CN104409791B - Prepare the method for flower-shaped nickel hydroxide electrode material from waste battery - Google Patents
Prepare the method for flower-shaped nickel hydroxide electrode material from waste battery Download PDFInfo
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- CN104409791B CN104409791B CN201410647680.6A CN201410647680A CN104409791B CN 104409791 B CN104409791 B CN 104409791B CN 201410647680 A CN201410647680 A CN 201410647680A CN 104409791 B CN104409791 B CN 104409791B
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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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
- 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
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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 kind of method of preparing flower-shaped nickel hydroxide electrode material from waste battery, it is that Nickel-bearing Waste rechargeable batteries powder is heated in water-bath, adds 95% fuming nitric aicd, centrifugal mixer, filter, get filtered fluid in hydrothermal reaction kettle, then add surfactant and industrial ammonia, then by hydrothermal reaction kettle, add thermal response 10～20h, be precipitated, then by washing of precipitate, oven dry, grinding, obtain having the nickel hydroxide superfines of chrysanthemum flower-like structure. Nickel hydroxide prepared by the present invention has the advantages such as chrysanthemum shape, high-purity, particle size be even, simultaneously, preparation method one of the present invention directly extracts and prepares nickel hydroxide from electronic waste, overcome China's nickel problem that there is lack of raw materials, the 2nd, adopt hydro-thermal method to prepare particle size homogeneous, chrysanthemum shape nickel hydroxide, overcome the problems such as ball-shape nickel hydroxide capacity is little, adapt to the demand of the large capacity of Ni-MH power cell, lightweight development.
Description
Technical field
The present invention relates to a kind of method of preparing nickel hydroxide electrode material from waste battery, relate in particular to a kind of from discardedIn battery, reclaim electron wastes, prepare the method for flower-shaped nickel hydroxide electrode material.
Background technology
The Nickel-cobalt resources of China lacks, and country is every year all by a large amount of foreign exchange import nickel minerals and deep processing resource, along with ore depositThe exhaustion of producing this non-renewable resources of resource, non-ferrous metal emphasis from now on will turn to the recovery profit of non-ferrous metal in discarded objectWith. In waste and old ni-mh, nickel-cadmium cell and production waste thereof and electroplating industry solid waste, contain heavy metal nickel, cobalt, rare earth goldBelong to etc., if do not recycled, not only environment is caused to great pollution, and wasted the metal money of national strategySource. In the today of being becoming tight resource day, the recycling of waste secondary battery and production waste thereof can not only be saved limitedMetallic mineral resources, is conducive to the sustainable development of national economy, and goes out the complete of metal from exploration, exploitation, ore dressing to metallurgyProcess considers the impact of environment, and the recycling integrated cost of waste secondary battery is lower, and its meaning is brighterAobvious.
Ni-MH battery is a kind of novel high-energy battery, is have the reality property used in electric motor car Application and Development process movingPower source. As compared with sodium sulphur, lithium ion, polymer Li-ion battery, Ni-MH battery has with other high energy battery systemsOvercharging resisting and cross exoergic power, pollution-free, low cost and high-energy-density and large current density electrical dominance, becomes electric automobileFirst-selected power supply. And for power-type Ni-H battery, the volume of battery and specific discharge capacity, large current density power, cyclicityCan with and serviceability under varying environment become the principal element of its development of restriction. Above-mentioned all in order to solveProblem, as the performance of the active material of the battery important component part especially positive electrode of battery be processed in order to affect" bottleneck " problem that battery performance improves. As the positive pole of Ni-MH battery, nickel electrode will adapt to larger charging and discharging currents, meetsHarsher environment for use, specific energy will significantly improve, and therefore, carries out the research of active material of nickel electrode nickel hydroxide is hadVery important realistic meaning. Nickel hydroxide subject matter is at present: (1) specific capacitance is on the low side; (2) particle diameter of particle distributes notAll and crystal grain larger, thereby bulk density is not very high; (3) crystalline structure is unfavorable for electrode high current charge-discharge and cycle lifeRaising. Because nickel hydroxide is not only the positive electrode of Ni-MH battery, it is also the anodal material of Ni/Cd, Ni/Fe, Ni/Zn batteryMaterial, therefore, the preparation technology of Study of Hydrogen nickel oxide, produces high performance nickel hydroxide electrode material and not only can improve ni-mhThe chemical property of battery, also can make the overall performance of other nickel series battery improve a lot.
