CN103274469B - Trimanganese tetroxide nanocrystal and preparation method thereof - Google Patents
Trimanganese tetroxide nanocrystal and preparation method thereof Download PDFInfo
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- CN103274469B CN103274469B CN201310220143.9A CN201310220143A CN103274469B CN 103274469 B CN103274469 B CN 103274469B CN 201310220143 A CN201310220143 A CN 201310220143A CN 103274469 B CN103274469 B CN 103274469B
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 title claims abstract description 70
- 239000002159 nanocrystal Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 26
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 26
- 239000011572 manganese Substances 0.000 claims abstract description 26
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 17
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 150000002696 manganese Chemical class 0.000 claims abstract description 6
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 6
- 239000012266 salt solution Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 4
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims abstract description 4
- 239000012456 homogeneous solution Substances 0.000 claims description 18
- 238000011026 diafiltration Methods 0.000 claims description 16
- BZDIAFGKSAYYFC-UHFFFAOYSA-N manganese;hydrate Chemical compound O.[Mn] BZDIAFGKSAYYFC-UHFFFAOYSA-N 0.000 claims description 14
- MJOQJPYNENPSSS-XQHKEYJVSA-N [(3r,4s,5r,6s)-4,5,6-triacetyloxyoxan-3-yl] acetate Chemical compound CC(=O)O[C@@H]1CO[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O MJOQJPYNENPSSS-XQHKEYJVSA-N 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 claims description 3
- CNFDGXZLMLFIJV-UHFFFAOYSA-L manganese(II) chloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Mn+2] CNFDGXZLMLFIJV-UHFFFAOYSA-L 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 23
- 239000000047 product Substances 0.000 abstract description 21
- 239000012467 final product Substances 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 3
- 238000005406 washing Methods 0.000 abstract 3
- 229910021380 Manganese Chloride Inorganic materials 0.000 abstract 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 abstract 2
- 229940071125 manganese acetate Drugs 0.000 abstract 2
- 235000002867 manganese chloride Nutrition 0.000 abstract 2
- 239000011565 manganese chloride Substances 0.000 abstract 2
- 229940099607 manganese chloride Drugs 0.000 abstract 2
- 229940099596 manganese sulfate Drugs 0.000 abstract 2
- 235000007079 manganese sulphate Nutrition 0.000 abstract 2
- 239000011702 manganese sulphate Substances 0.000 abstract 2
- 239000002243 precursor Substances 0.000 abstract 2
- 239000006185 dispersion Substances 0.000 abstract 1
- 150000004677 hydrates Chemical class 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 230000015572 biosynthetic process Effects 0.000 description 9
- 238000003786 synthesis reaction Methods 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 8
- 238000000576 coating method Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910015645 LiMn Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- -1 and can find out Substances 0.000 description 1
- 239000006183 anode active material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- IPJKJLXEVHOKSE-UHFFFAOYSA-L manganese dihydroxide Chemical compound [OH-].[OH-].[Mn+2] IPJKJLXEVHOKSE-UHFFFAOYSA-L 0.000 description 1
- ZWXOQTHCXRZUJP-UHFFFAOYSA-N manganese(2+);manganese(3+);oxygen(2-) Chemical group [O-2].[O-2].[O-2].[O-2].[Mn+2].[Mn+3].[Mn+3] ZWXOQTHCXRZUJP-UHFFFAOYSA-N 0.000 description 1
- 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 1
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical compound [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of a trimanganese tetroxide nanocrystal. The method comprises the following steps: adding 10-1000mg of a manganese source precursor into 30-300ml of deionized water, stirring and then obtaining a manganese salt solution; and adding 0.1-30ml of hydrazine hydrate to the manganese salt solution, continuing to stir for 6-24 hours, filtering and washing, drying, then grinding to obtain the trimanganese tetroxide nanocrystal. The whole reaction process can be performed at a room temperature. The manganese source precursor is one or a plurality of substances from the following substances: manganese acetate, manganese chloride, manganese sulfate and crystalline hydrates of the manganese acetate, the manganese chloride, and the manganese sulfate. The step of filtering and washing is carried out for 2-4 times by use of the deionized water, and a product after the step of filtering and washing is dried for 3-5 hours under an air-blast condition at the temperature of 80-150DEG C. The reaction process is performed at the room temperature, and the preparation process is simple, the material selection range is wide, and the cost is low. The trimanganese tetroxide nanocrystals prepared by use of the method have high crystallinity, high homogeneity of morphology and size, high dispersion and high water solubility, and condition control of the morphology and size of the final product can be realized through adjusting.
