CN114604898A - Porous MnO 2 Preparation method of nano material - Google Patents
Porous MnO 2 Preparation method of nano material Download PDFInfo
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- CN114604898A CN114604898A CN202210206629.6A CN202210206629A CN114604898A CN 114604898 A CN114604898 A CN 114604898A CN 202210206629 A CN202210206629 A CN 202210206629A CN 114604898 A CN114604898 A CN 114604898A
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims description 24
- 239000012265 solid product Substances 0.000 claims description 12
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 3
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 abstract description 8
- 239000010405 anode material Substances 0.000 abstract description 7
- 238000005303 weighing Methods 0.000 abstract description 3
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 abstract description 2
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 abstract description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 26
- 239000007772 electrode material Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 239000003245 coal Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229940063656 aluminum chloride Drugs 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000012983 electrochemical energy storage Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- SZKTYYIADWRVSA-UHFFFAOYSA-N zinc manganese(2+) oxygen(2-) Chemical compound [O--].[O--].[Mn++].[Zn++] SZKTYYIADWRVSA-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
-
- 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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
-
- 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
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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
- C01P2004/01—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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses porous MnO 2 The preparation method of the nano material comprises the following steps: weighing urea and citric acid with a molar ratio of 1; then weighing aluminum chloride hexahydrate and potassium permanganate with the molar ratio of 1; slowly dripping the solution A into the solution B under the stirring condition, stirring for two hours after dripping, and standing for one hour; centrifuging with centrifuge, washing with deionized water for 3 times, washing with ethanol for 1 time, drying in oven at 90 deg.C for 10 hr, grinding, and storing. The core of the method is to adopt lemonReduction of potassium permanganate by citric acid to prepare MnO 2 The nano material is used as the anode material of the zinc-manganese secondary battery, and has good electrochemical performance, good charge-discharge reversibility and high charge-discharge specific capacity.
Description
Technical Field
The invention relates to porous MnO 2 A method for preparing nano material.
Background
With the development of human society, energy and environmental issues become the two most important issues in the world today. Particularly, with the development of economy, the demand of human beings for energy is increasing. The traditional energy sources represented by coal and petroleum face a plurality of problems, one is that the application of the coal and the petroleum can generate toxic gas to pollute the environment, and in addition, the coal and the petroleum belong to non-renewable resources and face rapid exhaustion of the resources. Therefore, the development of new green renewable energy sources becomes a hot spot of scientific research at present. At present, new energy sources such as wind energy, solar energy, and nuclear energy are being developed in large quantities. However, the electric energy generated by wind energy, solar energy and nuclear energy has the characteristic of being incapable of being stored, so the research and development of energy storage technology are the core problems of the current energy problems. At present, electrochemical energy storage devices are widely used due to convenience and practicality, for example, lithium ion batteries are widely used in notebook computers, small electronic products, electric vehicles and other devices. Therefore, batteries are widely used as the main device for electrochemical energy storage for a long time in the future.
Manganese dioxide is the most widely used positive electrode material for zinc-manganese batteries. MnO (MnO) 2 Has the advantages of rich natural resources, low cost, no toxicity, high specific capacity and the like, and becomes the most potential electrode material.
The anode material of the current zinc-manganese battery is mainly electrolytic manganese dioxide, and although the electrolytic manganese dioxide is the best electrode material of the current zinc-manganese battery, the electrolytic manganese dioxide has some defects. One is that the electrolytic manganese dioxide is only the anode material of the zinc-manganese primary battery, can not be charged, and has poor electrochemical cycle performance; and the specific capacity of the electrolytic manganese dioxide cathode material is relatively low. Influence of MnO 2 The electrochemical performance of the electrode material is relatively complex, and the electrochemical performance of the electrode material is greatly influenced by crystal form, particle size, morphology and the like of manganese dioxide. Therefore, the key to improving the electrochemical performance of manganese dioxide is to prepare a manganese dioxide material with a proper crystal form and proper particle size and morphology. The main solution at present is to prepare manganese dioxide nano-material, which has the characteristics of small particle size, large specific surface area and the like, and the small particle size and the large specific surface area are beneficial to full contact between the electrode material and the electrolyte, so that the electrochemical performance of the electrode material can be improved. The method for reducing potassium permanganate by using citric acid prepares the porous manganese dioxide nano material, and greatly improvesThe electrochemical performance of manganese dioxide is improved.