Have not yet to see the report of preparing flower-shaped High Purity Hydrogen nickel oxide cell positive material with battery discarded object, flower-shaped hydrogenNickel oxide is large than spherical nickel hydroxide specific area, contributes to improve battery capacity. Along with power vehicle high capacity lightweightQuantize requirement, flower-shaped High Purity Hydrogen nickel oxide electrode developing material will more and more be subject to people and pay close attention to.
Summary of the invention
Technical problem to be solved by this invention is the defect that overcomes prior art, provides a kind of from waste battery preparation flowerThe method of shape nickel hydroxide electrode material, the nickel hydroxide of preparation has the advantages such as chrysanthemum shape, high-purity, particle size be even,This preparation method one directly extracts and prepares high-purity hydrogen nickel oxide from electronic waste, and what overcome China's nickel there is lack of raw materials asksTopic, the 2nd, adopt hydro-thermal method to prepare particle size homogeneous, chrysanthemum shape nickel hydroxide, overcome the little grade of ball-shape nickel hydroxide capacity and askTopic, the demand of the large capacity of adaptation Ni-MH power cell, lightweight development.
The technical solution adopted for the present invention to solve the technical problems is: one is prepared flower-shaped nickel hydroxide from waste batteryThe method of electrode material, comprises the following steps:
(1) Nickel-bearing Waste rechargeable batteries are shattered to taking 100 grams after 100 orders and be placed in 500ml beaker, measure with graduated cylinder200ml distilled water joins in above-mentioned beaker, and magnetic agitation, puts into water-bath by beaker, heating water bath to 60～80 DEG C;
(2) measuring concentration with graduated cylinder is that 95% fuming nitric aicd 50ml joins in above-mentioned beaker, is put on magnetic stirring apparatusMagnetic agitation, rotating speed is controlled at 500～800r/min, continues to stir 60min, and temperature remains on 60～80 DEG C; Then naturally coldBut;
(3) separate above-mentioned solid-liquid mixing system with centrifuge, measure filtered fluid 200ml and proceed to hydrothermal reaction kettle and make componentA；
(4) measure in water-bath distilled water 20～30ml in small beaker with pipette, add surfactant 0.1～0.5mmol, adds industrial ammonia 50-80ml, stirs and obtains B component with glass;
(5) B component is slowly joined in component A, magnetic agitation is even;
(6) by hydrothermal reaction kettle, at 180～250 DEG C, react 10～20h, be precipitated;
(7) distilled water, the absolute ethanol washing for white precipitate that step (6) are obtained are for several times, super with supersonic wave cleaning machineSound 5～20min, for several times, the precipitation then suction filtration being obtained is put into drying box to suction filtration, and at 80～100 DEG C, dry 16～24h grindsAfter mill, obtain having the nickel hydroxide superfines of chrysanthemum flower-like structure.
Further, in described step (1): water bath heating temperature is 70 DEG C.
Further, in described step (2): magnetic agitation changes 600r/min into.
Further, in described step (4): industrial ammonia amount is 60ml, amount of surfactant is 0.2mmol, lives in surfaceProperty agent can be neopelex, polyethylene glycol, polyvinylpyrrolidone, softex kw, 12One or more in sodium alkyl sulfate, dodecylphosphoric acid monoesters di-potassium.
Further, in described step (6): temperature is controlled at 200 DEG C, the reaction time is 15h.
In sum, utilize a kind of method of preparing flower-shaped nickel hydroxide electrode material from waste battery of the present invention to haveFollowing advantage:
(1) adopting containing nickel-based battery discarded object is that raw material are prepared nickel hydroxide, embody from battery, and in battery,Realize comprehensive utilization of resources.
(2) adopt hydro-thermal reaction to prepare nickel hydroxide, the material of preparation is chrysanthemum shape, particle homogeneous, and purity is high.
Specific embodiments
Embodiment 1
The technical solution adopted for the present invention to solve the technical problems is: one is prepared flower-shaped nickel hydroxide from waste batteryThe method of electrode material, comprises the following steps:
(1) Nickel-bearing Waste rechargeable batteries are shattered to taking 100 grams after 100 orders and be placed in 500ml beaker, measure with graduated cylinder200ml distilled water joins in above-mentioned beaker, and magnetic agitation, puts into water-bath by beaker, heating water bath to 70 DEG C;
(2) measuring concentration with graduated cylinder is that 95% fuming nitric aicd 50ml joins in above-mentioned beaker, is put on magnetic stirring apparatusMagnetic agitation, rotating speed is controlled at 600r/min, continues to stir 60min, and temperature remains on 70 DEG C; Then naturally cooling;
(3) separate above-mentioned solid-liquid mixing system with centrifuge, measure filtered fluid 200ml and proceed to hydrothermal reaction kettle and make componentA；
(4) measure distilled water 25ml in water-bath with pipette and, in small beaker, add surfactant detergent alkylateSodium sulfonate amount 0.2mmol, adds industrial ammonia 60ml, stirs and obtains B component with glass;
(5) B component is slowly joined in component A, magnetic agitation is even;
(6) by hydrothermal reaction kettle, at 200 DEG C, react 15h, be precipitated;
(7) distilled water, the absolute ethanol washing for white precipitate that step (6) are obtained are for several times, super with supersonic wave cleaning machineSound 15min, for several times, the precipitation then suction filtration being obtained is put into drying box to suction filtration, and at 90 DEG C, dry 20h is had after grindingThe nickel hydroxide superfines of chrysanthemum flower-like structure.
