CN1831210A - Method for preparing multi-branched hydroxy manganese oxide single crystal nanometer flower - Google Patents
Method for preparing multi-branched hydroxy manganese oxide single crystal nanometer flower Download PDFInfo
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- CN1831210A CN1831210A CN 200610049546 CN200610049546A CN1831210A CN 1831210 A CN1831210 A CN 1831210A CN 200610049546 CN200610049546 CN 200610049546 CN 200610049546 A CN200610049546 A CN 200610049546A CN 1831210 A CN1831210 A CN 1831210A
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- single crystal
- manganese oxide
- oxide single
- flower
- nanometer flower
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- 239000013078 crystal Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 10
- PVIFNYFAXIMOKR-UHFFFAOYSA-M manganese(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Mn+3] PVIFNYFAXIMOKR-UHFFFAOYSA-M 0.000 title claims description 17
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 229960003511 macrogol Drugs 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- 239000012456 homogeneous solution Substances 0.000 claims description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- -1 polyoxyethylene Polymers 0.000 claims description 5
- IQXJCCZJOIKIAD-UHFFFAOYSA-N 1-(2-methoxyethoxy)hexadecane Chemical compound CCCCCCCCCCCCCCCCOCCOC IQXJCCZJOIKIAD-UHFFFAOYSA-N 0.000 claims description 3
- 229950009789 cetomacrogol 1000 Drugs 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 12
- 239000002808 molecular sieve Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 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
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 abstract 4
- 239000002202 Polyethylene glycol Substances 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 229920001223 polyethylene glycol Polymers 0.000 abstract 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 13
- 229910052748 manganese Inorganic materials 0.000 description 13
- 239000011572 manganese Substances 0.000 description 13
- 239000000047 product Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000002003 electron diffraction Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 150000002927 oxygen compounds Chemical class 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 238000003828 vacuum filtration Methods 0.000 description 2
- 229910008090 Li-Mn-O Inorganic materials 0.000 description 1
- 229910006369 Li—Mn—O Inorganic materials 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method to make multi-branch hydroxy group manganese oxide single crystal nm flower that uses potassium permanganate as oxidant, polyethylene glycol as reducer to take hydrothermal reaction in 100-200 degree centigrade in sealed reactor. By controlling the reacting temperature, time, and raw material proportion, the multi-branch hydroxyl group manganese oxide single crystal nm flower would be gained. The diameter could be between 40-100nm, and the length is 800-1200nm. The method has simple technology, low cost, high purity, and stable quality. The flower could be used to do basic theory research in lithium ion battery and molecular sieve.
Description
Technical field
The present invention relates to a kind of preparation of nanomaterials, be specifically related to the preparation method of multi-branched hydroxy manganese oxide single crystal nanometer flower.
Background technology
The oxyhydroxide of manganese all has crucial purposes in fields such as electrochemistry, battery, electrochromism.Hydroxyl oxidize manganese also can be used as Li-Mn-O spinel structure and MnO
2Wait the presoma of other manganese and oxygen compounds, and manganese and oxygen compound there is being very superior performance aspect secondary cell, molecular sieve and the catalysis, also is being subjected to scientific circles always and pays close attention to widely.At present, hydroxyl oxidize manganese nano material synthetic report mainly is the synthetic of nanometer rod, [Materials Letters 2001 such as Sharma, 48,319] synthesized hydroxyl oxidize manganese nanometer rod in the auxiliary hydro-thermal down of tensio-active agent, [Solid State Communications2005 such as Zhang Yuangguang, 124,523] in the auxiliary reductive water thermal synthesis down of surfactant-free hydroxyl oxidize manganese nanometer rod, [chemical journal, 2004,62 such as Dong Xiyan, 2441] synthesized hydroxyl oxidize manganese nanometer rod with reverse micelle method, the synthetic report that yet there are no of the hydroxyl oxidize manganese of racemosus shape nanometer flower structure.
Summary of the invention
The purpose of this invention is to provide a kind of being beneficial to and realize large-scale industrial production, technology is simple, and cost is low, the method for preparing multi-branched hydroxy manganese oxide single crystal nanometer flower of constant product quality.
