CN104591298A - Preparation method of ultra-thin Co(CO3)0.5(OH).0.11H2O nano film adhesive product - Google Patents
Preparation method of ultra-thin Co(CO3)0.5(OH).0.11H2O nano film adhesive product Download PDFInfo
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- CN104591298A CN104591298A CN201510020268.6A CN201510020268A CN104591298A CN 104591298 A CN104591298 A CN 104591298A CN 201510020268 A CN201510020268 A CN 201510020268A CN 104591298 A CN104591298 A CN 104591298A
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Abstract
The invention discloses a preparation method of an ultra-thin Co(CO3)0.5(OH).0.11H2O nano film adhesive product. The method mainly comprises the following steps: adding excessive metal cobalt and carbonate to an alkaline solution of which the pH is greater than 10 at the stoichiometric ratio; and standing at a room temperature for over 10 days to prepare a supersaturated solution containing cobalt; mixing the supersaturated solution containing cobalt with deionized water at the volume ratio which is greater than 1 to 2, so as to obtain flocculent sediment; centrifuging or filtering and separating the obtained flocculent sediment to obtain the flocculent sediment and then washing the sediment; and firstly, washing and centrifuging or filtering and separating by using deionized water, ethyl alcohol, ethylene glycol or acetone, and then storing in an organic solvent. A fine structure of a Co(CO3)0.5(OH).0.11H2O product prepared by the method is an ultra-thin nanosheet structure; the product is high in purity, uniform in thickness, and high in superficial area; the preparation method is simple in process, mild in condition, easy to operate, low in production price, short in cycle, and suitable for industrial massive production.
Description
Technical field
The present invention relates to a kind of preparation method of cobalt-based ultrathin nanometer sheet material.
Background technology
Cobalt/cobalt oxide (such as Co
3o
4) have a wide range of applications in battery, catalyzer, sensor, electrochromism and Flied emission field value, therefore develops advanced in performance, cheap cobalt/cobalt oxide or its presoma is significant.
Co (CO
3)
0.5(OH) 0.11H
2o is one of a kind of important cobalt-based material, can be used as the presoma preparing various cobalt/cobalt oxide.But current reported Co (CO
3)
0.5(OH) 0.11H
2there is following deficiency in the preparation method of O product: first, and preparation method is comparatively single, and product type is less; Secondly, preparation technology is comparatively complicated, and preparation cost is higher; Moreover, prepared Co (CO
3)
0.5(OH) 0.11H
2the particle size of O product is comparatively large, and specific surface area is lower.Below this product industrialization process what time is limited.
Summary of the invention
The object of the present invention is to provide a kind of preparation technology simple, cost is low, and products obtained therefrom purity is high, and thickness is even, has the ultra-thin Co (CO of very high surface area
3)
0.5(OH) 0.11H
2the preparation method of O nanometer sheet gel-like prod.
Technical scheme of the present invention is specific as follows:
One, raw material
Raw material of the present invention mainly comprises: cobalt metal, carbonate and strong base solution.Wherein, cobalt metal is the powder of simple substance, particle or film; Carbonate is water-soluble carbonate, as salt of wormwood, and sodium carbonate and Quilonum Retard; Strong base solution is potassium hydroxide, sodium hydroxide and lithium hydroxide.
Two, preparation method
1, stoichiometrically excessive cobalt metal and carbonate being joined pH is greater than in the basic solution of 10, leaves standstill more than 10 days at ambient temperature, prepares the supersaturated solution containing cobalt.The metal ion of best carbonate is identical with the metal ion of basic solution.
2, the supersaturated solution containing cobalt is mixed by the volume ratio being greater than 1:2 with deionized water, can flocculent precipitate be obtained.
3, by centrifugal for gained flocculent precipitate or filtering separation, again this flocculent precipitate is washed, one or more in priority deionized water and ethanol, ethylene glycol or acetone etc. wash and centrifugal or filtering separation, then preserve in organic solvent, as one or more in methyl alcohol, ethanol, ethylene glycol or acetone and other organic solvent, namely obtain ultra-thin Co (CO
3)
0.5(OH) 0.11H
2o nanometer sheet gel-like prod.
The present invention compared with prior art tool has the following advantages:
1, the Co (CO prepared by the present invention
3)
0.5(OH) 0.11H
2the fine structure of O product is ultrathin nanometer chip architecture, and product purity is high, and thickness is even, has very high surface-area.
2, this preparation method's technique is simple, mild condition, easy handling, and production prices are low, the cycle is short, is applicable to industrialized production.
Below in conjunction with embodiment, 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 electronic scanning Electronic Speculum figure that the embodiment of the present invention 1 obtains.
