CN109326774B - Method for preparing high-performance ferric oxide/zinc ferrite composite electrode material from wet-process zinc smelting slag pickle liquor and application - Google Patents
Method for preparing high-performance ferric oxide/zinc ferrite composite electrode material from wet-process zinc smelting slag pickle liquor and application Download PDFInfo
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- CN109326774B CN109326774B CN201810828699.9A CN201810828699A CN109326774B CN 109326774 B CN109326774 B CN 109326774B CN 201810828699 A CN201810828699 A CN 201810828699A CN 109326774 B CN109326774 B CN 109326774B
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- 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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention discloses a method for preparing a high-performance ferric oxide/zinc ferrite composite electrode material from a hydrometallurgy zinc slag pickle liquor and application thereof. (1) Determination of Zn in wet-process zinc smelting slag pickle liquor2+And FeGeneral assemblyThe quantitative concentration of the substance(s). (2) Distilled water and zinc sulfate heptahydrate are added into the pickle liquor of the zinc-making slag by the wet method under the stirring at normal temperature. (3) Preparing an ammonia solution. (4) And (3) slowly dropwise adding the ammonia water solution prepared in the step (3) into the mixed solution obtained in the step (2), stirring, standing for aging, filtering, washing, and collecting a filter cake. (5) And drying and sintering the filter cake to obtain the ferric oxide/zinc ferrite composite electrode material. The method is very simple and convenient, has low cost and high yield, the preparation conditions are easy to control, and the method is suitable for large-scale production.
Description
Technical Field
The invention relates to the technical field of lithium ion battery cathode materials, in particular to a method for preparing a high-performance ferric oxide/zinc ferrite composite electrode material from a zinc hydrometallurgy slag pickle liquor and application thereof.
Technical Field
A large amount of wet smelting zinc slag is inevitably generated in the wet smelting zinc process. Because some metal elements with recovery value and heavy metal elements polluting the environment still exist in the zinc hydrometallurgy residues, the residues need to be subjected to further enhanced acid leaching treatment, so that a large amount of zinc hydrometallurgy residue acid leaching solution is generated. The wet zinc-smelting slag pickle liquor mainly contains zinc and iron ions, and also contains a very small amount of other metal impurity elements. In order to recover the zinc in the pickling liquid, it is usually necessary to first separate the zinc and iron. However, the separation process of zinc and iron is complex, the separation is not thorough, and the iron source in the leachate after separation cannot be fully utilized. Therefore, the invention provides a method for preparing a ferric oxide/zinc ferrite composite electrode material with high added value and high performance for a lithium ion battery by directly utilizing the hydrometallurgy zinc slag pickle liquor without separating zinc and iron.
Disclosure of Invention
The invention aims to provide a method for preparing a high-performance ferric oxide/zinc ferrite composite electrode material from a wet-method zinc smelting slag pickle liquor.
The method comprises the following specific steps:
(1) determination of Zn in wet-process zinc smelting slag pickle liquor2+And FeGeneral assemblyIn the amount concentration of the substance(s) of (1), wherein Zn2+The amount concentration of the substance(s) is 0.045mol/L, FeGeneral assemblyThe amount concentration of the substance (2) was 0.12 mol/L.
(2) Putting 100mL of the wet-process zinc-smelting slag pickle liquor obtained in the step (1) into a 500mL beaker, adding 100mL of distilled water into the beaker under normal-temperature stirring to enable Fe in the solutionGeneral assemblyIn an amount of 0.06mol/L, and then 0.4635g of zinc sulfate heptahydrate was added to make Zn in the solution2+With FeGeneral assemblyIn a molar ratio of 1: 2.
(3) Diluting 20-40 mL of analytically pure ammonia water by 5-10 times with distilled water, and transferring the prepared ammonia water solution to a constant-pressure separating funnel for later use.
(4) Slowly dropwise adding the ammonia water solution obtained in the step (3) into the solution obtained in the step (2) through a constant-pressure separating funnel under the condition of conventional stirring (the stirring speed is 350 revolutions per minute) at 25 ℃; after the ammonia solution is added dropwise, stirring for 3 hours, and then standing and aging for 12 hours; and (4) after aging, filtering and washing (repeating the operation for 3-5 times), and collecting a filter cake.
