CN104591298B - A kind of ultra-thin Co (CO3)0.5(OH) 0.11H2the preparation method of O nanometer sheet gel-like prod - Google Patents
A kind of ultra-thin Co (CO3)0.5(OH) 0.11H2the preparation method of O nanometer sheet gel-like prod Download PDFInfo
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- CN104591298B CN104591298B CN201510020268.6A CN201510020268A CN104591298B CN 104591298 B CN104591298 B CN 104591298B CN 201510020268 A CN201510020268 A CN 201510020268A CN 104591298 B CN104591298 B CN 104591298B
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Abstract
A kind of ultra-thin Co (CO3)0.5(OH)·0.11H2The preparation method of O nanometer sheet gel-like prod, it is mainly: metallic cobalt and the carbonate of stoichiometrically excess is joined in the pH alkaline solution more than 10, stands more than 10 days at ambient temperature, prepare the supersaturated solution containing cobalt；Supersaturated solution containing cobalt is mixed by the volume ratio more than 1:2 with deionized water, i.e. can get flocky precipitate；Gained flocky precipitate is centrifuged or filters and separate to obtain flocky precipitate, then precipitate is washed, successively with deionized water and ethanol, ethylene glycol or washing with acetone centrifugal or filtration separation, then preserve in organic solvent.Co (CO prepared by the present invention3)0.5(OH)·0.11H2The fine structure of O product is ultrathin nanometer chip architecture, and product purity is high, and thickness is uniform, has the highest surface area.This preparation method technique is simple, mild condition, it is easy to operation, and production prices are low, the cycle is short, is suitable for industrialized great production.
Description
Technical field
The present invention relates to the preparation method of a kind of cobalt-based ultrathin nanometer sheet material.
Background technology
Cobalt/cobalt oxide (such as Co3O4) have a wide range of applications value in battery, catalyst, sensor, electrochromism and Flied emission field, therefore develop advanced in performance, cheap cobalt/cobalt oxide or its presoma is significant.
Co(CO3)0.5(OH)·0.11H2O is one of a kind of important cobalt-based material, can be used as preparing the presoma of various cobalt/cobalt oxide.But the Co (CO reported at present3)0.5(OH)·0.11H2The preparation method of O product exists following not enough: first, preparation method is the most single, and product type is less；Secondly, preparation technology is complex, and preparation cost is higher；Furthermore, prepared Co (CO3)0.5(OH)·0.11H2The particle size of O product is relatively big, and specific surface area is relatively low.Below this product industrialization process what time is limited.
Summary of the invention
It is an object of the invention to provide a kind of preparation technology simple, low cost, products obtained therefrom purity is high, and thickness is uniform, has the ultra-thin Co (CO of very high surface3)0.5(OH)·0.11H2The preparation method of O nanometer sheet gel-like prod.
Technical scheme is specific as follows:
One, raw material
The raw material of the present invention specifically includes that metallic cobalt, carbonate and strong base solution.Wherein, metallic cobalt is the powder body of simple substance, granule or thin film；Carbonate is the carbonate being dissolved in water, such as potassium carbonate, sodium carbonate and lithium carbonate；Strong base solution is potassium hydroxide, sodium hydroxide and Lithium hydrate.
Two, preparation method
1, metallic cobalt and the carbonate of stoichiometrically excess are joined in the pH alkaline solution more than 10, stand more than 10 days at ambient temperature, prepare the supersaturated solution containing cobalt.The preferably metal ion of carbonate is identical with the metal ion of alkaline solution.
2, the supersaturated solution containing cobalt is mixed by the volume ratio more than 1:2 with deionized water, i.e. can get flocky precipitate.
3, centrifugal for gained flocky precipitate or filtration are separated, again this flocky precipitate is washed, separation is washed and be centrifuged or filtered to one or more in priority deionized water and ethanol, ethylene glycol or acetone etc., then preserve in organic solvent, such as one or more in methanol, ethanol, ethylene glycol or acetone and other organic solvent, i.e. obtain ultra-thin Co (CO3)0.5(OH)·0.11H2O nanometer sheet gel-like prod.
The present invention compared with prior art has the advantage that
1, the Co (CO prepared by the present invention3)0.5(OH)·0.11H2The fine structure of O product is ultrathin nanometer chip architecture, and product purity is high, and thickness is uniform, has the highest surface area.
2, this preparation method technique is simple, mild condition, it is easy to operation, and production prices are low, the cycle is short, is suitable for industrialized great production.
Below in conjunction with detailed description of the invention, the invention will be further described.
Accompanying drawing explanation
Fig. 1 is the photo figure in kind of the product that the embodiment of the present invention 1 obtains.
Fig. 2 is the XRD figure of the product that the embodiment of the present invention 1 obtains.
Fig. 3 is the product electron scanning Electronic Speculum figure that the embodiment of the present invention 1 obtains.