Description
Technical field
The present invention relates to a kind of Trimanganese tetroxide nanocrystal and preparation method thereof, belong to chemical production technical field.
Background technology
Mn
3o
4be a kind of important inorganic materials, be widely used in the fields such as magneticsubstance, electrochemical field and catalysis.In electronic industry, Mn
3o
4it is the important source material making soft magnetic ferrite; In chemical industry, Mn
3o
4it is the catalyzer of multiple reaction; In coatings industry, containing Mn
3o
4coating, have, than the coating containing titanium dioxide or ferric oxide, there is better resistance to corrosion; In electrochemistry, Mn
3o
4prepare battery anode active material LiMn
2o
4presoma.
Current industrial main employing metal magnesium powder catalytic oxidation produces trimanganese tetroxide, and the method technical maturity is simple, but product foreign matter content is general higher.In order to produce high-quality Trimanganese tetroxide nanocrystal, the more method of research comprises at present: sol-gel method, hydrothermal method or solvent-thermal method etc.As in publication number CN101219809A, CN 101565208A the method utilizing solvent structure Trimanganese tetroxide nanocrystal reported, aforesaid method often requires higher to synthesis condition, and needs additive or organic solvent as auxiliary.
Utilize alkaline matter divalent manganesetion precipitation to be obtained to recycle after manganous hydroxide air or oxygen to be oxidized the method preparing trimanganese tetroxide and simplify preparation process, oxidising process can be carried out again under the room temperature condition of gentleness, prepares a large amount of Mn to cheapness
3o
4product is significant.But based on patent and the paper of the method, as the method reported in publication number CN1935673A, CN102627330A, CN102040246A, be not difficult the Mn finding to be produced by this process
3o
4nanocrystal is often not satisfactory in the homogeneity of pattern or size.
Summary of the invention
Nano manganic manganous oxide of the present invention prepares scheme, and key is: use hydrazine hydrate as alkaline matter and oxidising process control agent.
In order to solve Mn (OH)
2the problem of the oxidized excessive velocities of middle bivalent manganese, prepares the Mn of pattern and size uniformity simultaneously
3o
4nanocrystal, the present invention is to provide a kind of control Mn (OH)
2the method of oxidation rate, namely by introducing hydrazine hydrate in the reaction, not only create the environment of alkalescence, also effectively control the carrying out of oxidizing reaction, meanwhile, production process can be carried out under the room temperature of gentleness, the Mn produced
3o
4nanocrystal pattern and size have homogeneous feature.Nanocrystalline size and pattern can be effectively controlled by regulating experiment parameter.
A preparation method for Trimanganese tetroxide nanocrystal, comprises the steps: 10 ~ 1000mg manganese source presoma to add in 30 ~ 300ml deionized water, obtains manganese salt solution after stirring; Then in manganese salt solution, add 0.1 ~ 30ml hydrazine hydrate, continue stirring 6 ~ 24 hours, diafiltration, dry, after grinding, obtain described Trimanganese tetroxide nanocrystal.
Whole reaction process all can at room temperature be carried out.
Described manganese source presoma is one or more in following substances: the crystalline hydrate of manganous acetate, Manganous chloride tetrahydrate, manganous sulfate and above material.
Described diafiltration deionized water diafiltration 2 ~ 4 times, subsequently the product after diafiltration is carried out drying in 80 ~ 150 DEG C under air blast condition, time of drying is 3 ~ 5 hours.