The method for preparing multi-branched hydroxy manganese oxide single crystal nanometer flower of the present invention is an oxygenant with potassium permanganate, and polyoxyethylene glycol is a reductive agent, carries out in closed reactor, and its step is as follows:
1) is to join in deionized water at 0.5～3: 10～20 potassium permanganate and polyoxyethylene glycol by the ratio of amount of substance, is stirred to homogeneous solution;
2) above-mentioned solution is put into the encloses container reactor, reacted 8～16 hours under 100～200 ℃ of temperature condition, be cooled to room temperature then, filtration, washing, drying get final product.
Among the present invention, said polyoxyethylene glycol can be Macrogol 200, cetomacrogol 1000 0 or Macrogol 2000 0.
Among the present invention, the stirring of step 1) was generally 5～30 minutes; The said dry conventional vacuum-drying of adopting; Said washing is to adopt deionized water and the unreacted unnecessary ion of dehydrated alcohol eccysis.
The present invention can prepare multi-branched hydroxy manganese oxide single crystal nanometer flower by control hydrothermal temperature, reaction times and proportioning raw materials.Each branched diameter of the multi-branched hydroxy manganese oxide single crystal nanometer flower that makes is at 40～100nm, and length is 800～1200nm.
The inventive method raw material is cheap and easy to get, and technology is simple, and cost is low, the product purity height, and steady quality, good reproducibility helps large-scale industrial production.The multi-branched hydroxy manganese oxide single crystal nanometer flower that makes can be widely used in the fundamental research of lithium ion battery, molecular sieve etc. and association area.
Description of drawings
Fig. 1 is the XRD figure of multi-branched hydroxy manganese oxide single crystal nanometer flower;
Fig. 2 is the transmission electron microscope photo of multi-branched hydroxy manganese oxide single crystal nanometer flower;
Fig. 3 is the transmission electron microscope photo of single multi-branched hydroxy manganese oxide single crystal nanometer flower;
Fig. 4 is that transmission electron microscope photo is amplified in the part of single multi-branched hydroxy manganese oxide single crystal nanometer flower;
Fig. 5 is the electron diffraction photo of single branch hydroxyl oxidize manganese.
Embodiment
Embodiment
Embodiment 1
0.325 gram analytical pure potassium permanganate and 2ml Macrogol 200 are placed the withstand voltage reactor of 150ml Stainless Steel, add 80% still volumetrical deionized water, stir and form homogeneous solution.Sealed reactor was 160 ℃ of reactions 12 hours.Be cooled to room temperature then, open reactor, vacuum filtration, with deionized water and absolute ethanol washing, the dry brown-green powder that gets.Product is accredited as hydroxyl oxidize manganese through X-ray powder diffraction, its XRD figure such as Fig. 1; TEM Electronic Speculum testing product pattern, its TEM are schemed as Fig. 2, and 3,4, the single branch diameter of nanometer flower is 40～100nm as can be seen, length is 800～1200nm.The single branch electron diffraction (Fig. 5) of nanometer flower proves that product is a monocrystalline.Under similarity condition, temperature of reaction is controlled at 100 ℃ or 200 ℃, all can obtain multi-branched hydroxy manganese oxide nanometer flower.
Embodiment 2
0.325 gram analytical pure potassium permanganate and 6ml cetomacrogol 1000 0 are placed the withstand voltage reactor of 150ml Stainless Steel, add 80% still volumetrical deionized water, stir and form homogeneous solution.Sealed reactor was 160 ℃ of reactions 12 hours.Be cooled to room temperature then, open reactor, vacuum filtration, with deionized water and absolute ethanol washing, the dry brown-green powder that gets.Product is accredited as hydroxyl oxidize manganese through X-ray powder diffraction; TEM Electronic Speculum testing product pattern: diameter 40～120nm, length 800～1000nm.The single branch electron diffraction proof product of nanometer flower is a monocrystalline.Under similarity condition, temperature of reaction is controlled at 100 ℃ or 200 ℃, all can obtain multi-branched hydroxy manganese oxide nanometer flower.
Embodiment 3
0.325 gram analytical pure potassium permanganate and 12ml Macrogol 2000 0 are placed the withstand voltage reactor of 150ml Stainless Steel, add 80% still volumetrical deionized water, stir and form homogeneous solution.Sealed reactor was 160 ℃ of reactions 12 hours.Be cooled to room temperature then, open reactor, vacuum filters, with deionized water and absolute ethanol washing, and the dry brown-green powder that gets.Product is accredited as hydroxyl oxidize manganese through X-ray powder diffraction; TEM Electronic Speculum testing product pattern: diameter 40～160nm, length 600～1000nm.The single branch electron diffraction proof product of nanometer flower is a monocrystalline.Under similarity condition, temperature of reaction is controlled at 100 ℃ or 200 ℃, all can obtain multi-branched hydroxy manganese oxide nanometer flower.
