CN104773763A - Method for preparing nanometer crystalline nickel cobalt ferrite by using waste nickel-hydrogen battery - Google Patents
Method for preparing nanometer crystalline nickel cobalt ferrite by using waste nickel-hydrogen battery Download PDFInfo
- Publication number
- CN104773763A CN104773763A CN201510140668.0A CN201510140668A CN104773763A CN 104773763 A CN104773763 A CN 104773763A CN 201510140668 A CN201510140668 A CN 201510140668A CN 104773763 A CN104773763 A CN 104773763A
- Authority
- CN
- China
- Prior art keywords
- solution
- nickel
- hydrogen battery
- waste
- cobalt ferrite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for preparing nanometer crystalline nickel cobalt ferrite by using a waste nickel-hydrogen battery. The method comprises the following steps: 1, cutting the positive electrode material of the waste nickel-hydrogen battery to form blocks with uniform size, and dissolving the blocks in a sulfuric acid solution with the mole concentration of 2-4mol/L to obtain a solution containing Ni<2+>, Co<2+> and Fe<3+>; 2, filtering the solution, adding nickel sulfate, cobalt sulfate and ferrous sulfate into the above obtained filtrate to make a molar ratio of Ni<2+> to Co<2+> to Fe<3+> in the solution reach 1:1:4, adding sodium hydroxide in order to adjust the pH value of the solution to 8-12, and carrying out water bath boiling for 1h; 3, adding the boiled solution into a reaction kettle, putting the reaction kettle provided with the boiled solution in a microwave digestion instrument, and reacting at 100-180DEG C for 0.5-2.5h; and 4, filtering the solution in the reaction kettle, repeatedly washing the filtered product by using deionized water and anhydrous ethanol, and drying at 110DEG C for 1h to obtain powdery nanometer crystalline nickel cobalt ferrite. The method has the advantages of simple process, low cost, environmental protection, and realization of recycling of the waste nickel-hydrogen battery, and the prepared nanometer crystalline nickel cobalt ferrite has wide uses.
Description
Technical field
The invention belongs to waste nickel hydrogen battery reutilization field, be specifically related to a kind of method utilizing waste nickel hydrogen battery to prepare nano-crystal nickel vectolite.
Background technology
Along with socioeconomic development, battery is widely used, and it is that the production of people and life are provided convenience.The kind of current battery has multiple, and wherein nickel metal hydride battery application is comparatively extensive, and nickel metal hydride battery entered the useization stage in 1988, and nineteen ninety starts large-scale production in Japan, and after this output is multiplied.In the new environment of new forms of energy growing tension, be that the new-energy automobile of the main force has become the trend of future development with nickel metal hydride battery.Containing a large amount of metallic substance such as nickel, cobalt, iron in nickel metal hydride battery, if do not reclaimed directly to abandon and can be caused environmental pollution and the wasting of resources, and nickel in nickel metal hydride battery and cobalt are the metals that prices are rather stiff, therefore to the comprehensive utilization of waste nickel hydrogen battery, there is very large economic worth and important environment protection significance.
The main Footwall drift of current recovery waste nickel hydrogen battery, its complex process, separating difficulty is large, added value of product is low, containing the main raw material preparing Ni-Co ferrite in the positive electrode material of waste nickel hydrogen battery, Ni-Co ferrite is a kind of permanent magnet material of excellent property, its chemical stability is good, saturation magnetization is higher, magnetocrystalline anisotropy constant is larger, be widely used in magnetic core with low loss material, perpendicular recording material and magnetic passive wave device etc., and there is not been reported to utilize waste nickel hydrogen battery directly to prepare the method for nano-crystal nickel vectolite at present.
Summary of the invention
The technical problem that the present invention solves there is provided that a kind of technique is simple, less energy intensive, with low cost and added value of product the is high waste nickel hydrogen battery that utilizes prepares the method for nano-crystal nickel vectolite.
The present invention adopts following technical scheme for solving the problems of the technologies described above, utilize waste nickel hydrogen battery to prepare the method for nano-crystal nickel vectolite, it is characterized in that comprising the following steps: it is obtain containing Ni in the sulphuric acid soln of 2-4mol/L that the square that the positive electrode material of waste nickel hydrogen battery is cut into even size by (1) is dissolved in volumetric molar concentration
2+, Co
2+and Fe
3+solution, wherein the mass ratio of positive electrode material and sulphuric acid soln is 7-9:1, and dissolved water bath temperature is 75-95 DEG C; (2) Ni is contained by above-mentioned
2+, Co
2+and Fe
3+solution filter after in filtrate, add single nickel salt, rose vitriol and ferrous sulfate, make Ni in solution
2+, Co
2+and Fe
3+mol ratio be 1:1:4, the pH then adding sodium hydrate regulator solution is 8-12, and water-bath boiling 1h; (3) microwave dissolver is put into after the solution boiled being loaded reactor in 100-180 DEG C of reaction 0.5-2.5h; (4) filtered by the solution in reactor after having reacted, the product with deionized water filtered out and dehydrated alcohol repetitive scrubbing, obtain Powdered nano-crystal nickel vectolite at 110 DEG C of dry 1h.