Under room temperature, 0.25-1.0g tetra-acetate hydrate manganese is dissolved in 60ml deionized water, stirs 2 hours, obtain homogeneous solution, in homogeneous solution, inject 1 ml hydrazine hydrate fast, continue stirring 24 hours; Diafiltration, dry, obtaining Trimanganese tetroxide nanocrystal after grinding is homogeneous square mesa-shaped pattern.
Be dissolved in 60ml deionized water by 0.5g tetra-acetate hydrate manganese under room temperature, 60 DEG C are stirred 2 hours, obtain homogeneous solution, in homogeneous solution, inject 1 ml hydrazine hydrate fast, continue stirring 24 hours.Diafiltration, dry, obtaining Trimanganese tetroxide nanocrystal after grinding is homogeneous ellipse spherical morphology.
Under room temperature, 0.125g tetra-acetate hydrate manganese is dissolved in 60ml deionized water, stirs 2 hours, obtain homogeneous solution.In solution, inject 5 ml hydrazine hydrates fast, continue stirring 24 hours.Take out product, diafiltration, dry, obtaining Trimanganese tetroxide nanocrystal after grinding is homogeneous disc-shaped pattern.
Under room temperature, 0.01g tetra-chloride hydrate manganese is dissolved in 60ml deionized water, stirs 2 hours, obtain homogeneous solution.In solution, inject 5 ml hydrazine hydrates fast, continue stirring 24 hours.Take out product, diafiltration, dry, obtaining Trimanganese tetroxide nanocrystal after grinding is homogeneous square sheet-like morphology.
The Trimanganese tetroxide nanocrystal that a kind of described preparation method obtains.
Compared with existing Trimanganese tetroxide nanocrystal preparation method, the present invention has the following advantages:
1, reaction is at room temperature carried out, and preparation process is simple, and Material selec-tion is extensive, with low cost.
2, synthesized trimanganese tetroxide has higher dispersiveness and water-soluble preferably.
3, the trimanganese tetroxide of synthesis has high crystalline, and pattern and dimensional homogeneity by force, and can control pattern and the size of final product by regulation experiment condition.
Accompanying drawing explanation
Fig. 1 the inventive method prepares the process flow sheet of Trimanganese tetroxide nanocrystal.
The XRD spectra of the Trimanganese tetroxide nanocrystal of Fig. 2 the inventive method example 1 preparation.
The stereoscan photograph of the Trimanganese tetroxide nanocrystal of Fig. 3 the inventive method example 1 preparation.
The transmission electron microscope photo of the Trimanganese tetroxide nanocrystal of Fig. 4 the inventive method example 1 preparation.
The transmission electron microscope photo of the Trimanganese tetroxide nanocrystal of Fig. 5 the inventive method example 2 preparation.
The transmission electron microscope photo of the Trimanganese tetroxide nanocrystal of Fig. 6 the inventive method example 3 preparation.
The transmission electron microscope photo of the Trimanganese tetroxide nanocrystal of Fig. 7 the inventive method example 4 preparation.
The stereoscan photograph of the Trimanganese tetroxide nanocrystal of Fig. 8 the inventive method example 5 preparation.
The stereoscan photograph of the Trimanganese tetroxide nanocrystal of Fig. 9 the inventive method example 6 preparation.
Embodiment
Below in conjunction with the drawings and specific embodiments, set forth the present invention further.These embodiments are interpreted as only being not used in for illustration of the present invention limiting the scope of the invention.After the content of having read the present invention's record, those skilled in the art can make various changes or modifications the present invention, and these equivalence changes and modification fall into the scope of the claims in the present invention equally.