Claims (2)
1. method for preparing multi-branched hydroxy manganese oxide single crystal nanometer flower, its step is as follows:
1) is to join in deionized water at 0.5～3: 10～20 potassium permanganate and polyoxyethylene glycol by the ratio of amount of substance, is stirred to homogeneous solution;
2) above-mentioned solution is put into the encloses container reactor, reacted 8～16 hours under 100～200 ℃ of temperature condition, be cooled to room temperature then, filtration, washing, drying get final product.
2. the method for preparing multi-branched hydroxy manganese oxide single crystal nanometer flower according to claim 1 is characterized in that said polyoxyethylene glycol is Macrogol 200, cetomacrogol 1000 0 or Macrogol 2000 0.
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| CNB2006100495461A CN100347345C (en) | 2006-02-20 | 2006-02-20 | Method for preparing multi-branched hydroxy manganese oxide single crystal nanometer flower |
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| CNB2006100495461A CN100347345C (en) | 2006-02-20 | 2006-02-20 | Method for preparing multi-branched hydroxy manganese oxide single crystal nanometer flower |
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| CN1831210A true CN1831210A (en) | 2006-09-13 |
| CN100347345C CN100347345C (en) | 2007-11-07 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531064A (en) * | 2010-12-13 | 2012-07-04 | 西安迈克森新材料有限公司 | Method used for preparing hydroxy manganese oxide superfine single crystal nanometer line |
| CN103496745A (en) * | 2013-10-09 | 2014-01-08 | 南京信息工程大学 | Method for preparing multi-branched nanometer gamma-MnOOH |
| CN104211123A (en) * | 2014-09-16 | 2014-12-17 | 吉林大学 | Preparation method for manganese oxide nano rods |
| CN104229780A (en) * | 2014-08-30 | 2014-12-24 | 长春工业大学 | Preparation method of graphene-based complex |
| CN104658763A (en) * | 2015-01-21 | 2015-05-27 | 西北大学 | Manganese dioxide dendritic nano array electrode material and preparation method |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1142103C (en) * | 2002-01-18 | 2004-03-17 | 清华大学 | Process for synthesizing different crystal form one-dimensional single crystal mangnesium dioxide nano wire |
| JP3903175B2 (en) * | 2002-07-30 | 2007-04-11 | 独立行政法人産業技術総合研究所 | Method for producing manganese dioxide crystal having rock salt type crystal structure |
| CN1312330C (en) * | 2004-07-02 | 2007-04-25 | 中国科学院金属研究所 | α－MnO 2 Preparation method of single crystal nanorod |
-
2006
- 2006-02-20 CN CNB2006100495461A patent/CN100347345C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531064A (en) * | 2010-12-13 | 2012-07-04 | 西安迈克森新材料有限公司 | Method used for preparing hydroxy manganese oxide superfine single crystal nanometer line |
| CN103496745A (en) * | 2013-10-09 | 2014-01-08 | 南京信息工程大学 | Method for preparing multi-branched nanometer gamma-MnOOH |
| CN103496745B (en) * | 2013-10-09 | 2015-04-29 | 南京信息工程大学 | Method for preparing multi-branched nanometer gamma-MnOOH |
| CN104229780A (en) * | 2014-08-30 | 2014-12-24 | 长春工业大学 | Preparation method of graphene-based complex |
| CN104211123A (en) * | 2014-09-16 | 2014-12-17 | 吉林大学 | Preparation method for manganese oxide nano rods |
| CN104658763A (en) * | 2015-01-21 | 2015-05-27 | 西北大学 | Manganese dioxide dendritic nano array electrode material and preparation method |
| CN104658763B (en) * | 2015-01-21 | 2017-03-15 | 西北大学 | A kind of manganese dioxide dendroid nano-array electrode material and preparation method |
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| CN100347345C (en) | 2007-11-07 |
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Granted publication date: 20071107 Termination date: 20100220 |