CN106379948A - Method for preparing nano hydroxyl manganese cobalt oxide - Google Patents
Method for preparing nano hydroxyl manganese cobalt oxide Download PDFInfo
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- CN106379948A CN106379948A CN201610883535.7A CN201610883535A CN106379948A CN 106379948 A CN106379948 A CN 106379948A CN 201610883535 A CN201610883535 A CN 201610883535A CN 106379948 A CN106379948 A CN 106379948A
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- manganese
- cobalt
- cobalt oxide
- mixed solution
- acetate
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- 238000000034 method Methods 0.000 title claims abstract description 34
- RHBREZMHGBURNU-UHFFFAOYSA-M O[Mn]O[Co] Chemical compound O[Mn]O[Co] RHBREZMHGBURNU-UHFFFAOYSA-M 0.000 title abstract 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 13
- 230000001590 oxidative effect Effects 0.000 claims abstract description 13
- 229940071125 manganese acetate Drugs 0.000 claims abstract description 11
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229940011182 cobalt acetate Drugs 0.000 claims abstract description 8
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims description 6
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 5
- 238000005273 aeration Methods 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 239000003990 capacitor Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 239000000047 product Substances 0.000 description 13
- 235000013495 cobalt Nutrition 0.000 description 10
- 239000010941 cobalt Substances 0.000 description 7
- 229910017052 cobalt Inorganic materials 0.000 description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000011572 manganese Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 description 3
- MZZUATUOLXMCEY-UHFFFAOYSA-N cobalt manganese Chemical compound [Mn].[Co] MZZUATUOLXMCEY-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- MSBWDNNCBOLXGS-UHFFFAOYSA-L manganese(2+);diacetate;hydrate Chemical compound O.[Mn+2].CC([O-])=O.CC([O-])=O MSBWDNNCBOLXGS-UHFFFAOYSA-L 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 229910001429 cobalt ion Inorganic materials 0.000 description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 2
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229910008090 Li-Mn-O Inorganic materials 0.000 description 1
- 229910006369 Li—Mn—O Inorganic materials 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- SVMCDCBHSKARBQ-UHFFFAOYSA-N acetic acid;cobalt Chemical compound [Co].CC(O)=O SVMCDCBHSKARBQ-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- 150000001869 cobalt compounds Chemical class 0.000 description 1
- XEUFSQHGFWJHAP-UHFFFAOYSA-N cobalt(2+) manganese(2+) oxygen(2-) Chemical compound [O--].[O--].[Mn++].[Co++] XEUFSQHGFWJHAP-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- DLHSXQSAISCVNN-UHFFFAOYSA-M hydroxy(oxo)cobalt Chemical compound O[Co]=O DLHSXQSAISCVNN-UHFFFAOYSA-M 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- -1 manganese Hydroxy cobalt oxide Chemical compound 0.000 description 1
- WSHADMOVDWUXEY-UHFFFAOYSA-N manganese oxocobalt Chemical compound [Co]=O.[Mn] WSHADMOVDWUXEY-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
-
- 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
- Y02E60/13—Energy storage using capacitors
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method for preparing nano hydroxyl manganese cobalt oxide. The method comprises the following steps: (1) adjusting the pH (Potential of Hydrogen) value of a mixed solution of manganese acetate and cobalt acetate to 2.5 to 6; (2) introducing oxidizing gas into the mixed solution of the step (1) and carrying out an oxidization reaction; after the reaction, centrifuging, washing and drying to obtain the nano hydroxyl manganese cobalt oxide. By adopting the preparation method provided by the invention, the nano hydroxyl manganese cobalt oxide can be processed through one step; the nano hydroxyl manganese cobalt oxide can be applied to related fields of super-capacitors, lithium-ion batteries and the like. The preparation method provided by the invention has the advantages that raw materials are cheap and easy to obtain, the cost is low and a synthesis process is simple and easy to realize; the quality of a product is stable and the process repeatability is good; the reaction can be finished within relatively short time and the efficiency is high.