Disclosure of Invention
The invention aims to provide porous MnO 2 A method for preparing nano material, which aims to solve the problems in the prior art. The method provided by the invention is simple to operate and quick in reaction, and the prepared product has good charge-discharge cycle performance and higher specific capacity when being used as the anode material of the zinc-manganese secondary battery.
In order to achieve the purpose, the invention provides the following technical scheme:
porous MnO 2 The preparation method of the nano material comprises the following steps:
s1: preparing a mixed solution A by utilizing analytically pure urea and analytically pure citric acid with a certain molar ratio, and preparing a mixed solution B by utilizing analytically pure aluminum chloride and analytically pure potassium permanganate with a certain molar ratio for later use;
s2: slowly dripping the mixed solution A into the mixed solution B, and stirring and mixing to obtain a mixture C;
s3: and separating the mixture C by using a centrifugal machine to obtain a solid product, washing the solid product, drying, grinding and storing.
Further, in S1, analytically pure urea and analytically pure citric acid were prepared in a molar ratio of 1.
Further, in S1, analytically pure aluminum chloride and analytically pure potassium permanganate are prepared into a mixed solution B according to a molar ratio of 1.
Further, in the step S2, the mixed solution a is mixed with the mixed solution B in a dropping manner, and is continuously stirred during the mixing process.
Further, in S3, after the mixed solution C is obtained, the mixed solution C is continuously stirred for 2 hours, and is kept stand for 1 hour and then is separated by a centrifuge.
Further, in S3, the solid product obtained by separation is washed by deionized water for 3 times and ethanol for 1 time, then the solid product is dried in an oven at 90 ℃ for 10 hours, and then the finished product is ground and stored.
Compared with the prior art, the invention has the beneficial effects that:
(1) The prepared manganese dioxide material has small particles, reaches the micro-nano size, and is a porous material. The zinc-manganese oxide/zinc oxide composite anode material is used as an anode material of a zinc-manganese battery, has relatively symmetrical redox peaks in zinc sulfate neutral electrolyte, and is suitable for being used as an anode material of a neutral zinc-manganese secondary battery. The charging and discharging tests show that the highest specific discharge capacity reaches 456.3mAh/g in the charging and discharging tests of 100 cycles, and the specific discharge capacity can still be maintained at 156.3mAh/g after 100 cycles of charging and discharging.
Drawings
FIG. 1 shows porous MnO prepared according to the present invention 2 XDR pattern of the nanomaterials;
FIG. 2 shows porous MnO prepared according to the present invention 2 SEM images of nanomaterials.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples:
examples
As shown in FIG. 1 and FIG. 2, a porous MnO is provided 2 The preparation method of the nano material comprises the following steps:
s1: accurately weighing analytically pure urea and analytically pure citric acid in a molar ratio of 1; analytically pure aluminum chloride hexahydrate and analytically pure potassium permanganate in a molar ratio of 1.
S2: and slowly dripping the mixed solution A into the mixed solution B under the stirring condition to obtain a mixed solution C, stirring the mixed solution C for 2 hours after the dripping of the mixed solution C is finished, and standing for 1 hour.
S3: and (3) carrying out centrifugal separation on the mixed solution C by using a centrifugal machine to obtain a solid product, washing the solid product by using deionized water for 3 times and ethanol for 1 time, then drying the solid product in an oven at the temperature of 90 ℃ for 10 hours, and grinding and storing the dried solid product.