The present invention compared with prior art technique is simple, with low cost and environmentally friendly, and the renewable resources achieving waste nickel hydrogen battery utilizes, and obtained Ni-Co ferrite tool has been widely used.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the nano-crystal nickel vectolite that the embodiment of the present invention 1 obtains, and Fig. 2 is the SEM collection of illustrative plates of the nano-crystal nickel vectolite that the embodiment of the present invention 1 obtains.
Embodiment
Be described in further details foregoing of the present invention by the following examples, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
(1) it is obtain containing Ni in the sulphuric acid soln of 3mol/L that the square positive electrode material of waste nickel hydrogen battery being cut into even size is dissolved in volumetric molar concentration
2+, Co
2+and Fe
3+solution, wherein the mass ratio of positive electrode material and sulphuric acid soln is 8:1, and dissolved water bath temperature is 85 DEG C; (2) Ni is contained by above-mentioned
2+, Co
2+and Fe
3+solution filter after in filtrate, add single nickel salt, rose vitriol and ferrous sulfate, make Ni in solution
2+, Co
2+and Fe
3+mol ratio be 1:1:4, the pH then adding sodium hydrate regulator solution is 10, and water-bath boiling 1h; (3) microwave dissolver is put into after the solution boiled being loaded reactor in 160 DEG C of reaction 1h; (4) filtered by the solution in reactor after having reacted, the product with deionized water filtered out and dehydrated alcohol repetitive scrubbing, obtain Powdered nano-crystal nickel vectolite at 110 DEG C of dry 1h.Fig. 1 is the XRD figure spectrum of obtained nano-crystal nickel vectolite, as seen from the figure: now the diffraction peak intensities of product is the strongest, illustrate that each ionic reaction is under this condition complete, generate the good Powdered nano-crystal nickel vectolite of performance, Fig. 2 is the SEM collection of illustrative plates of obtained nano-crystal nickel vectolite, the product of gained is little spherical structure as seen from the figure, and be uniformly dispersed good nano crystals.
Embodiment 2
(1) it is obtain containing Ni in the sulphuric acid soln of 2mol/L that the square positive electrode material of waste nickel hydrogen battery being cut into even size is dissolved in volumetric molar concentration
2+, Co
2+and Fe
3+solution, wherein the mass ratio of positive electrode material and sulphuric acid soln is 7:1, and dissolved water bath temperature is 95 DEG C, (2) by above-mentioned containing Ni
2+, Co
2+and Fe
3+solution filter after in filtrate, add single nickel salt, rose vitriol and ferrous sulfate, make Ni in solution
2+, Co
2+and Fe
3+mol ratio be 1:1:4, the pH then adding sodium hydrate regulator solution is 8, and water-bath boiling 1h; (3) microwave dissolver is put into after the solution boiled being loaded reactor in 180 DEG C of reaction 0.5h; (4) filtered by the solution in reactor after having reacted, the product with deionized water filtered out and dehydrated alcohol repetitive scrubbing, obtain Powdered nano-crystal nickel vectolite at 110 DEG C of dry 1h.
Embodiment 3
(1) it is obtain containing Ni in the sulphuric acid soln of 4mol/L that the square positive electrode material of waste nickel hydrogen battery being cut into even size is dissolved in volumetric molar concentration
2+, Co
2+and Fe
3+solution, wherein the mass ratio of positive electrode material and sulphuric acid soln is 9:1, and dissolved water bath temperature is 75 DEG C, (2) by above-mentioned containing Ni
2+, Co
2+and Fe
3+solution filter after in filtrate, add single nickel salt, rose vitriol and ferrous sulfate, make Ni in solution
2+, Co
2+and Fe
3+mol ratio be 1:1:4, the pH then adding sodium hydrate regulator solution is 12, and water-bath boiling 1h; (3) microwave dissolver is put into after the solution boiled being loaded reactor in 100 DEG C of reaction 2.5h; (4) filtered by the solution in reactor after having reacted, the product with deionized water filtered out and dehydrated alcohol repetitive scrubbing, obtain Powdered nano-crystal nickel vectolite at 110 DEG C of dry 1h.
