CN108538615B - Preparation method of cobaltosic oxide-rare earth ore composite material - Google Patents
Preparation method of cobaltosic oxide-rare earth ore composite material Download PDFInfo
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- CN108538615B CN108538615B CN201810485736.0A CN201810485736A CN108538615B CN 108538615 B CN108538615 B CN 108538615B CN 201810485736 A CN201810485736 A CN 201810485736A CN 108538615 B CN108538615 B CN 108538615B
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- cobaltosic oxide
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- 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
Abstract
The invention discloses a preparation method of cobaltosic oxide-rare earth ore composite material, which comprises the following steps: step one, preparing nanometer cobaltosic oxide: adding a mixed solution of ethylene glycol and water into a magnetic stirrer, then adding cobalt acetate and polyvinyl alcohol, starting the magnetic stirrer, stirring at the rotation speed of 115-125r/min for 25-35min, then sending into a reaction kettle, carrying out hydrothermal reaction at the temperature of 155-255 ℃ for 35-45min, then cooling to room temperature, then centrifuging, washing, drying in a drying box for 18-24h, and heating the dried product in a heating furnace to obtain the nano cobaltosic oxide. According to the preparation method of the cobaltosic oxide-rare earth ore composite material, the prepared composite material is applied to the super capacitor, the specific capacitance is improved, the process is simple, and the preparation cost is low.
Description
Technical Field
The invention relates to the technical field of composite material preparation, in particular to a preparation method of a cobaltosic oxide-rare earth ore composite material.
Background
The super capacitor is a novel energy storage device between a traditional capacitor and a rechargeable battery, the capacity of the super capacitor can reach hundreds to thousands of methods, and compared with the traditional capacitor, the super capacitor has larger capacity, specific energy or capacity density, wider working temperature range and extremely long service life; compared with a storage battery, the battery has higher specific power and no pollution to the environment; because the environmental problem is serious day by day, the research on clean energy is continuously developed, and the nano cobaltosic oxide is applied to the lithium ion battery, has the advantages of low self-discharge rate, long service life, high energy density and the like, so that the nano cobaltosic oxide is more and more popular to be researched in the aspect of a super capacitor, and the high specific capacitance is related to the morphological structure and the specific surface area of a composite material, therefore, the invention researches the preparation of the cobaltosic oxide-rare earth ore composite material and applies the cobaltosic oxide-rare earth ore composite material to the super capacitor.
In the prior art, the preparation of the cobaltosic oxide-rare earth ore composite material rarely occurs, and meanwhile, the performance deviation of the composite material is very large due to the fact that multiple factors are not controlled in place in the preparation process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a cobaltosic oxide-rare earth ore composite material, the prepared composite material is applied to a super capacitor, the specific capacitance is improved, the process is simple, and the preparation cost is low.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides a preparation method of cobaltosic oxide-rare earth ore composite material, which comprises the following steps:
step one, preparing nanometer cobaltosic oxide: adding a mixed solution of ethylene glycol and water into a magnetic stirrer, then adding cobalt acetate and polyvinyl alcohol, starting the magnetic stirrer, stirring at the rotation speed of 115-125r/min for 25-35min, then sending into a reaction kettle, carrying out hydrothermal reaction at the temperature of 155-255 ℃ for 35-45min, then cooling to room temperature, then centrifuging, washing, drying in a drying box for 18-24h, and heating the dried product in a heating furnace to obtain the nano cobaltosic oxide;
step two, crushing the rare earth ore, then calcining at the temperature of 1050-, cooling to obtain the cobaltosic oxide-rare earth ore composite material.
Preferably, the mass ratio of the cobalt acetate, the polyvinyl alcohol, the glycol and the water in the first step is (5-9): (1-3): (6-10): 15.
preferably, the conditions in the step one heating furnace are that the temperature is firstly raised to 200-300 ℃, the temperature is preserved for 15-25min, and then the temperature is raised to 450 ℃ and the temperature is preserved for 2 h.
Preferably, the rare earth ore in the second step is one or more of xenotime, spodumene, zircon, mullite, apatite, rutile, ilmenite, fluorite, barite and niobite.
