaching solution from tin ore tailings Granted publication date: 20221111 License type: Common License Record date: 20231030 |