Embodiment above describes ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; under the scope not departing from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.
Claims (1)
1. utilize waste nickel hydrogen battery to prepare the method for nano-crystal nickel vectolite, it is characterized in that comprising the following steps: it is obtain containing Ni in the sulphuric acid soln of 2-4mol/L that the square that the positive electrode material of waste nickel hydrogen battery is cut into even size by (1) is dissolved in volumetric molar concentration
2+, Co
2+and Fe
3+solution, wherein the mass ratio of positive electrode material and sulphuric acid soln is 7-9:1, and dissolved water bath temperature is 75-95 DEG C; (2) Ni is contained by above-mentioned
2+, Co
2+and Fe
3+solution filter after in filtrate, add single nickel salt, rose vitriol and ferrous sulfate, make Ni in solution
2+, Co
2+and Fe
3+mol ratio be 1:1:4, the pH then adding sodium hydrate regulator solution is 8-12, and water-bath boiling 1h; (3) microwave dissolver is put into after the solution boiled being loaded reactor in 100-180 DEG C of reaction 0.5-2.5h; (4) filtered by the solution in reactor after having reacted, the product with deionized water filtered out and dehydrated alcohol repetitive scrubbing, obtain Powdered nano-crystal nickel vectolite at 110 DEG C of dry 1h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510140668.0A CN104773763A (en) | 2015-03-30 | 2015-03-30 | Method for preparing nanometer crystalline nickel cobalt ferrite by using waste nickel-hydrogen battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510140668.0A CN104773763A (en) | 2015-03-30 | 2015-03-30 | Method for preparing nanometer crystalline nickel cobalt ferrite by using waste nickel-hydrogen battery |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104773763A true CN104773763A (en) | 2015-07-15 |
Family
ID=53615581
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510140668.0A Pending CN104773763A (en) | 2015-03-30 | 2015-03-30 | Method for preparing nanometer crystalline nickel cobalt ferrite by using waste nickel-hydrogen battery |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104773763A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109231979A (en) * | 2018-11-09 | 2019-01-18 | 河南师范大学 | A method of Conjugate ferrite magnetostriction materials are prepared by raw material of waste and old lithium ion battery |
| CN113461071A (en) * | 2021-06-10 | 2021-10-01 | 贵州理工学院 | Method for preparing nickel-zinc ferrite from waste nickel-hydrogen waste battery |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1357938A (en) * | 2000-12-08 | 2002-07-10 | 同济大学 | Comprehensive recovery and utilization method of waste NiCd battery |
| JP2003045506A (en) * | 2001-07-31 | 2003-02-14 | Toyota Motor Corp | Method of separating and recovering alkaline secondary battery positive electrode material, method of analyzing characteristics of alkaline secondary battery positive electrode material, and the alkaline secondary battery |
| CN101219812A (en) * | 2008-01-24 | 2008-07-16 | 河南师范大学 | Method for producing vectolite with waste and old lithium ion battery |
| CN101237075A (en) * | 2008-01-24 | 2008-08-06 | 河南师范大学 | Method for making lithium with the abandoned lithium ion battery and replacing cobalt ferrite |
| CN101891483A (en) * | 2010-07-09 | 2010-11-24 | 东华大学 | Method for preparing Co1-xNixFe2O4 magnetic nano-powder by solvothermal method |
| CN102649639A (en) * | 2012-05-09 | 2012-08-29 | 上海颜钛实业有限公司 | Hydrothermal preparation method for spinel type ferrite nanopowder |
| CN103757317A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for leaching positive pole material of waste nickel-metal hydride battery |
| CN104617349A (en) * | 2014-12-09 | 2015-05-13 | 张国英 | Method for preparing nickel sulfate by utilizing waste Ni-NH battery cathode material |
-
2015
- 2015-03-30 CN CN201510140668.0A patent/CN104773763A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1357938A (en) * | 2000-12-08 | 2002-07-10 | 同济大学 | Comprehensive recovery and utilization method of waste NiCd battery |
| JP2003045506A (en) * | 2001-07-31 | 2003-02-14 | Toyota Motor Corp | Method of separating and recovering alkaline secondary battery positive electrode material, method of analyzing characteristics of alkaline secondary battery positive electrode material, and the alkaline secondary battery |
| CN101219812A (en) * | 2008-01-24 | 2008-07-16 | 河南师范大学 | Method for producing vectolite with waste and old lithium ion battery |