Preferably, the rare earth ore in the second step is spodumene.
Preferably, the amount of aluminum chloride added in the second step is 6-10% of the total amount of the solution.
Preferably, the mass ratio of the nano cobaltosic oxide to the polyvinylpyrrolidone in the second step is (13-17): 3.
preferably, the mass ratio of the nano cobaltosic oxide to the polyvinylpyrrolidone in the second step is 15: 3
Preferably, the heating condition of the two-tube furnace is that the temperature is 350 ℃ for 25-35min, and nitrogen is used as protective gas.
Preferably, the heating condition of the two-tube furnace is that the temperature is 350 ℃ for 30min, and nitrogen is used as protective gas.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the preparation method of the cobaltosic oxide-rare earth ore composite material, the nano cobaltosic oxide is prepared, the mass ratio of cobalt acetate, polyvinyl alcohol, glycol and water substances and the calcining condition of a heating furnace are explored in the preparation process, so that the specific surface area of the nano cobaltosic oxide is large, the nano cobaltosic oxide has a good surface structure, and the nano cobaltosic oxide is compounded with the rare earth ore, so that the specific capacitance is improved.
(2) According to the preparation method of the cobaltosic oxide-rare earth ore composite material, the rare earth ore is compounded with the nano cobaltosic oxide after a series of treatments, and the change of various factors in compounding can greatly influence the material properties.
(3) According to the preparation method of the cobaltosic oxide-rare earth ore composite material, the prepared composite material is applied to the super capacitor, the specific capacitance is improved, the process is simple, and the preparation cost is low.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1.
The preparation method of the cobaltosic oxide-rare earth ore composite material of the embodiment comprises the following steps:
step one, preparing nanometer cobaltosic oxide: adding a mixed solution of ethylene glycol and water into a magnetic stirrer, then adding cobalt acetate and polyvinyl alcohol, starting the magnetic stirrer, stirring at the rotating speed of 115r/min for 25min, then sending into a reaction kettle, carrying out hydrothermal reaction at the temperature of 155 ℃ for 35min, then cooling to room temperature, then centrifuging, washing, drying in a drying oven for 18h, and heating the dried product in a heating furnace to obtain nano cobaltosic oxide;
and step two, crushing the rare earth ore, then calcining at 1050 ℃, calcining for 25min, then sending into an ethanol solution for ultrasonic dispersion, dispersing for 15-25min, then centrifuging at 2500r/min, taking centrifugate for suction filtration, drying, adding the dried rare earth ore into water for stirring and mixing at 55r/min, then regulating the pH to 4 with hydrochloric acid, then adding an aluminum chloride solution with the mass fraction of 2%, then adding polyvinylpyrrolidone, continuing stirring for 5min, then adding the nano cobaltosic oxide prepared in the step one, increasing the stirring speed to 105r/min, stirring for 45min, then centrifuging, sending the centrifugate into a tube furnace for heating, and cooling to obtain the cobaltosic oxide-rare earth ore composite material.
In the first step of this embodiment, the mass ratio of the cobalt acetate, the polyvinyl alcohol, the ethylene glycol, and the water is 5: 1: 6: 15.
in the first step of this example, the temperature in the furnace is first raised to 200 ℃ and kept for 15min, and then raised to 450 ℃ and kept for 2 h.
In the second step of this example, the rare earth ore is xenotime.
In the second step of this example, aluminum chloride was added in an amount of 6% of the total amount of the solution.
In the second step of this embodiment, the mass ratio of the nano cobaltosic oxide to the polyvinylpyrrolidone is 13: 3.
in the present example, the two-tube furnace was heated at 350 ℃ for 25min under nitrogen as a shielding gas.
Example 2.
