CN109326774A - High-performance di-iron trioxide/zinc ferrite combination electrode material method and application are prepared by Zinc Hydrometallurgy Residue pickle liquor - Google Patents

High-performance di-iron trioxide/zinc ferrite combination electrode material method and application are prepared by Zinc Hydrometallurgy Residue pickle liquor Download PDF

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CN109326774A
CN109326774A CN201810828699.9A CN201810828699A CN109326774A CN 109326774 A CN109326774 A CN 109326774A CN 201810828699 A CN201810828699 A CN 201810828699A CN 109326774 A CN109326774 A CN 109326774A
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zinc
electrode material
combination electrode
iron trioxide
pickle liquor
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CN109326774B (en
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姚金环
严靖
李延伟
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Guilin University of Technology
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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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • H01M10/05—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
    • 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
    • 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
    • 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
    • H01M4/58—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
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

High-performance di-iron trioxide/zinc ferrite combination electrode material method and application are prepared by Zinc Hydrometallurgy Residue pickle liquor the invention discloses a kind of.(1) Zn in Zinc Hydrometallurgy Residue pickle liquor is measured2+And FeAlwaysSubstance withdrawl syndrome.(2) distilled water and Zinc vitriol is added into Zinc Hydrometallurgy Residue pickle liquor under stirring at normal temperature.(3) ammonia spirit is configured.(4) ammonia spirit that step (3) configure is slowly dropped in the mixed liquor of step (2) acquisition, stirring is still aging, is filtered, washed, and collects filter cake.(5) by filtration cakes torrefaction, sintering obtains di-iron trioxide/zinc ferrite combination electrode material.The method of the present invention is very easy, at low cost, yield is high, preparation condition is easily controllable, is suitable for large-scale production, and di-iron trioxide/zinc ferrite combination electrode material of preparation has preferable cyclical stability and high rate performance as lithium ion battery negative material.