| CN101237075A (en) * | 2008-01-24 | 2008-08-06 | 河南师范大学 | Method for making lithium with the abandoned lithium ion battery and replacing cobalt ferrite |
| CN101891483A (en) * | 2010-07-09 | 2010-11-24 | 东华大学 | Method for preparing Co1-xNixFe2O4 magnetic nano-powder by solvothermal method |
| CN102649639A (en) * | 2012-05-09 | 2012-08-29 | 上海颜钛实业有限公司 | Hydrothermal preparation method for spinel type ferrite nanopowder |
| CN103757317A (en) * | 2013-12-29 | 2014-04-30 | 四川师范大学 | Method for leaching positive pole material of waste nickel-metal hydride battery |
| CN104617349A (en) * | 2014-12-09 | 2015-05-13 | 张国英 | Method for preparing nickel sulfate by utilizing waste Ni-NH battery cathode material |
Non-Patent Citations (3)
| Title |
|---|
| GUOXI XI ET AL.: ""Study on preparation of NiCo ferrite using spent lithium-ion and nickel-metal hydride batteries"", 《SEPARATION AND PURIFICATION TECHNOLGY》 * |
| NERMIN KASAPOGLU ET AL.: ""Synthesis and magnetic properties of octahedral ferrite NixCo1-xFe2O4 nanocrystals"", 《CENTRAL EUROPEAN JOURNAL OF CHEMISTRY》 * |
| 席国喜等: ""废旧镍氢电池溶胶-凝胶法制备Ni0.5Co0.5Fe2O4的研究"", 《电子元件与材料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109231979A (en) * | 2018-11-09 | 2019-01-18 | 河南师范大学 | A method of Conjugate ferrite magnetostriction materials are prepared by raw material of waste and old lithium ion battery |
| CN113461071A (en) * | 2021-06-10 | 2021-10-01 | 贵州理工学院 | Method for preparing nickel-zinc ferrite from waste nickel-hydrogen waste battery |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106745331B (en) | A kind of preparation method of low-sulfur small particle nickel cobalt manganese hydroxide | |
| CN103606651A (en) | Method for preparing lithium nickelate cobaltate manganate cathode material by taking waste lithium ion batteries as raw material | |
| CN102517448B (en) | Method for recycling metal ion from waste lithium-ion battery | |
| CN103435104B (en) | A kind of preparation method of lithium ion battery negative electrode material-nano zinc ferrite | |
| CN111916687A (en) | Cathode material, preparation method thereof and lithium ion battery | |
| CN104692465B (en) | The preparation method of anode material for lithium-ion batteries α-LiFeO2 nano-powder | |
| CN107342418B (en) | A kind of ferrocyanogen positive electrode and its preparation method and application | |
| CN101264875A (en) | Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite | |
| CN107623124B (en) | Preparation method of spherical nickel-cobalt-manganese precursor material | |
| CN111082003A (en) | Vanadate hydrate electrode material and preparation method and application thereof | |
| CN106654205A (en) | Method for preparing ternary cathode material precursor by using waste lithium battery material | |
| CN106571465A (en) | Hydrotalcite precursor technique nitrogen-sulfur co-doped carbon loaded transition metal sulfide solid solution, preparation method and application thereof | |
| CN104600390A (en) | Method for preparing magnetostriction material by utilizing spent lithium ion batteries | |
| CN101875488A (en) | Method for preparing lithium titanate precursor and lithium iron phosphate precursor by comprehensively utilizing ilmenite | |
| CN103022491A (en) | Method for preparing lithium iron phosphate precursor for positive pole material of lithium-ion battery | |
| CN104701527A (en) | Preparation method for lithium ion battery anode material Li(Ni1-x-yCoxAly)O2 | |
| CN102897739A (en) | Novel process for preparing battery-grade iron phosphate material by using iron hydroxide | |
| CN107026256A (en) | A kind of thermal cell positive electrode FexCo1‑xS2Powder and preparation method thereof | |
| CN103011117B (en) | Production method of iron phosphate nano powder body with controllable size and granularity | |
| CN104760999A (en) | Porous nano manganese sulfide and preparation method thereof | |
| CN108862406A (en) | A kind of carbonate precursor and its preparation method and application | |
| CN109244459A (en) | A kind of codope flexibility sodium-ion battery positive material and preparation method thereof | |
| CN104183827B (en) | A kind of lithium iron phosphate nano rod and preparation method thereof | |
| CN103066249B (en) | Cobalt-based complex oxide/graphene composite material as well as preparation method and application thereof | |
| CN109671937B (en) | In-situ synthesis method of transition metal oxide/graphene composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150715 |