The method tool that adopts the present invention to prepare flower-shaped nickel hydroxide electrode material from waste battery has the following advantages:
(1) adopting containing nickel-based battery discarded object is that raw material are prepared nickel hydroxide, embody from battery, and in battery,Realize comprehensive utilization of resources.
(2) adopt hydro-thermal reaction to prepare nickel hydroxide, the material of preparation is chrysanthemum shape, particle homogeneous, and purity is high.
Embodiment 2
The technical solution adopted for the present invention to solve the technical problems is: one is prepared flower-shaped nickel hydroxide from waste batteryThe method of electrode material, comprises the following steps:
(1) Nickel-bearing Waste rechargeable batteries are shattered to taking 100 grams after 100 orders and be placed in 500ml beaker, measure with graduated cylinder200ml distilled water joins in above-mentioned beaker, and magnetic agitation, puts into water-bath by beaker, heating water bath to 60 DEG C;
(2) measuring concentration with graduated cylinder is that 95% fuming nitric aicd 50ml joins in above-mentioned beaker, is put on magnetic stirring apparatusMagnetic agitation, rotating speed is controlled at 550r/min, continues to stir 60min, and temperature remains on 60 DEG C; Then naturally cooling;
(3) separate above-mentioned solid-liquid mixing system with centrifuge, measure filtered fluid 200ml and proceed to hydrothermal reaction kettle and make componentA；
(4) measure distilled water 30ml in water-bath with pipette and, in small beaker, take surfactant detergent alkylateThe each 0.15mmol of sodium sulfonate and polyethylene glycol, measures industrial ammonia 80ml, stirs and obtains B component with glass;
(5) B component is slowly joined in component A, magnetic agitation is even;
(6) by hydrothermal reaction kettle, at 230 DEG C, react 12h, be precipitated;
(7) distilled water, the absolute ethanol washing for white precipitate that step (6) are obtained are for several times, super with supersonic wave cleaning machineSound 20min, for several times, the precipitation then suction filtration being obtained is put into drying box to suction filtration, and at 95 DEG C, dry 18h is had after grindingThe nickel hydroxide superfines of chrysanthemum flower-like structure.
Embodiment 3
The technical solution adopted for the present invention to solve the technical problems is: one is prepared flower-shaped nickel hydroxide from waste batteryThe method of electrode material, comprises the following steps:
(1) Nickel-bearing Waste rechargeable batteries are shattered to taking 100 grams after 100 orders and be placed in 500ml beaker, measure with graduated cylinder200ml distilled water joins in above-mentioned beaker, and magnetic agitation, puts into water-bath by beaker, heating water bath to 80 DEG C;
(2) measuring concentration with graduated cylinder is that 95% fuming nitric aicd 50ml joins in above-mentioned beaker, is put on magnetic stirring apparatusMagnetic agitation, rotating speed is controlled at 750r/min, continues to stir 60min, and temperature remains on 80 DEG C; Then naturally cooling;
(3) separate above-mentioned solid-liquid mixing system with centrifuge, measure filtered fluid 200ml and proceed to hydrothermal reaction kettle and make componentA；
(4) measure distilled water 30ml in water-bath with pipette and, in small beaker, add surfactant dodecyl phosphorusAcid monoester di-potassium 0.4mmol, adds industrial ammonia 75ml, stirs and obtains B component with glass;
(5) B component is slowly joined in component A, magnetic agitation is even;
(6) by hydrothermal reaction kettle, at 250 DEG C, react 12h, be precipitated;
(7) distilled water, the absolute ethanol washing for white precipitate that step (6) are obtained are for several times, super with supersonic wave cleaning machineSound 10min, for several times, the precipitation then suction filtration being obtained is put into drying box to suction filtration, and at 85 DEG C, dry 16h is had after grindingThe nickel hydroxide superfines of chrysanthemum flower-like structure.