The preparation method of the cobaltosic oxide-rare earth ore composite material of the embodiment comprises the following steps:
step one, preparing nanometer cobaltosic oxide: adding a mixed solution of ethylene glycol and water into a magnetic stirrer, then adding cobalt acetate and polyvinyl alcohol, starting the magnetic stirrer, stirring at the rotating speed of 125r/min for 35min, then sending into a reaction kettle, carrying out hydrothermal reaction at the temperature of 255 ℃ for 45min, then cooling to room temperature, then centrifuging, washing, drying in a drying oven for 24h, and heating the dried product in a heating furnace to obtain nano cobaltosic oxide;
and step two, crushing the rare earth ore, then calcining at 1150 ℃, calcining for 35min, then sending into an ethanol solution for ultrasonic dispersion, dispersing for 15-25min, then centrifuging at 3500r/min, taking centrifugate for suction filtration, drying, adding the dried rare earth ore into water for stirring and mixing at 65r/min, then adjusting the pH to 6 with hydrochloric acid, then adding an aluminum chloride solution with the mass fraction of 2%, then adding polyvinylpyrrolidone, continuing stirring for 5-15min, then adding the nano cobaltosic oxide prepared in the step one, increasing the stirring speed to 115r/min, stirring for 55min, then centrifuging, sending the centrifugate into a tube furnace for heating, and cooling to obtain the cobaltosic oxide-rare earth ore composite material.
In the first step of this embodiment, the mass ratio of the cobalt acetate, the polyvinyl alcohol, the ethylene glycol, and the water is 9: 3: 10: 15.
in the first step of this example, the temperature in the furnace is first raised to 300 ℃ and then kept for 25min, and then raised to 450 ℃ and kept for 2 h.
In the second step of this example, the rare earth ore is spodumene.
In the second step of this example, the rare earth ore is spodumene.
In the second step of this example, aluminum chloride was added in an amount of 10% of the total amount of the solution.
In the second step of this embodiment, the mass ratio of the nano cobaltosic oxide to the polyvinylpyrrolidone is 17: 3.
in the present example, the two-tube furnace is heated at 350 deg.C for 35min under nitrogen as a shielding gas.
Example 3.
The preparation method of the cobaltosic oxide-rare earth ore composite material of the embodiment comprises the following steps:
step one, preparing nanometer cobaltosic oxide: adding a mixed solution of ethylene glycol and water into a magnetic stirrer, then adding cobalt acetate and polyvinyl alcohol, starting the magnetic stirrer, stirring at the rotating speed of 120r/min for 30min, then sending into a reaction kettle, carrying out hydrothermal reaction at the temperature of 200 ℃ for 40min, then cooling to room temperature, then centrifuging, washing, drying in a drying oven for 21h, and heating the dried product in a heating furnace to obtain nano cobaltosic oxide;
and step two, crushing the rare earth ore, then calcining at 1100 ℃, calcining for 30min, then sending into an ethanol solution for ultrasonic dispersion, dispersing for 20min, then centrifuging at a centrifugal rotation speed of 3000r/min, taking the centrifugal liquid for suction filtration, drying, adding the dried rare earth ore into water for stirring and mixing at a stirring rotation speed of 60r/min, then regulating the pH to 5 with hydrochloric acid, then adding an aluminum chloride solution with a mass fraction of 2%, then adding polyvinylpyrrolidone, continuing stirring for 10min, then adding the nano cobaltosic oxide prepared in the step one, increasing the stirring rotation speed to 110r/min, stirring for 50min, then centrifuging, sending the centrifugal liquid into a tubular furnace for heating, and cooling to obtain the cobaltosic oxide-rare earth ore composite material.
In the first step of this embodiment, the mass ratio of the cobalt acetate, the polyvinyl alcohol, the ethylene glycol, and the water is 7: 2: 8: 15.
in the first step of this example, the temperature in the furnace is first raised to 250 ℃ and then maintained for 20min, and then the temperature is raised to 450 ℃ and maintained for 2 h.
In the second step of this example, the rare earth ore is zircon.
In the second step of this example, aluminum chloride was added in an amount of 8% of the total amount of the solution.
In the second step of this embodiment, the mass ratio of the nano cobaltosic oxide to the polyvinylpyrrolidone is 15: 3.
in the present example, the two-tube furnace is heated at 350 deg.C for 30min under nitrogen as the shielding gas.