(5) And (3) drying the filter cake obtained in the step (4) in a drying oven at 80 ℃ for 12 hours, then transferring the filter cake into a muffle furnace, heating the filter cake to 800 ℃ from room temperature in an air atmosphere, heating the filter cake at the speed of 5 ℃/min, and sintering the filter cake for 2 hours at the temperature of 800 ℃ to obtain the ferric oxide/zinc ferrite composite electrode material.
The prepared ferric oxide/zinc ferrite composite electrode material can be applied to the preparation of high-performance lithium ion batteries.
The invention has the advantages that: the invention directly utilizes the acid leaching solution of the zinc hydrometallurgy slag to prepare the ferric oxide/zinc ferrite composite electrode material with high added value, and solves the problems that the separation of zinc and iron is difficult in industry, the iron source cannot be fully utilized, the environment is polluted, and the like. Meanwhile, the method is simple and convenient, low in cost, high in yield, easy to control preparation conditions and suitable for large-scale production, and the prepared ferric oxide/zinc ferrite composite electrode material has good cycling stability as a lithium ion battery cathode material.
Drawings
FIG. 1 is an XRD spectrum of the iron sesquioxide/zinc ferrite composite electrode material prepared in examples 1-3.
FIG. 2 is a graph showing the cycle performance of the iron trioxide/zinc ferrite composite electrode material prepared in examples 1 to 3.
FIG. 3 is a graph showing rate capability of the iron sesquioxide/zinc ferrite composite electrode material prepared in examples 1 to 3.
Detailed Description
The present invention is further described with reference to the following specific examples, which are intended to provide those skilled in the art with a better understanding of the present invention, and are not intended to limit the scope of the present invention, which is to be construed as limited thereby.
Example 1:
(1) determination of Zn in wet-process zinc smelting slag pickle liquor2+And FeGeneral assemblyIn the amount concentration of the substance(s) of (1), wherein Zn2+The amount concentration of the substance(s) is 0.045mol/L, FeGeneral assemblyThe amount concentration of the substance (2) was 0.12 mol/L.
(2) Putting 100mL of the wet-process zinc-smelting slag pickle liquor obtained in the step (1) into a 500mL beaker, adding 100mL of distilled water into the beaker under normal-temperature stirring to enable Fe in the solutionGeneral assemblyIn an amount of 0.06mol/L, and then 0.4635g of zinc sulfate heptahydrate was added to the solution to make Zn in the solution2+With FeGeneral assemblyIn a molar ratio of 1: 2.
(3) 20mL of analytically pure ammonia water is measured, diluted to 200mL by distilled water, and the prepared ammonia water solution is transferred to a constant-pressure separating funnel for later use.
(4) Slowly dropwise adding the ammonia water solution obtained in the step (3) into the solution obtained in the step (2) through a constant-pressure separating funnel under the condition of conventional stirring (the stirring speed is 350 revolutions per minute) at 25 ℃; after the ammonia solution is added dropwise, stirring for 3 hours, and then standing and aging for 12 hours; after aging, filtration and washing operations (repeated 3 times) were carried out, and the filter cake was collected.
(5) And (3) drying the filter cake obtained in the step (4) in a drying oven at 80 ℃ for 12 hours, then transferring the filter cake into a muffle furnace, heating the filter cake to 800 ℃ from room temperature in an air atmosphere, heating the filter cake at the speed of 5 ℃/min, and sintering the filter cake for 2 hours at the temperature of 800 ℃ to obtain the ferric oxide/zinc ferrite composite electrode material.
Example 2:
(1) determination of Zn in wet-process zinc smelting slag pickle liquor2+And FeGeneral assemblyIn the amount concentration of the substance(s) of (1), wherein Zn2+The amount concentration of the substance(s) is 0.045mol/L, FeGeneral assemblyThe amount concentration of the substance (2) was 0.12 mol/L.