Description
Technical field
The invention belongs to field of nanometer material technology, more particularly, to a kind of method preparing nano-hydroxy cobalt oxide manganese.
Background technology
Manganese, the oxyhydroxide of cobalt suffer from highly important purposes in fields such as electrochemistry, battery, electrochromism.Hydroxyl
Base manganese oxide cobalt can act also as the presoma of the manganese and oxygen compound of Li-Mn-O spinel structure and ginseng cobalt, and joins the manganese oxidation of cobalt
Compound has very superior performance at secondary cell, ultracapacitor aspect, is constantly subjected to the extensive of scientific circles and industrial quarters
Concern.Chinese patent application 201210578760.1, discloses a kind of preparation method of the hydroxy cobalt oxide of doping trace manganese, this
Method is to add precipitant (KOH, NaOH etc.) and oxidant (compressed air) in cobalt salt and M salt, and synthesis is containing trace manganese
Hydroxy cobalt oxide, because the method adds precipitant and oxidant can cause the uneven of reaction in building-up process, product is steady
Qualitative poor, reaction needs just can complete in longer period of time, inefficient, is unfavorable for being produced in enormous quantities.Therefore,
Study a kind of synthesis technique simply easily to realize, the preparation side of the hydroxyl oxidize manganese cobalt that product quality is stable and process repeatability energy is good
Method, is necessary.
Content of the invention
The technical problem to be solved is to overcome the shortcomings of to mention and defect in background above technology, provide one
Plant the method preparing nano-hydroxy cobalt oxide manganese.
For solving above-mentioned technical problem, technical scheme proposed by the present invention is：
A kind of method preparing nano-hydroxy cobalt oxide manganese, comprises the following steps：
(1) pH value of mixed solution adjusting manganese acetate and cobalt acetate is to 2.5～6；
(2) it is passed through oxidizing gas in the mixed solution after step (1) and carry out oxidation reaction, be centrifuged after reaction, wash,
Dry, obtain described nano-hydroxy manganese oxide cobalt.
Applicant passes through research repeatedly and experimental verification finds, when the pH value of mixed solution is less than 2.5, cobalt ion is difficult to
Oxidized precipitation, at short notice only a small amount of cobalt precipitate, reaction efficiency is too low；When pH value is higher than 6, reaction rate mistake
Hurry up, particle size is difficult to control to；Also find, Co under identical pH simultaneously2+Oxidizing potential is higher, and precipitation is compared with Mn2+Slowly, identical
In time, both precipitation capacities are different, thus can adjust the atomic ratio of cobalt manganese in product by adjusting pH, change and mix cobalt
Content.
Above-mentioned method is it is preferred that the chemical formula of described nano-hydroxy manganese oxide cobalt is (CoxMn1-x) OOH, wherein 0 ＜ x
＜ 1；Described nano-hydroxy manganese oxide cobalt is spherical in shape, and mean diameter is 180nm～200nm.
Above-mentioned method it is preferred that in the mixed solution of described manganese acetate and cobalt acetate, the concentration of manganese acetate and cobalt acetate
For 0.01mol/L～0.02mol/L.
Above-mentioned method is it is preferred that described oxidizing gas are chlorine or the mixed gas for ozone and oxygen.
Above-mentioned method it is preferred that in described step (2) oxidation reaction time be 45min～75min.
Above-mentioned method it is preferred that in described step (2), at 25 DEG C～70 DEG C to mixed solution in be passed through oxidisability
Gas, controlling reaction temperature is 25 DEG C～70 DEG C, can change the nucleation and growth speed of manganese, cobalt, adjusts particle size size,
Adjust settling rate, make product be nano-particle；The temperature of course of reaction is less than 25 DEG C, and reaction becomes relatively slow, production efficiency
Low；Reaction temperature is higher than 70 DEG C, is swift in response, and solution moisture content testing volatilization is serious, is unfavorable for crystallite dimension control and stable system.