embodiment 1
Under room temperature, 0.5g tetra-acetate hydrate manganese is dissolved in 60ml deionized water, stirs 2 hours under 20 DEG C of environment, obtain homogeneous solution.In solution, inject 1 ml hydrazine hydrate with liquid-transfering gun fast, continue stirring 24 little of reaction end.Go out product, and filter repeatedly with deionized water, ethanol successively, dry, grinding.Fig. 2 is the X ray diffractive crystal structure collection of illustrative plates of this target product, and can find out, product is hausmannite type, does not have dephasign, and peak is narrow, peak shape is sharp-pointed and intensity is high, shows this Mn
3o
4crystalline structure complete, phase Mn oxide substantially free from foreign meter.Fig. 3 is the stereoscan photograph of this product, can find out, the Mn of synthesis
3o
4nanocrystal has homogeneous square mesa-shaped pattern.Fig. 4 is the transmission electron microscope photo of this product, can find out, the Mn of synthesis
3o
4the length of side of nanocrystal is 100nm.
embodiment 2
Under room temperature, 0.5g tetra-acetate hydrate manganese is dissolved in 60ml deionized water, stirs 2 hours under 60 DEG C of environment, obtain homogeneous solution.In solution, inject 1ml hydrazine hydrate with liquid-transfering gun fast, continue stirring 24 little of reaction end.Take out product, and filter repeatedly with deionized water, ethanol successively, dry, grinding.Fig. 5 is the transmission electron microscope photo of this product, can find out, the Mn of synthesis
3o
4the pattern of nanocrystal is elliposoidal.
embodiment 3
Under room temperature, 0.25g tetra-acetate hydrate manganese is dissolved in 60ml deionized water, stirs 2 hours under 20 DEG C of environment, obtain homogeneous solution.In solution, inject 1ml hydrazine hydrate with liquid-transfering gun fast, continue stirring reaction in 24 hours and terminate.Take out product, and filter repeatedly with deionized water, ethanol successively, dry, grinding.Fig. 6 is the transmission electron microscope photo of this product, can find out, the square mesa-shaped Mn of synthesis
3o
4the length of side of nanocrystal is 50nm.
embodiment 4
Under room temperature, 1g tetra-acetate hydrate manganese is dissolved in 60ml deionized water, stirs 2 hours under 20 DEG C of environment, obtain homogeneous solution.In solution, inject 1ml hydrazine hydrate with liquid-transfering gun fast, continue stirring reaction in 24 hours and terminate.Take out product, and centrifugal with deionized water, ethanol and filter repeatedly successively, dry, grinding.Fig. 7 is the transmission electron microscope photo of this product, can find out, the square mesa-shaped Mn of synthesis
3o
4the length of side of nanocrystal is 160nm.
embodiment 5
Under room temperature, 0.125g tetra-acetate hydrate manganese is dissolved in 60ml deionized water, stirs 2 hours under 20 DEG C of environment, obtain homogeneous solution.In solution, inject 5ml hydrazine hydrate with liquid-transfering gun fast, continue stirring 24 little of reaction end.Take out product, and centrifugal with deionized water, ethanol and filter repeatedly successively, dry, grinding.Fig. 8 is the stereoscan photograph of this product, can find out, the Mn of synthesis
3o
4nanocrystal be disc-shaped, diameter is 370nm.
embodiment 6
Under room temperature, 0.01g tetra-chloride hydrate manganese is dissolved in 60ml deionized water, stirs 2 hours under 20 DEG C of environment, obtain homogeneous solution.In solution, inject 5ml hydrazine hydrate with liquid-transfering gun fast, continue stirring 24 little of reaction end.Take out product, and centrifugal with deionized water, ethanol and filter repeatedly successively, dry, grinding.Fig. 9 is the stereoscan photograph of this product, can find out, the Mn of synthesis
3o
4nanocrystal be square piece shape, the length of side is 100nm.