(2) Putting 100mL of the wet-process zinc-smelting slag pickle liquor obtained in the step (1) into a 500mL beaker, adding 100mL of distilled water into the beaker under normal-temperature stirring to enable Fe in the solutionGeneral assemblyIn an amount of 0.06mol/L, and then 0.4635g of zinc sulfate heptahydrate was added to the solution to make Zn in the solution2+With FeGeneral assemblyIn a molar ratio of 1: 2.
(3) 30mL of analytically pure ammonia water is measured, diluted to 200mL by distilled water, and the prepared ammonia water solution is transferred to a constant-pressure separating funnel for later use.
(4) Slowly dripping the ammonia water solution obtained in the step (3) into the solution obtained in the step (2) through a constant-pressure separating funnel under the condition of constant-temperature conventional stirring (the stirring speed is 350 revolutions per minute) at 25 ℃; after the ammonia solution is added dropwise, stirring for 3 hours, and then standing and aging for 12 hours; after aging, filtration and washing operations (repeated 5 times) were carried out to collect a cake.
(5) And (3) drying the filter cake obtained in the step (4) in a drying oven at 80 ℃ for 12 hours, then transferring the filter cake into a muffle furnace, heating the filter cake to 800 ℃ from room temperature in an air atmosphere, heating the filter cake at the speed of 5 ℃/min, and sintering the filter cake for 2 hours at the temperature of 800 ℃ to obtain the ferric oxide/zinc ferrite composite electrode material.
Example 3:
(1) determination of Zn in wet-process zinc smelting slag pickle liquor2+And FeGeneral assemblyIn the amount concentration of the substance(s) of (1), wherein Zn2+The amount concentration of the substance(s) is 0.045mol/L, FeGeneral assemblyThe amount concentration of the substance (2) was 0.12 mol/L.
(2) Putting 100mL of the wet-process zinc-making slag pickle liquor obtained in the step (1) into a 500mL beaker, adding 100mL of distilled water into the beaker under normal-temperature stirringWater to make Fe in the solutionGeneral assemblyIn an amount of 0.06mol/L, and then 0.4635g of zinc sulfate heptahydrate was added to the solution to make Zn in the solution2+With FeGeneral assemblyIn a molar ratio of 1: 2.
(3) 40mL of analytically pure ammonia water is measured, diluted to 200mL by distilled water, and the prepared ammonia water solution is transferred to a constant-pressure separating funnel for later use.
(4) Slowly dripping the ammonia water solution obtained in the step (3) into the solution obtained in the step (2) through a constant-pressure separating funnel under the condition of constant-temperature conventional stirring (the stirring speed is 350 revolutions per minute) at 25 ℃; after the ammonia solution is added dropwise, stirring for 3 hours, and then standing and aging for 12 hours; after aging, filtration and washing operations (repeated 4 times) were carried out to collect a cake.
(5) And (3) drying the filter cake obtained in the step (4) in a drying oven at 80 ℃ for 12 hours, then transferring the filter cake into a muffle furnace, heating the filter cake to 800 ℃ from room temperature in an air atmosphere, heating the filter cake at the speed of 5 ℃/min, and sintering the filter cake for 2 hours at the temperature of 800 ℃ to obtain the ferric oxide/zinc ferrite composite electrode material.
The hydrometallurgical zinc slag pickle liquor used in the examples is only an example, in order to enable a person skilled in the art to better understand the invention, and the invention is not limited in any way.
And (3) electrochemical performance testing: the ferric oxide/zinc ferrite composite material prepared in the embodiment 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 mixture is uniformly mixed and ground according to the mass ratio of 6:3:1, a proper amount of N-methyl-2-pyrrolidone (NMP) is added, the mixture is uniformly mixed into slurry and then is uniformly coated on a copper foil, the copper foil is dried in vacuum at the temperature of 80 ℃ for 12 hours, and the electrode plate is obtained after blanking. A ferric oxide/zinc ferrite composite material electrode plate is used as a working electrode, a metal lithium plate is used as a counter electrode, a polypropylene porous membrane (Celgard 2400) is used as a diaphragm, 1mol/L of a mixed solution (v (EC): v (DMC): v (DEC): 1:1:1) of Ethylene Carbonate (EC), dimethyl carbonate (DMC) and diethyl carbonate (DEC) of LiPF6 is used as an electrolyte, and the CR2032 button cell is assembled in a glove box filled with argon. The constant-current charge and discharge performance of the battery is tested by adopting a BTS-5V/10mA type charge and discharge tester of Shenzhen Xinwei corporation, the charge and discharge voltage range is 0.01-3.0V, and the current density of the cycle performance test is 500 mA/g. The current densities of the multiplying power performance test are respectively 0.5A/g, 1A/g, 2A/g, 3A/g, 4A/g and 5A/g.