Description

High-performance di-iron trioxide/zinc ferrite compound electric is prepared by Zinc Hydrometallurgy Residue pickle liquor The method and application of pole material
Technical field
The present invention relates to the technical fields of lithium ion battery negative material, and in particular to one kind is by Zinc Hydrometallurgy Residue pickle liquor Prepare high-performance di-iron trioxide/zinc ferrite combination electrode material method and application.
Technical background
A large amount of Zinc Hydrometallurgy Residue is inevitably resulted from Zinc Hydrometallurgy Process.Due to still being deposited in Zinc Hydrometallurgy Residue In the heavy metal element of some metallic elements with recovery value and pollution environment, need to carry out these slags further strong Change acidleach processing, to generate a large amount of Zinc Hydrometallurgy Residue pickle liquor.Zinc Hydrometallurgy Residue pickle liquor mainly contains zinc, iron ion, In addition to this also contain minimal amount of other metallic impurity elements.In order to recycle the zinc in pickle liquor, it usually needs first by zinc and Iron separation.However, zinc, iron separation process are complicated, separation is not thorough, and the source of iron after separating in leachate is unable to fully utilize. For this purpose, the present invention proposes that one kind directly utilizes the Zinc Hydrometallurgy Residue pickle liquor preparation high property of high added value without carrying out zinc, iron separation Lithium ion battery di-iron trioxide/zinc ferrite combination electrode material method of energy.
Summary of the invention
The purpose of the present invention is to provide one kind to prepare high-performance di-iron trioxide/zinc ferrite by Zinc Hydrometallurgy Residue pickle liquor The method of combination electrode material.
Specific steps are as follows:
(1) Zn in Zinc Hydrometallurgy Residue pickle liquor is measured2+And FeAlwaysSubstance withdrawl syndrome, wherein Zn2+Substance amount it is dense Degree is 0.045mol/L, FeAlwaysSubstance withdrawl syndrome be 0.12mol/L.
(2) the resulting Zinc Hydrometallurgy Residue pickle liquor of 100mL step (1) is put into the beaker of 500mL, under stirring at normal temperature 100mL distilled water is added into beaker, makes Fe in solutionAlwaysSubstance withdrawl syndrome be 0.06mol/L, then add 0.4635g Zinc vitriol makes Zn in solution2+With FeAlwaysMolar ratio be 1:2.
(3) 20~40mL is analyzed into pure ammonium hydroxide distilled water and dilutes 5~10 times, the ammonia spirit prepared is transferred to constant pressure It is stand-by in separatory funnel.
(4) pass through constant pressure separatory funnel under the conditions of 25 DEG C of convention stirs (350 revs/min of mixing speed) slowly to step (2) a dropping step (3) resulting ammonia spirit in acquired solution；After ammonia spirit is added dropwise to complete, stirs 3 hours, be then allowed to stand Ageing 12 hours；It after ageing, is filtered, washing operation (operating 3~5 times repeatedly), collects filter cake.
(5) filter cake that step (4) obtain is put into drying box drying 12 hours at 80 DEG C, is then transferred to horse Not in furnace, 800 DEG C are heated to from room temperature in air atmosphere, 5 DEG C/min of heating rate, is sintered 2 hours under the conditions of 800 DEG C, Obtain di-iron trioxide/zinc ferrite combination electrode material.
Obtained di-iron trioxide/zinc ferrite combination electrode material can apply to prepare high performance lithium ion battery.
Advantages of the present invention: the present invention directly prepares three oxidations two of high added value using Zinc Hydrometallurgy Residue pickle liquor Iron/zinc ferrite combination electrode material, solves industrial zinc, iron separation difficulty, and source of iron is unable to fully ask using pollution environment etc. Topic.Meanwhile the method for the present invention is very easy, at low cost, yield is high, preparation condition is easily controllable, is suitable for large-scale production, system Standby di-iron trioxide/zinc ferrite combination electrode material has preferable cyclical stability as lithium ion battery negative material.
Detailed description of the invention
Fig. 1 is di-iron trioxide/zinc ferrite combination electrode material XRD spectrum of Examples 1 to 3 preparation.
Fig. 2 is di-iron trioxide/zinc ferrite combination electrode material cycle performance figure of Examples 1 to 3 preparation.
Fig. 3 is di-iron trioxide/zinc ferrite combination electrode material high rate performance figure of Examples 1 to 3 preparation.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below, it is pointed out that following embodiment be in order to Those skilled in the art more fully understands the present invention, rather than limiting the scope of the invention, the technology people in the field Member can make some nonessential modifications and adaptations according to above content.
Embodiment 1:
(1) Zn in Zinc Hydrometallurgy Residue pickle liquor is measured2+And FeAlwaysSubstance withdrawl syndrome, wherein Zn2+Substance amount it is dense Degree is 0.045mol/L, FeAlwaysSubstance withdrawl syndrome be 0.12mol/L.
(2) the resulting Zinc Hydrometallurgy Residue pickle liquor of 100mL step (1) is put into the beaker of 500mL, under stirring at normal temperature 100mL distilled water is added into beaker, makes Fe in solutionAlwaysSubstance withdrawl syndrome be 0.06mol/L, be then added into solution 0.4635g Zinc vitriol makes Zn in solution2+With FeAlwaysMolar ratio be 1:2.
(3) it measures 20mL and analyzes pure ammonium hydroxide, be diluted to 200mL with distilled water, the ammonia spirit prepared is transferred to constant pressure It is stand-by in separatory funnel.
(4) pass through constant pressure separatory funnel under the conditions of 25 DEG C of convention stirs (350 revs/min of mixing speed) slowly to step (2) a dropping step (3) resulting ammonia spirit in acquired solution；After ammonia spirit is added dropwise to complete, stirs 3 hours, be then allowed to stand Ageing 12 hours；It after ageing, is filtered, washing operation (operating 3 times repeatedly), collects filter cake.