Above-mentioned method is it is preferred that in described step (2), oxidizing gas are to be passed through in mixed solution through aeration head
's.Oxidizing gas can form the minute bubbles of disperse in the solution through aeration head, and oxidizing gas even dispersion is in liquid
In, then with solution in manganese, cobalt ion reaction generate precipitation, make reaction more abundant.
Compared with prior art, it is an advantage of the current invention that：
(1) preparation method of the present invention step processing can obtain nano-hydroxy cobalt oxide manganese, this nano-hydroxy cobalt oxide manganese
Can be applicable to the association areas such as ultracapacitor and lithium ion battery.
(2) raw material involved by the preparation method of the present invention is cheap and easy to get, low cost, and synthesis technique is simply easily realized, product
Steady quality and process repeatability can be good, and reaction can complete within a short period of time, efficiency high.
Brief description
Fig. 1 is the XRD figure of the nano-hydroxy cobalt oxide manganese of the embodiment of the present invention 1 preparation.
Fig. 2 is the FESEM figure of the nano-hydroxy cobalt oxide manganese of the embodiment of the present invention 2 preparation.
Specific embodiment
For the ease of understanding the present invention, below in conjunction with Figure of description and preferred embodiment, invention herein is done more complete
Face, meticulously describe, but protection scope of the present invention is not limited to specific examples below.
Unless otherwise defined, all technical term used hereinafter and those skilled in the art are generally understood that implication phase
With.Technical term used herein is intended merely to describe the purpose of specific embodiment, is not intended to limit the present invention's
Protection domain.
Unless otherwise specified, the various raw materials used in the present invention, reagent, instrument and equipment etc. all can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
A kind of method preparing nano-hydroxy cobalt oxide manganese of present invention, comprises the following steps：
(1) four acetate hydrate manganese and four acetate hydrate cobalts are dissolved in 200mL deionized water, prepared manganese acetate and acetic acid
The concentration of cobalt is in the mixed solution of 0.0125mol/L；
(2) dilute sulfuric acid is utilized to adjust the pH value of mixed solution to 2.5；
(3) at 35 DEG C, in the mixed solution after processing to step (2), it is passed through ozone, react 1h, be then centrifuged for, washing,
Finally dry at 80 DEG C, obtain nano-hydroxy cobalt oxide manganese product.
The XRD figure of nano-hydroxy cobalt oxide manganese product manufactured in the present embodiment is as shown in figure 1, show that product is hydroxyl oxidize
Cobalt manganese, chemical formula is (Coa,Mn1-a) OOH, standard card number is JCPDS 42-1316；Nano-hydroxy prepared by the present embodiment
Cobalt oxide manganese is spherical in shape, and particle diameter is 181nm；Further demonstrate that its chemical formula is (Co through XPS detection0.15Mn0.85)OOH.
The nano-hydroxy cobalt oxide manganese that the present embodiment is prepared is prepared into electrode slice, and in 6mol/L KOH solution
Carry out constant current charge-discharge detection, recording specific capacity is 707F/g.
Embodiment 2：
A kind of method preparing nano-hydroxy cobalt oxide manganese of present invention, comprises the following steps：
(1) four acetate hydrate manganese and four acetate hydrate cobalts are dissolved in 200mL deionized water, prepared manganese acetate and acetic acid
The concentration of cobalt is in the mixed solution of 0.0125mol/L；
(2) dilute sulfuric acid is utilized to adjust the pH value of mixed solution to 3.5；
(3) at 35 DEG C, in the mixed solution after processing to step (2), it is passed through ozone, react 45min, be then centrifuged for, wash
Wash, finally dry at 80 DEG C, obtain nano-hydroxy cobalt oxide manganese product.
The FESEM of nano-hydroxy cobalt oxide manganese product manufactured in the present embodiment schemes as shown in Fig. 2 as seen from the figure, this enforcement
Nano-hydroxy cobalt oxide manganese prepared by example is spherical in shape, and particle diameter is in 200nm；Through XRD and XPS detection, show the present embodiment
Nano-hydroxy cobalt oxide manganese product chemical formula be (Co0.27Mn0.73)OOH.