Embodiment
Embodiment 1
First, by the K of 5g metal simple-substance cobalt powder and 10g
2cO
3joining volume is that the 0.1mol/LKOH pH of 1L is greater than in 10 solution, prepares the supersaturated solution containing cobalt by settled process; Then supersaturated solution and deionized water are pressed 1:5 volume ratio Homogeneous phase mixing, thus obtain flocculent precipitate; Gained flocculent precipitate is carried out centrifugal, and the throw out priority deionized water obtained centrifugal, washing with alcohol for several times after, preserve product with ethanol, namely obtain ultra-thin Co (CO
3)
0.5(OH) 0.11H
2o nanometer sheet gel-like prod.The photo figure in kind of this product as shown in Figure 1.Fig. 2 is the XRD figure of the product that embodiment 1 obtains, and contrasts with XRD standard card general in the world, and known prepared product is Co (CO
3)
0.5(OH) 0.11H
2o.Fig. 3 is the product electronic scanning Electronic Speculum figure that the embodiment of the present invention 1 obtains, and can be seen by this figure, and prepared product is ultra-thin nanometer sheet structure.
Embodiment 2
First, by the Na of 5g metal simple-substance cobalt thin film and 10g
2cO
3joining volume is that 1mol/LNaOH, pH of 1L is greater than in 10 solution, prepares the supersaturated solution containing cobalt by settled process; Then supersaturated solution and deionized water are pressed 1:3 volume ratio Homogeneous phase mixing, thus obtain flocculent precipitate; Gained flocculent precipitate is carried out centrifugal, and after the washing for several times of the throw out priority deionized water obtained centrifugal, ethanol, ethylene glycol, spent glycol preserve product, namely obtains ultra-thin Co (CO
3)
0.5(OH) 0.11H
2o nanometer sheet gel-like prod.
Embodiment 3
First, by the Li of 5g cobalt metal nano particle and 5g
2cO
3joining volume is that 1mol/LLiOH, pH of 1L is greater than in 10 solution, prepares the supersaturated solution containing cobalt by settled process; Then supersaturated solution and deionized water are pressed 1:8 volume ratio Homogeneous phase mixing, thus obtain flocculent precipitate; Gained flocculent precipitate is carried out centrifugal, and the throw out priority deionized water obtained centrifugal, washing with acetone for several times after, preserve product with methyl alcohol, namely obtain ultra-thin Co (CO
3)
0.5(OH) 0.11H
2o nanometer sheet gel-like prod.
Claims (1)
1. a ultra-thin Co (CO
3)
0.5(OH) 0.11H
2the preparation method of O nanometer sheet gel-like prod, is characterized in that:
1) stoichiometrically excessive cobalt metal and carbonate being joined pH is greater than in the basic solution of 10, leaves standstill more than 10 days at ambient temperature, prepares the supersaturated solution containing cobalt;
2) supersaturated solution containing cobalt is mixed by the volume ratio being greater than 1:2 with deionized water, can flocculent precipitate be obtained;
3) by centrifugal for gained flocculent precipitate or filtering separation, again this flocculent precipitate is washed, one or more in priority deionized water and ethanol, ethylene glycol or acetone etc. wash and centrifugal or filtering separation, then preserve in organic solvent, as one or more in methyl alcohol, ethanol, ethylene glycol or acetone and other organic solvent, namely obtain ultra-thin Co (CO
3)
0.5(OH) 0.11H
2o 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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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 true CN104591298A (en) | 2015-05-06 |
CN104591298B CN104591298B (en) | 2016-10-05 |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1185143A (en) * | 1995-05-26 | 1998-06-17 | H·C·施塔克公司 | Basic cobaltous carbonates, prodn. method and use thereof |
CN1190947A (en) * | 1995-05-26 | 1998-08-19 | H·C·施塔克公司 | Spheroidally agglomerated basic cobalt (II) carbonate and spheroidally agglomerated cobalt (II) hydroxide, process for their production and their use |
CN1470460A (en) * | 2003-07-08 | 2004-01-28 | 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 |
CN1583576A (en) * | 2004-06-03 | 2005-02-23 | 曾福兴 | Method for manufacturing high-density cobaltosic oxide |
-
2015
- 2015-01-15 CN CN201510020268.6A patent/CN104591298B/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1185143A (en) * | 1995-05-26 | 1998-06-17 | H·C·施塔克公司 | Basic cobaltous carbonates, prodn. method and use thereof |
CN1190947A (en) * | 1995-05-26 | 1998-08-19 | H·C·施塔克公司 | Spheroidally agglomerated basic cobalt (II) carbonate and spheroidally agglomerated cobalt (II) hydroxide, process for their production and their use |
CN1470460A (en) * | 2003-07-08 | 2004-01-28 | 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 |
CN1583576A (en) * | 2004-06-03 | 2005-02-23 | 曾福兴 | Method for manufacturing high-density cobaltosic oxide |
Non-Patent Citations (1)
Title |
---|
YUQIAN FAN ET AL.: ""Ultrathin Nanoflakes Assembled 3D Hierarchical Mesoporous Co3O4 Nanoparticles for High-Rate Pseudocapacitors"", 《PART. PART. SYST. CHARACT.》 * |
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