(5) filter cake that step (4) obtain is put into drying box drying 12 hours at 80 DEG C, is then transferred to horse Not in furnace, 800 DEG C are heated to from room temperature in air atmosphere, 5 DEG C/min of heating rate, is sintered 2 hours under the conditions of 800 DEG C, Obtain di-iron trioxide/zinc ferrite combination electrode material.
Embodiment 2:
(1) Zn in Zinc Hydrometallurgy Residue pickle liquor is measured2+And FeAlwaysSubstance withdrawl syndrome, wherein Zn2+Substance amount it is dense Degree is 0.045mol/L, FeAlwaysSubstance withdrawl syndrome be 0.12mol/L.
(2) the resulting Zinc Hydrometallurgy Residue pickle liquor of 100mL step (1) is put into the beaker of 500mL, under stirring at normal temperature 100mL distilled water is added into beaker, makes Fe in solutionAlwaysSubstance withdrawl syndrome be 0.06mol/L, be then added into solution 0.4635g Zinc vitriol makes Zn in solution2+With FeAlwaysMolar ratio be 1:2.
(3) it measures 30mL and analyzes pure ammonium hydroxide, be diluted to 200mL with distilled water, the ammonia spirit prepared is transferred to constant pressure It is stand-by in separatory funnel.
(4) under the conditions of 25 DEG C of constant temperature convention stirs (350 revs/min of mixing speed) by constant pressure separatory funnel slowly to A dropping step (3) resulting ammonia spirit in step (2) acquired solution；After ammonia spirit is added dropwise to complete, stirring 3 hours, then Still aging 12 hours；It after ageing, is filtered, washing operation (operating 5 times repeatedly), collects filter cake.
(5) filter cake that step (4) obtain is put into drying box drying 12 hours at 80 DEG C, is then transferred to horse Not in furnace, 800 DEG C are heated to from room temperature in air atmosphere, 5 DEG C/min of heating rate, is sintered 2 hours under the conditions of 800 DEG C, Obtain di-iron trioxide/zinc ferrite combination electrode material.
Embodiment 3:
(1) Zn in Zinc Hydrometallurgy Residue pickle liquor is measured2+And FeAlwaysSubstance withdrawl syndrome, wherein Zn2+Substance amount it is dense Degree is 0.045mol/L, FeAlwaysSubstance withdrawl syndrome be 0.12mol/L.
(2) the resulting Zinc Hydrometallurgy Residue pickle liquor of 100mL step (1) is put into the beaker of 500mL, under stirring at normal temperature 100mL distilled water is added into beaker, makes Fe in solutionAlwaysSubstance withdrawl syndrome be 0.06mol/L, be then added into solution 0.4635g Zinc vitriol makes Zn in solution2+With FeAlwaysMolar ratio be 1:2.
(3) it measures 40mL and analyzes pure ammonium hydroxide, be diluted to 200mL with distilled water, the ammonia spirit prepared is transferred to constant pressure It is stand-by in separatory funnel.
(4) under the conditions of 25 DEG C of constant temperature convention stirs (350 revs/min of mixing speed) by constant pressure separatory funnel slowly to A dropping step (3) resulting ammonia spirit in step (2) acquired solution；After ammonia spirit is added dropwise to complete, stirring 3 hours, then Still aging 12 hours；It after ageing, is filtered, washing operation (operating 4 times repeatedly), collects filter cake.
(5) filter cake that step (4) obtain is put into drying box drying 12 hours at 80 DEG C, is then transferred to horse Not in furnace, 800 DEG C are heated to from room temperature in air atmosphere, 5 DEG C/min of heating rate, is sintered 2 hours under the conditions of 800 DEG C, Obtain di-iron trioxide/zinc ferrite combination electrode material.
Zinc Hydrometallurgy Residue pickle liquor used by each embodiment is only citing, in order to enable those skilled in the art to more The present invention is understood well, but the present invention is not imposed any restrictions.
Electrochemical property test: it using di-iron trioxide/zinc ferrite composite material of embodiment preparation as active material, leads Electric carbon black (Super P) is used as conductive agent, and Kynoar (PVDF) is ground as the ratio mixing of binder 6:3:1 in mass ratio After mill is uniform, suitable n-methyl-2-pyrrolidone (NMP) is added, mixes well and is coated uniformly on copper foil after being slurried, at 80 DEG C Vacuum drying 12 hours, obtains electrode slice after punching.Using di-iron trioxide/zinc ferrite composite electrode piece as working electrode, Metal lithium sheet is to electrode, and polypropylene porous film (Celgard 2400) is diaphragm, the ethylene carbonate of 1mol/L LiPF6 (EC), the mixed liquor (v (EC): v (DMC): v (DEC)=1:1:1) of dimethyl carbonate (DMC) and diethyl carbonate (DEC) is electricity Liquid is solved, is assembled into CR2032 type button cell in the glove box full of argon gas.Using the BTS-5V/10mA of Shenzhen Xin Wei company Type charge-discharge test instrument tests the constant current charge-discharge performance of battery, and charging/discharging voltage range is 0.01~3.0V, and cycle performance is surveyed The current density of examination is 500mA/g.High rate performance test current density be respectively 0.5A/g, 1A/g, 2A/g, 3A/g, 4A/g, 5A/g。
As shown in Figure 1, the XRD spectrum of the material for Examples 1 to 3 preparation.It can be seen from the figure that prepared by the present invention Material is di-iron trioxide/zinc ferrite combination electrode material.
As shown in Fig. 2, di-iron trioxide/zinc ferrite combination electrode material for Examples 1 to 3 preparation is electric in 500mA/g Cycle performance curve under current density.It can be seen from the figure that the electrode material of Examples 1 to 3 preparation has preferable circulation Stability, but 3 embodiments are compared it is found that embodiment 3 has relatively better cycle performance.
As shown in figure 3, di-iron trioxide/zinc ferrite combination electrode material for Examples 1 to 3 preparation is close in different electric currents Spend the high rate performance curve under (0.5,1,2,3,4,5A/g).It can be seen from the figure that the electrode material of Examples 1 to 3 preparation With preferable high rate performance, but 3 embodiments are compared it is found that embodiment 3 has relatively better high rate performance.