The foregoing is merely an example of the present invention and common general knowledge in the art of designing and/or characterizing particular aspects and/or features is not described in any greater detail herein. It should be noted that, for those skilled in the art, without departing from the technical solution of the present invention, several variations and modifications can be made, and these should also be considered as the protection scope of the present invention, which will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be defined by the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (6)
1. Porous MnO 2 The preparation method of the nano material is characterized by comprising the following steps of:
s1: preparing a mixed solution A by utilizing analytically pure urea and analytically pure citric acid with a certain molar ratio, and preparing a mixed solution B by utilizing analytically pure aluminum chloride and analytically pure potassium permanganate with a certain molar ratio for later use;
s2: slowly dripping the mixed solution A into the mixed solution B, and stirring and mixing to obtain a mixture C;
s3: and separating the mixture C by using a centrifugal machine to obtain a solid product, washing the solid product, drying, grinding and storing.
2. The porous MnO of claim 1 2 The preparation method of the nano material is characterized by comprising the following steps: in S1, the analytically pure urea and the analytically pure citric acid are prepared into a mixed solution A according to a molar ratio of 1.
3. The porous MnO of claim 1 2 The preparation method of the nano material is characterized by comprising the following steps: in S1, preparing a mixed solution B from analytically pure aluminum chloride and analytically pure potassium permanganate according to a molar ratio of 1.
4. The method of claim 1Porous MnO 2 The preparation method of the nano material is characterized by comprising the following steps: and in the step S2, the mixed solution A is mixed with the mixed solution B in a dropping mode and is continuously stirred in the mixing process.
5. The porous MnO of claim 1 2 The preparation method of the nano material is characterized by comprising the following steps: and in the S3, continuously stirring for 2h after the mixed solution C is obtained, standing for 1h, and then separating by using a centrifugal machine.
6. The porous MnO of claim 1 2 The preparation method of the nano material is characterized by comprising the following steps: and S3, washing the solid product obtained by separation for 3 times by using deionized water and 1 time by using ethanol, then drying the solid product in an oven at the temperature of 90 ℃ for 10 hours, and grinding and storing the finished product.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001087775A1 (en) * | 2000-05-15 | 2001-11-22 | Eveready Battery Company Inc. | A method of preparation of porous manganese dioxide |
| US20110044887A1 (en) * | 2008-03-25 | 2011-02-24 | Nanotecture Ltd. | Mesoporous manganese dioxide |
| CN103754936A (en) * | 2014-01-23 | 2014-04-30 | 山东科技大学 | Method for synthesizing mesoporous manganese oxide |
| CN104124074A (en) * | 2014-07-09 | 2014-10-29 | 上海应用技术学院 | Porous manganese dioxide and preparation method thereof |
| CN106430263A (en) * | 2016-09-13 | 2017-02-22 | 苏州市泽镁新材料科技有限公司 | Preparation method of magnesium oxide nanoparticles |
| CN106848290A (en) * | 2017-03-10 | 2017-06-13 | 陕西科技大学 | A kind of lithium ion battery MnO nano bowls and preparation method thereof |
-
2022
- 2022-03-03 CN CN202210206629.6A patent/CN114604898A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001087775A1 (en) * | 2000-05-15 | 2001-11-22 | Eveready Battery Company Inc. | A method of preparation of porous manganese dioxide |
| US20110044887A1 (en) * | 2008-03-25 | 2011-02-24 | Nanotecture Ltd. | Mesoporous manganese dioxide |
| CN103754936A (en) * | 2014-01-23 | 2014-04-30 | 山东科技大学 | Method for synthesizing mesoporous manganese oxide |
| CN104124074A (en) * | 2014-07-09 | 2014-10-29 | 上海应用技术学院 | Porous manganese dioxide and preparation method thereof |
| CN106430263A (en) * | 2016-09-13 | 2017-02-22 | 苏州市泽镁新材料科技有限公司 | Preparation method of magnesium oxide nanoparticles |
| CN106848290A (en) * | 2017-03-10 | 2017-06-13 | 陕西科技大学 | A kind of lithium ion battery MnO nano bowls and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| YAN-JING YANG: "Nanostructured amorphous MnO2 prepared by reaction of KMnO4 with triethanolamine", JOURNAL OF ALLOYS AND COMPOUNDS, vol. 505, pages 555 - 559, XP027220440 * |
| 曹凤;张文彦;张思思;燕阳天;杨瑞锋;: "多孔金属材料的化学制备方法及性能研究进展", 材料导报, no. 21, pages 142 - 148 * |
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