CN111087027A - Flower-shaped Co3O4Preparation method of micro-sodium structure - Google Patents
Flower-shaped Co3O4Preparation method of micro-sodium structure Download PDFInfo
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- CN111087027A CN111087027A CN201811232720.5A CN201811232720A CN111087027A CN 111087027 A CN111087027 A CN 111087027A CN 201811232720 A CN201811232720 A CN 201811232720A CN 111087027 A CN111087027 A CN 111087027A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/30—Particle morphology extending in three dimensions
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Abstract
The invention discloses flower-shaped Co3O4The preparation method of the micro-sodium structure comprises the following steps: dissolving polyvinylpyrrolidone in water, adding cobalt acetate tetrahydrate, continuously stirring for dissolving, finally adding diethylene glycol, uniformly mixing, transferring the reaction solution into a microwave reaction kettle with a polytetrafluoroethylene lining, sealing, heating to 185-195 ℃ in a microwave digestion instrument for reacting for 1.5-2.5h, stopping the reaction, cooling the reaction product to room temperature, centrifugally separating the obtained precipitate, washing for 4-6 times by using deionized water and ethanol, and drying at 60-70 ℃ to obtain a precursor; transferring the precursor into a crucible, placing the crucible into a muffle furnace, heating to 480-490 ℃ at the heating rate of 2 ℃/min, calcining for 2-3h, and cooling to obtain the catalyst. The method is simple, convenient, quick and easy to operate, and the flower-shaped Co is successfully prepared3O4Micro-sodium structure, good performance and large-scale preparation.
Description
Technical Field
The invention relates to flower-shaped Co3O4A preparation method of a micro-sodium structure.
Background
In recent years, cobalt oxide nano materials have been widely used in the fields of magnetics, catalysis, lithium ion batteries, supercapacitors, sensors and the like due to their unique physical and chemical properties. The performance of the nano material is closely related to the shape, size, crystal structure and other factors, so that the cobalt oxide micro-nano structures with different shapes and sizes are prepared by a simple and cheap synthesis method, and the application of the cobalt oxide micro-nano structures in different fields is especially important to explore. The preparation method of cobalt oxide is mainly divided into a solid phase method and a liquid phase method. The liquid phase method is various, mainly comprises a hydrothermal method, a solvothermal method, a microemulsion method, a sol-gel method, a spray pyrolysis method and the like, and can be used for preparing nano structures with different shapes more easily. Research shows that the cobalt oxide hollow microsphere with the three-layer shell has the best lithium storage performance, and the specific capacity of the cobalt oxide hollow microsphere is still as high as 1615.8mAh/g after 30 cycles under the current density of 50 mA/g. Microwave heating makes the raw material easier to form a large number of crystal nuclei in the initial reaction stage, improves the reaction rate and shortens the reaction time.
Disclosure of Invention
The invention aims to provide flower-shaped Co3O4A preparation method of a micro-sodium structure.
The invention is realized by the following technical scheme:
flower-shaped Co3O4The preparation method of the micro-sodium structure comprises the following steps: dissolving 5-7 parts of polyvinylpyrrolidone in 45-55 parts of water, adding 8-14 parts of cobalt acetate tetrahydrate, continuously stirring for dissolving, finally adding 15-25 parts of diethylene glycol, uniformly mixing, transferring the reaction solution to a microwave reaction kettle with a polytetrafluoroethylene lining, sealing, heating to 185-195 ℃ in a microwave digestion instrument for reaction for 1.5-2.5h, stopping the reaction, cooling the reaction product to room temperature, centrifugally separating the obtained precipitate, washing with deionized water and ethanol for 4-6 times, and drying at 60-70 ℃ to obtain a precursor; transferring the precursor into a crucible, placing the crucible into a muffle furnace, heating to 480-490 ℃ at the heating rate of 2 ℃/min, calcining for 2-3h, and cooling to obtain the catalyst; the raw materials are in parts by weight.
Preferably, in the preparation method, the reaction is carried out for 2 hours by heating to 190 ℃ in a microwave digestion instrument.
Preferably, in the preparation method, the drying is carried out at 65 ℃.
Preferably, in the preparation method, the temperature is increased to 485 ℃ at the temperature increase rate of 2 ℃/min, and the calcination is carried out for 2.5 h.
The invention has the technical effects that:
the method is simple, convenient, quick and easy to operate, and the flower-shaped Co is successfully prepared3O4Micro-sodium structure, good performance and large-scale preparation.
Detailed Description
The following describes the substance of the present invention with reference to the examples.
Example 1
Flower-shaped Co3O4Preparation of micro-sodium structureThe preparation method comprises the following steps: dissolving 6 parts of polyvinylpyrrolidone in 50 parts of water, adding 11 parts of cobalt acetate tetrahydrate, continuously stirring for dissolving, finally adding 20 parts of diethylene glycol, uniformly mixing, transferring the reaction solution into a microwave reaction kettle with a polytetrafluoroethylene lining, sealing, heating in a microwave digestion instrument to 190 ℃ for reaction for 2 hours, stopping the reaction, cooling a reaction product to room temperature, centrifugally separating the obtained precipitate, washing with deionized water and ethanol for 5 times, and drying at 65 ℃ to obtain a precursor; transferring the precursor into a crucible, placing the crucible in a muffle furnace, heating to 485 ℃ at the heating rate of 2 ℃/min, calcining for 2.5h, and cooling to obtain the catalyst; the raw materials are in parts by weight.