Claims (2)

1. a kind of prepare high-performance di-iron trioxide/zinc ferrite combination electrode material method by Zinc Hydrometallurgy Residue pickle liquor, It is characterized in that specific steps are as follows:
(1) Zn in Zinc Hydrometallurgy Residue pickle liquor is measured2+And FeAlwaysSubstance withdrawl syndrome, wherein Zn2+Substance withdrawl syndrome be 0.045mol/L, FeAlwaysSubstance withdrawl syndrome be 0.12mol/L；
(2) the resulting Zinc Hydrometallurgy Residue pickle liquor of 100mL step (1) is put into the beaker of 500mL, to burning under stirring at normal temperature 100mL distilled water is added in cup, makes Fe in solutionAlwaysSubstance withdrawl syndrome be 0.06mol/L, then add 0.4635g seven Zinc sulphate hydrate makes Zn in solution2+With FeAlwaysMolar ratio be 1:2；
(3) 20~40mL is analyzed into pure ammonium hydroxide distilled water and dilutes 5~10 times, the ammonia spirit prepared is transferred to constant pressure liquid separation It is stand-by in funnel；
(4) pass through constant pressure separatory funnel under the conditions of 25 DEG C 350 revs/min of mixing speed of convention stir slowly to step (2) A dropping step (3) resulting ammonia spirit in acquired solution；After ammonia spirit is added dropwise to complete, stirs 3 hours, be then allowed to stand ageing 12 hours；It after ageing, is filtered, washs 3~5 times, collect filter cake；
(5) filter cake that step (4) obtain is put into drying box drying 12 hours at 80 DEG C, is then transferred to Muffle furnace In, 800 DEG C are heated to from room temperature in air atmosphere, 5 DEG C/min of heating rate, is sintered 2 hours, obtains under the conditions of 800 DEG C Di-iron trioxide/zinc ferrite combination electrode material.
2. di-iron trioxide/zinc ferrite combination electrode material application of preparation method preparation according to claim 1, It is characterized in that the di-iron trioxide/zinc ferrite combination electrode material can apply to prepare high performance lithium ion battery.
CN201810828699.9A 2018-07-25 2018-07-25 Method for preparing high-performance ferric oxide/zinc ferrite composite electrode material from wet-process zinc smelting slag pickle liquor and application Active CN109326774B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103094558A (en) * 2012-12-18 2013-05-08 深圳市贝特瑞新能源材料股份有限公司 Zinc-ferrite-based nanometer composite as well as preparation method and application thereof
CN105449193A (en) * 2015-11-24 2016-03-30 桂林理工大学 Method for preparing high-performance zinc ferrite electrode material in assistance of P123
CN106025271A (en) * 2016-05-31 2016-10-12 山东玉皇新能源科技有限公司 Preparation method of negative electrode material zinc ferrite
CN108269980A (en) * 2018-01-03 2018-07-10 桂林理工大学 A kind of method for preparing high-performance di-iron trioxide/zinc ferrite combination electrode material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103094558A (en) * 2012-12-18 2013-05-08 深圳市贝特瑞新能源材料股份有限公司 Zinc-ferrite-based nanometer composite as well as preparation method and application thereof
CN105449193A (en) * 2015-11-24 2016-03-30 桂林理工大学 Method for preparing high-performance zinc ferrite electrode material in assistance of P123
CN106025271A (en) * 2016-05-31 2016-10-12 山东玉皇新能源科技有限公司 Preparation method of negative electrode material zinc ferrite
CN108269980A (en) * 2018-01-03 2018-07-10 桂林理工大学 A kind of method for preparing high-performance di-iron trioxide/zinc ferrite combination electrode material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
姚金环: "超声波强化浸出湿法炼锌渣及浸出液制备纳米多孔铁酸锌电极材料的研究", 《科技成果》 *

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Denomination of invention: Preparation and Application of High Performance Ferric Oxide/Zinc Ferrite Composite Electrode Materials from Zinc Hydrometallurgical Slag Acid Leaching Solution

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