Claims (1)
1. a preparation method for Trimanganese tetroxide nanocrystal, is characterized in that comprising the steps: 10 ~ 1000mg manganese source presoma to add in 30 ~ 300ml deionized water, obtains manganese salt solution after stirring; Then in manganese salt solution, add 0.1 ~ 30ml hydrazine hydrate, continue stirring 6 ~ 24 hours, diafiltration, dry, after grinding, obtain described Trimanganese tetroxide nanocrystal;
Whole reaction process is all at room temperature carried out;
Described manganese source presoma is one or more in following substances: the crystalline hydrate of manganous acetate, Manganous chloride tetrahydrate, manganous sulfate and above material;
Described diafiltration deionized water diafiltration 2 ~ 4 times, subsequently the product after diafiltration is carried out drying in 80 ~ 150 DEG C under air blast condition, time of drying is 3 ~ 5 hours;
Concrete, under room temperature, 0.25-1.0g tetra-acetate hydrate manganese is dissolved in 60ml deionized water, stirs 2 hours, obtain homogeneous solution, in homogeneous solution, inject 1 ml hydrazine hydrate fast, continue stirring 24 hours; Diafiltration, dry, obtaining Trimanganese tetroxide nanocrystal after grinding is homogeneous square mesa-shaped pattern;
Or concrete, be dissolved in 60ml deionized water by 0.5g tetra-acetate hydrate manganese under room temperature, 60 DEG C are stirred 2 hours, obtain homogeneous solution, inject 1 ml hydrazine hydrate fast in homogeneous solution, continue stirring 24 hours; Diafiltration, dry, obtaining Trimanganese tetroxide nanocrystal after grinding is homogeneous ellipse spherical morphology;
Or concrete, under room temperature, 0.125g tetra-acetate hydrate manganese is dissolved in 60ml deionized water, stirs 2 hours, obtain homogeneous solution; In solution, inject 5 ml hydrazine hydrates fast, continue stirring 24 hours; Take out product, diafiltration, dry, obtaining Trimanganese tetroxide nanocrystal after grinding is homogeneous disc-shaped pattern;
Or concrete, under room temperature, 0.01g tetra-chloride hydrate manganese is dissolved in 60ml deionized water, stirs 2 hours, obtain homogeneous solution; In solution, inject 5 ml hydrazine hydrates fast, continue stirring 24 hours; Take out product, diafiltration, dry, obtaining Trimanganese tetroxide nanocrystal after grinding is homogeneous square sheet-like morphology.
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Citations (4)
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|---|---|---|---|---|
| CN1359854A (en) * | 2000-12-19 | 2002-07-24 | 中国科学技术大学 | High-purity tetragonal gamma-MnO3 nano crystal and its preparing process |
| CN102040246A (en) * | 2010-10-27 | 2011-05-04 | 江苏科技大学 | Method for synthesizing manganous-manganic oxide nano material at room temperature by using mild path |
| CN102627330A (en) * | 2012-05-10 | 2012-08-08 | 天津工业大学 | Preparation method of nanometer trimanganese tetroxide |
| CN103011295A (en) * | 2012-12-17 | 2013-04-03 | 攀枝花市立宇矿业有限公司 | Reduction method for producing manganese tetroxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB0011684D0 (en) * | 2000-05-15 | 2000-07-05 | Eveready Battery Inc | Porous manganese dioxide and method of preparation thereof |
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|---|---|---|---|---|
| CN1359854A (en) * | 2000-12-19 | 2002-07-24 | 中国科学技术大学 | High-purity tetragonal gamma-MnO3 nano crystal and its preparing process |
| CN102040246A (en) * | 2010-10-27 | 2011-05-04 | 江苏科技大学 | Method for synthesizing manganous-manganic oxide nano material at room temperature by using mild path |
| CN102627330A (en) * | 2012-05-10 | 2012-08-08 | 天津工业大学 | Preparation method of nanometer trimanganese tetroxide |
| CN103011295A (en) * | 2012-12-17 | 2013-04-03 | 攀枝花市立宇矿业有限公司 | Reduction method for producing manganese tetroxide |
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| 以硫酸锰为原料制备四氧化三锰的理论分析;薛娟琴等;《西安建筑科技大学学报》;20000930;第32卷(第3期);第298-299页 * |
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