Embodiment 3：
A kind of method preparing nano-hydroxy cobalt oxide manganese of present invention, comprises the following steps：
(1) four acetate hydrate manganese and four acetate hydrate cobalts are dissolved in 200mL deionized water, prepared manganese acetate and acetic acid
Cobalt mixed solution (in mixed solution, manganese acetate concentration is 0.0125mol/L, and the concentration of cobalt acetate is 0.025mol/L)；
(2) dilute sulfuric acid is utilized to adjust the pH value of mixed solution to 2.5；
(3) at 70 DEG C, in the mixed solution after processing to step (2), it is passed through ozone, react 1h, be then centrifuged for, washing,
Finally dry at 80 DEG C, obtain nano-hydroxy cobalt oxide manganese product.Nano-hydroxy cobalt oxide manganese prepared by the present embodiment is in ball
Shape, particle diameter is 123nm；Through XRD and XPS detection, show the chemical formula of the nano-hydroxy cobalt oxide manganese product of the present embodiment
For (Co0.48Mn0.52)OOH.
Claims (7)
1. a kind of method preparing nano-hydroxy cobalt oxide manganese is it is characterised in that comprise the following steps：
(1) pH value of mixed solution adjusting manganese acetate and cobalt acetate is to 2.5～6；
(2) it is passed through oxidizing gas in the mixed solution after step (1) and carry out oxidation reaction, centrifugation, washing, baking after reaction
Dry, obtain described nano-hydroxy manganese oxide cobalt.
2. the method for claim 1 is it is characterised in that the chemical formula of described nano-hydroxy manganese oxide cobalt is (CoxMn1-x)
OOH, wherein 0 ＜ x ＜ 1；Described nano-hydroxy manganese oxide cobalt is spherical in shape, and mean diameter is 180nm～200nm.
3. the method for claim 1 is it is characterised in that in the mixed solution of described manganese acetate and cobalt acetate, manganese acetate
It is 0.01mol/L～0.02mol/L with the concentration of cobalt acetate.
4. the method for claim 1 is it is characterised in that described oxidizing gas are chlorine or are ozone and oxygen
Mixed gas.
5. the method as described in any one of Claims 1 to 4 it is characterised in that in described step (2) time of oxidation reaction be
45min～75min.
6. the method as described in any one of Claims 1 to 4 is it is characterised in that in described step (2), at 25 DEG C～20 DEG C
It is passed through oxidizing gas in mixed solution.
7. the method as described in any one of Claims 1 to 4 is it is characterised in that in described step (2), oxidizing gas be through
Cross aeration head to be passed through in mixed solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109256532A (en) * | 2018-03-27 | 2019-01-22 | 清远佳致新材料研究院有限公司 | A kind of method of ternary cathode material of lithium ion battery precursor synthesis process mother liquor comprehensive utilization |
| CN112071659A (en) * | 2020-08-05 | 2020-12-11 | 新昌县华发机械股份有限公司 | Polyaniline hydrogel-coated Co3O4Super capacitor electrode material and preparation method thereof |
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|---|---|---|---|---|
| CN101127398A (en) * | 2007-06-28 | 2008-02-20 | 河南师范大学 | A ball hydroxide oxidated Ni-Co-Mn and its making method |
| CN100577576C (en) * | 2007-04-20 | 2010-01-06 | 南京大学 | Simple method for ozone oxidation preparation of alpha-FeOOH, beta-MnO2 and Co3O4 nano material |
| CN103904323A (en) * | 2012-12-28 | 2014-07-02 | 北京当升材料科技股份有限公司 | Preparation method for spherical cobalt oxyhydroxide |
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| CN109256532B (en) * | 2018-03-27 | 2021-04-02 | 清远佳致新材料研究院有限公司 | Method for comprehensively utilizing mother liquor in synthesis process of ternary cathode material precursor of lithium ion battery |
| CN112071659A (en) * | 2020-08-05 | 2020-12-11 | 新昌县华发机械股份有限公司 | Polyaniline hydrogel-coated Co3O4Super capacitor electrode material and preparation method thereof |
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