Example 2
Flower-shaped Co3O4The preparation method of the micro-sodium structure comprises the following steps: dissolving 5 parts of polyvinylpyrrolidone in 45 parts of water, adding 8 parts of cobalt acetate tetrahydrate, continuously stirring for dissolving, finally adding 15 parts of diethylene glycol, uniformly mixing, transferring the reaction solution into a microwave reaction kettle with a polytetrafluoroethylene lining, sealing, heating to 185 ℃ in a microwave digestion instrument for reaction for 1.5 hours, stopping the reaction, cooling a reaction product to room temperature, centrifugally separating the obtained precipitate, washing for 4 times by using deionized water and ethanol, and drying at 60 ℃ to obtain a precursor; transferring the precursor into a crucible, placing the crucible into a muffle furnace, heating to 480 ℃ at the heating rate of 2 ℃/min, calcining for 2h, and cooling to obtain the catalyst; the raw materials are in parts by weight.
Example 3
Flower-shaped Co3O4The preparation method of the micro-sodium structure comprises the following steps: dissolving 7 parts of polyvinylpyrrolidone in 55 parts of water, adding 14 parts of cobalt acetate tetrahydrate, continuously stirring for dissolving, finally adding 25 parts of diethylene glycol, uniformly mixing, transferring the reaction solution into a microwave reaction kettle with a polytetrafluoroethylene lining, sealing, heating in a microwave digestion instrument to 195 ℃ for reaction for 2.5 hours, stopping the reaction, cooling a reaction product to room temperature, centrifugally separating the obtained precipitate, washing with deionized water and ethanol for 6 times, and drying at 70 ℃ to obtain a precursor; transferring the precursor into a crucible, and placing the crucible in a muffle furnaceHeating to 490 ℃ at the heating rate of 2 ℃/min, calcining for 3h, and cooling to obtain the catalyst; the raw materials are in parts by weight.
The method is simple, convenient, quick and easy to operate, and the flower-shaped Co is successfully prepared3O4Micro-sodium structure, good performance and large-scale preparation.
Claims (4)
1. Flower-shaped Co3O4The preparation method of the micro-sodium structure is characterized by comprising the following steps: dissolving 5-7 parts of polyvinylpyrrolidone in 45-55 parts of water, adding 8-14 parts of cobalt acetate tetrahydrate, continuously stirring for dissolving, finally adding 15-25 parts of diethylene glycol, uniformly mixing, transferring the reaction solution to a microwave reaction kettle with a polytetrafluoroethylene lining, sealing, heating to 185-195 ℃ in a microwave digestion instrument for reaction for 1.5-2.5h, stopping the reaction, cooling the reaction product to room temperature, centrifugally separating the obtained precipitate, washing with deionized water and ethanol for 4-6 times, and drying at 60-70 ℃ to obtain a precursor; transferring the precursor into a crucible, placing the crucible into a muffle furnace, heating to 480-490 ℃ at the heating rate of 2 ℃/min, calcining for 2-3h, and cooling to obtain the catalyst; the raw materials are in parts by weight.
2. The method of claim 1, wherein: heating to 190 ℃ in a microwave digestion instrument and reacting for 2 h.
3. The method of claim 1, wherein: drying at 65 ℃.
4. The method of claim 1, wherein: heating to 485 deg.C at a heating rate of 2 deg.C/min, and calcining for 2.5 h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811232720.5A CN111087027A (en) | 2018-10-23 | 2018-10-23 | Flower-shaped Co3O4Preparation method of micro-sodium structure |
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| CN201811232720.5A CN111087027A (en) | 2018-10-23 | 2018-10-23 | Flower-shaped Co3O4Preparation method of micro-sodium structure |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112960702A (en) * | 2021-04-23 | 2021-06-15 | 华中科技大学 | Preparation method of cobaltosic oxide with thermochemical energy storage performance and product |
| CN114939420A (en) * | 2022-06-27 | 2022-08-26 | 中国科学院赣江创新研究院 | Palladium-based catalyst containing cobalt oxide carrier and preparation method and application thereof |
-
2018
- 2018-10-23 CN CN201811232720.5A patent/CN111087027A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112960702A (en) * | 2021-04-23 | 2021-06-15 | 华中科技大学 | Preparation method of cobaltosic oxide with thermochemical energy storage performance and product |
| CN112960702B (en) * | 2021-04-23 | 2022-02-15 | 华中科技大学 | Preparation method of cobaltosic oxide with thermochemical energy storage performance and product |
| CN114939420A (en) * | 2022-06-27 | 2022-08-26 | 中国科学院赣江创新研究院 | Palladium-based catalyst containing cobalt oxide carrier and preparation method and application thereof |
| CN114939420B (en) * | 2022-06-27 | 2023-10-20 | 中国科学院赣江创新研究院 | Palladium-based catalyst containing cobalt oxide carrier, and preparation method and application thereof |
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