Detailed description of the invention
Embodiment 1
First, by 5g metal simple-substance cobalt powder and the K of 10g2CO3Join the 0.1mol/L KOH pH that volume is 1L to be more than in 10 solution, prepare the supersaturated solution containing cobalt by settled process；Then supersaturated solution is uniformly mixed by 1:5 volume ratio with deionized water, thus obtain flocky precipitate；Gained flocky precipitate is centrifuged, and obtain centrifugal precipitate priority deionized water, washing with alcohol for several times after, preserve product with ethanol, i.e. obtain ultra-thin Co (CO3)0.5(OH)·0.11H2O nanometer sheet gel-like prod.The photo figure in kind of this product is as shown in Figure 1.Fig. 2 is the XRD figure of the product that embodiment 1 obtains, with the most general XRD standard card contrast, it is known that prepared product is Co (CO3)0.5(OH)·0.11H2O.Fig. 3 is the product electron scanning Electronic Speculum figure that the embodiment of the present invention 1 obtains, by this figure it will be seen that prepared product is ultra-thin nanometer sheet structure.
Embodiment 2
First, by 5g metal simple-substance cobalt thin film and the Na of 10g2CO3Join 1mol/L NaOH, pH that volume is 1L to be more than in 10 solution, prepare the supersaturated solution containing cobalt by settled process；Then supersaturated solution is uniformly mixed by 1:3 volume ratio with deionized water, thus obtain flocky precipitate；Gained flocky precipitate is centrifuged, and after the precipitate priority deionized water that obtains centrifugal, ethanol, ethylene glycol wash for several times, spent glycol preservation product, i.e. obtain ultra-thin Co (CO3)0.5(OH)·0.11H2O nanometer sheet gel-like prod.
Embodiment 3
First, by 5g metallic cobalt nano-particle and the Li of 5g2CO3Join 1mol/L LiOH, pH that volume is 1L to be more than in 10 solution, prepare the supersaturated solution containing cobalt by settled process；Then supersaturated solution is uniformly mixed by 1:8 volume ratio with deionized water, thus obtain flocky precipitate；Gained flocky precipitate is centrifuged, and obtain centrifugal precipitate priority deionized water, washing with acetone for several times after, preserve product with methanol, i.e. obtain ultra-thin Co (CO3)0.5(OH)·0.11H2O nanometer sheet gel-like prod.
Claims (1)
1. a ultra-thin Co (CO3)0.5(OH)·0.11H2The preparation method of O nanometer sheet gel-like prod, its feature
It is:
1) metallic cobalt and the carbonate of stoichiometrically excess are joined in the pH alkaline solution more than 10,
Stand more than 10 days at ambient temperature, prepare the supersaturated solution containing cobalt；
2) supersaturated solution containing cobalt is mixed by the volume ratio more than 1:2 with deionized water, the most available
Flocky precipitate；
3) centrifugal for gained flocky precipitate or filtration are separated, then this flocky precipitate is washed, successively
Wash and be centrifuged or filter separation by one or more in deionized water, ethanol, ethylene glycol or acetone, so
After be saved in one or more organic solvents in methanol, ethanol, ethylene glycol or acetone, i.e. obtain ultra-thin
Co(CO3)0.5(OH)·0.11H2O nanometer sheet gel-like prod.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510020268.6A CN104591298B (en) | 2015-01-15 | 2015-01-15 | A kind of ultra-thin Co (CO3)0.5(OH) 0.11H2the preparation method of O nanometer sheet gel-like prod |
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| CN201510020268.6A CN104591298B (en) | 2015-01-15 | 2015-01-15 | A kind of ultra-thin Co (CO3)0.5(OH) 0.11H2the preparation method of O nanometer sheet gel-like prod |
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| CN104591298A CN104591298A (en) | 2015-05-06 |
| CN104591298B true CN104591298B (en) | 2016-10-05 |
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| CN201510020268.6A Expired - Fee Related CN104591298B (en) | 2015-01-15 | 2015-01-15 | A kind of ultra-thin Co (CO3)0.5(OH) 0.11H2the preparation method of O nanometer sheet gel-like prod |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW412505B (en) * | 1995-05-26 | 2000-11-21 | Starck H C Gmbh Co Kg | Process for producing spheroidally agglomerated basic cobalt (II) carbonate |
| DE19519328C1 (en) * | 1995-05-26 | 1997-01-23 | Starck H C Gmbh Co Kg | Process for the preparation of basic cobalt (II) carbonates, the cobalt (II) carbonates produced by the process and their use |
| CN1189402C (en) * | 2003-07-08 | 2005-02-16 | 中信国安盟固利电源技术有限公司 | High-purity spherical cobalto-cobaltic oxide, and its preparing method and use |
| CN1302999C (en) * | 2004-06-03 | 2007-03-07 | 曾福兴 | Method for manufacturing high-density cobaltosic oxide |
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