FIG. 1 shows XRD patterns of the materials prepared in examples 1 to 3. As can be seen from the figure, the material prepared by the invention is ferric oxide/zinc ferrite composite electrode material.
FIG. 2 shows the cycle performance curve of the iron sesquioxide/zinc ferrite composite electrode material prepared in examples 1-3 at a current density of 500 mA/g. As can be seen from the figure, the electrode materials prepared in examples 1-3 have better cycling stability, but the comparison of 3 examples shows that example 3 has relatively better cycling performance.
FIG. 3 shows the rate performance curves of the iron sesquioxide/zinc ferrite composite electrode materials prepared in examples 1-3 at different current densities (0.5, 1, 2, 3, 4, 5A/g). As can be seen from the figure, the electrode materials prepared in the examples 1-3 have better rate performance, but the comparison of 3 examples shows that the example 3 has relatively better rate performance.
Claims (2)
1. A method for preparing a high-performance ferric oxide/zinc ferrite composite electrode material by using a wet-method zinc smelting slag pickle liquor is characterized by comprising the following specific steps:
(1) determination of Zn in wet-process zinc smelting slag pickle liquor2+And FeGeneral assemblyIn the amount concentration of the substance(s) of (1), wherein Zn2+The amount concentration of the substance(s) is 0.045mol/L, FeGeneral assemblyThe amount concentration of the substance(s) is 0.12 mol/L;
(2) putting 100mL of the wet-process zinc-smelting slag pickle liquor obtained in the step (1) into a 500mL beaker, adding 100mL of distilled water into the beaker under normal-temperature stirring to enable Fe in the solutionGeneral assemblyIn an amount of 0.06mol/L, and then 0.4635g of zinc sulfate heptahydrate was added to make Zn in the solution2+With FeGeneral assemblyIn a molar ratio of 1: 2;
(3) diluting 20-40 mL of analytically pure ammonia water by 5-10 times with distilled water, and transferring the prepared ammonia water solution to a constant-pressure separating funnel for later use;
(4) slowly dropwise adding the ammonia water solution obtained in the step (3) into the solution obtained in the step (2) through a constant-pressure separating funnel under the conventional stirring condition that the stirring speed is 350 revolutions per minute at 25 ℃; after the ammonia solution is added dropwise, stirring for 3 hours, and then standing and aging for 12 hours; after aging, filtering and washing for 3-5 times, and collecting a filter cake;
(5) and (3) drying the filter cake obtained in the step (4) in a drying oven at 80 ℃ for 12 hours, then transferring the filter cake into a muffle furnace, heating the filter cake to 800 ℃ from room temperature in an air atmosphere, heating the filter cake at the speed of 5 ℃/min, and sintering the filter cake for 2 hours at the temperature of 800 ℃ to obtain the ferric oxide/zinc ferrite composite electrode material.
2. The application of the ferric oxide/zinc ferrite composite electrode material prepared by the preparation method according to claim 1, which is characterized in that the ferric oxide/zinc ferrite composite electrode material can be applied to the preparation of high-performance lithium ion batteries.
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Application publication date: 20190212 Assignee: Guangxi Guiren Energy Saving Technology Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2022450000610 Denomination of invention: Preparation and Application of High Performance Ferric Oxide/Zinc Ferrite Composite Electrode Materials from Zinc Hydrometallurgical Slag Acid Leaching Solution Granted publication date: 20210803 License type: Common License Record date: 20221230 |