The embodiments 1 to 3 are only partial experimental data of the invention, and a large amount of experimental demonstration proves that the invention provides a preparation method of the cobaltosic oxide-rare earth ore composite material, and the prepared composite material is applied to the super capacitor, so that the specific capacitance is improved, in addition, the process is simple, and the preparation cost is low.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. The preparation method of the cobaltosic oxide-rare earth ore composite material is characterized by comprising the following steps of:
step one, preparing nanometer cobaltosic oxide: adding a mixed solution of ethylene glycol and water into a magnetic stirrer, then adding cobalt acetate and polyvinyl alcohol, starting the magnetic stirrer, stirring at the rotation speed of 115-125r/min for 25-35min, then sending into a reaction kettle, carrying out hydrothermal reaction at the temperature of 155-255 ℃ for 35-45min, then cooling to room temperature, then centrifuging, washing, drying in a drying box for 18-24h, and heating the dried product in a heating furnace to obtain the nano cobaltosic oxide;
step two, crushing rare earth ore which is one or a composition of more of xenotime, spodumene, zircon, andalusite, apatite, rutile, ilmenite, fluorite, barite and niobite, calcining at 1050-1150 ℃, calcining for 25-35min, then sending into ethanol solution for ultrasonic dispersion, dispersing for 15-25min, then centrifuging at 2500-3500r/min, taking the centrifugate for suction filtration, drying, adding the dried rare earth ore into water for stirring and mixing at 55-65r/min, then adjusting the pH to 4-6 with hydrochloric acid, then adding 2% aluminum chloride solution by mass fraction, then adding polyvinylpyrrolidone, continuing stirring for 5-15min, then adding the nano cobaltosic oxide prepared in the step one, the stirring speed is increased to 105-115r/min, the stirring time is 45-55min, then the centrifugal liquid is centrifuged, and the centrifugal liquid is sent into a tube furnace for heating and cooling, thus obtaining the cobaltosic oxide-rare earth ore composite material.
2. The method for preparing the cobaltosic oxide-rare earth ore composite material according to claim 1, wherein the mass ratio of the cobalt acetate, the polyvinyl alcohol, the ethylene glycol and the water in the first step is (5-9): (1-3): (6-10): 15.
3. the method as claimed in claim 1, wherein the heating furnace is heated to 200-300 ℃ for 15-25min, and then heated to 450 ℃ for 2 h.
4. The method for preparing the cobaltosic oxide-rare earth ore composite material according to claim 1, wherein the mass ratio of the nano cobaltosic oxide to the polyvinylpyrrolidone in the second step is (13-17): 3.
5. the method for preparing the cobaltosic oxide-rare earth ore composite material according to claim 4, wherein the mass ratio of the nano cobaltosic oxide to the polyvinylpyrrolidone in the second step is 15: 3.
6. the method for preparing a cobaltosic oxide-rare earth ore composite material according to claim 1, wherein the heating condition of the two-tube furnace in the step is heating at 350 ℃ for 25-35min, and nitrogen is used as shielding gas.
7. The method for preparing a cobaltosic oxide-rare earth ore composite material according to claim 6, wherein the heating condition of the two-tube furnace is that the temperature is 350 ℃ for 30min, and nitrogen is used as shielding gas.
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| CN107673412A (en) * | 2017-11-17 | 2018-02-09 | 东华大学 | A kind of porous Co3O4 nanometer material and its preparation method and application |
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| CN102842705B (en) * | 2011-06-22 | 2015-03-11 | 清华大学 | Cobalt oxide and composite material thereof, and preparation method of cobalt oxide composite material |
| CN102324320B (en) * | 2011-07-29 | 2015-06-10 | 上海奥威科技开发有限公司 | High-performance super capacitor |
| CN102531070B (en) * | 2011-12-30 | 2013-09-25 | 郑州轻工业学院 | Co3O4 nanometer material for supercapacitor and preparation method thereof |
| CN108034964B (en) * | 2017-12-20 | 2019-09-06 | 精细化学品集团有限公司 | A kind of technique for being separated from Rare Earth Mine and extracting phosphorus yttrium element |
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