Claims (6)
1. a method of preparing flower-shaped nickel hydroxide electrode material from waste battery, comprises the following steps:
(1) Nickel-bearing Waste rechargeable batteries are crushed to and take 100 grams after 100 orders and be placed in 500ml beaker, measure 200ml with graduated cylinder and steamHeat up in a steamer water and join in above-mentioned beaker, magnetic agitation, puts into water-bath by beaker, heating water bath to 60～80 DEG C;
(2) measuring concentration with graduated cylinder is that 95% fuming nitric aicd 50ml joins in above-mentioned beaker, is put into magnetic force on magnetic stirring apparatusStir, rotating speed is controlled at 500～800r/min, continues to stir 60min, and temperature remains on 60～80 DEG C, then naturally cooling;
(3) separate the solid-liquid mixing system in above-mentioned (2) with centrifuge, measure filtered fluid 200ml and proceed to hydrothermal reaction kettle and makeComponent A;
(4) measure in water-bath distilled water 20～30ml in small beaker with pipette, add surfactant 0.1～0.5mmol, adds industrial ammonia 50-80ml, stirs and obtains B component with glass bar;
(5) B component is slowly joined in component A, magnetic agitation is even;
(6) by hydrothermal reaction kettle, at 180～250 DEG C, react 10～20h, be precipitated;
(7) distilled water for white precipitate that step (6) obtained, absolute ethanol washing for several times, with supersonic wave cleaning machine ultrasonic 5～20min, for several times, the precipitation then suction filtration being obtained is put into drying box to suction filtration, after at 80～100 DEG C, dry 16～24h grindsObtain having the nickel hydroxide superfines of chrysanthemum flower-like structure.
2. the method for preparing according to claim 1 flower-shaped nickel hydroxide electrode material from waste battery, is characterized in that, instituteThe water bath heating temperature of stating step (1) is 70 DEG C.
3. the method for preparing according to claim 1 flower-shaped nickel hydroxide electrode material from waste battery, is characterized in that, instituteState in step (2), magnetic agitation rotating speed is 600r/min.
4. the method for preparing according to claim 1 flower-shaped nickel hydroxide electrode material from waste battery, is characterized in that, instituteState in step (4), surfactant used is neopelex, polyethylene glycol, polyvinylpyrrolidone, hexadecaneOne or more in base trimethylammonium bromide, lauryl sodium sulfate, dodecylphosphoric acid monoesters di-potassium.
5. the method for preparing according to claim 1 flower-shaped nickel hydroxide electrode material from waste battery, is characterized in that, instituteState in step (4), industrial ammonia amount is 60ml, and dosage of surfactant is 0.2mmol.
6. the method for preparing according to claim 1 flower-shaped nickel hydroxide electrode material from waste battery, is characterized in that, instituteState in step (6): temperature is controlled at 200 DEG C, the reaction time is 15h.
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| CN104409791B true CN104409791B (en) | 2016-05-18 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994900A (en) * | 2006-12-29 | 2007-07-11 | 北京工业大学 | Process for preparing sub-micrometer flower-shape Ni(OH)2 |
| CN102674483A (en) * | 2012-05-14 | 2012-09-19 | 江门市芳源环境科技开发有限公司 | Method for preparing spherical nickel hydroxide by means of waste battery anode materials |
| CN102674484A (en) * | 2012-05-29 | 2012-09-19 | 南京工业大学 | Preparation method of flower-like alpha-nickel hydroxide |
| JP2012234732A (en) * | 2011-05-02 | 2012-11-29 | Asahi Kasei Corp | Lithium recovery method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994900A (en) * | 2006-12-29 | 2007-07-11 | 北京工业大学 | Process for preparing sub-micrometer flower-shape Ni(OH)2 |
| JP2012234732A (en) * | 2011-05-02 | 2012-11-29 | Asahi Kasei Corp | Lithium recovery method |
| CN102674483A (en) * | 2012-05-14 | 2012-09-19 | 江门市芳源环境科技开发有限公司 | Method for preparing spherical nickel hydroxide by means of waste battery anode materials |
| CN102674484A (en) * | 2012-05-29 | 2012-09-19 | 南京工业大学 | Preparation method of flower-like alpha-nickel hydroxide |
Non-Patent Citations (1)
| Title |
|---|
| Hydrothermal synthesis of α-Ni(OH)2 and its conversion to NiO with electrochemical properties;Yong Cai et al;《Journal of Alloys and Compounds》;20130813;第582卷;第329页左栏第2部分和图1 * |
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