CN104787807A - Solvothermal preparation method of cobaltous oxide nanoparticles - Google Patents
Solvothermal preparation method of cobaltous oxide nanoparticles Download PDFInfo
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- CN104787807A CN104787807A CN201510224938.6A CN201510224938A CN104787807A CN 104787807 A CN104787807 A CN 104787807A CN 201510224938 A CN201510224938 A CN 201510224938A CN 104787807 A CN104787807 A CN 104787807A
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- cobaltous oxide
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Abstract
The invention relates to cobaltous oxide nanoparticles, particularly a solvothermal preparation method of cobaltous oxide nanoparticles, which comprises the following steps: 1) adding a cobalt nitrate solution into a sodium hydroxide solution, and adding a surfactant to obtain a mixed solution; 2) transferring the mixed solution obtained in the step 1) into a teflon-lined reaction kettle, sealing, putting the reaction kettle into a drying oven, reacting, cooling to room temperature, carrying out centrifugal cleaning, and discarding the supernate to obtain concentrated sol; and 3) drying the concentrated sol obtained in the step 2) to obtain the cobaltous oxide nanoparticle powder; or adding anhydrous ethanol into the concentrated sol obtained in the step 2) to obtain the cobaltous oxide nanoparticle sol, sealing, and carrying out long-term storage at 4 DEG C. The method has the advantages of simple and efficient preparation process, favorable reproducibility, high product purity, favorable crystallinity, low raw material price, low energy consumption, environment friendliness and the like, is easy for industrialized amplification, and is especially suitable for low-cost industrial production of cobaltous oxide.
Description
Technical field
The present invention relates to cobaltous oxide nanoparticle, especially relating to Cobaltous nitrate hexahydrate is cobalt source, by the solvothermal preparation method of a kind of cobaltous oxide nanoparticle of the techniques such as single step solvent-thermal method, eccentric cleaning and vacuum-drying.
Background technology
CoO is a kind of material extremely with application prospect, because of its magnetic property, chemical property and be subject to extensive concern, have the great potential as plate battery material, it all plays an important role in the electronic products such as lithium ion battery, gas sensor, electrochromic device and ultracapacitor.
(the He X M such as He, Shi H G.Synthesis and anomalous magnetic properties ofhexagonal CoO nanoparticles [J], Mater Res Bull, 2011,46 (10): 1692) simple thermal decomposition method is adopted to prepare CoO particle, distribution of sizes is within the scope of 38 ~ 93nm, and experimental data shows that they are pyramid, and has close-packed hexagonal structure.Find after tested, it has unusual magnetic property, is in particular in following several respects: (1), when about 300K, antiferromagnetic transition can disappear; (2) be 1090F/g at the blocking temperature electric capacity lower than 6 ~ 11K, now, scanning speed is 10mV/s.These nano particles as ultracapacitor cathode material test time there is outstanding electrochemical capacitance characteristic and cycle life.
Solvent-thermal process carries out in high-temperature high-pressure reaction kettle and adopts organic solvent as the medium of transmission of pressure and mineralizer, by heating reaction system, produce the environment of a High Temperature High Pressure wherein, thus carry out a kind of effective ways prepared by Inorganic synthese and material.It effectively can stop precursor, the hydrolysis oxidation of product, is conducive to carrying out smoothly of building-up reactions; The new chemical reaction being difficult to carry out under other normal condition can also be realized, various new thing phase, metastable phase, bertholide and multiple elements design nano material can also be obtained; Solvent-thermal process also helps the material generating and have crystal formation perfection, rule orientating, and the product purity of synthesis is higher, by selecting and adjust temperature of reaction, solvent, tensio-active agent etc., can control the shape of nano material, size and structure etc., thus for novel material lay a solid foundation (Lie group. the preparation and application technology [M] of nano material. Beijing: Chemical Industry Press, 2008).Solvent-thermal method is the common method of synthesis cobalt/cobalt oxide nanoparticle.
Summary of the invention
The object of this invention is to provide simple, efficient, the solvothermal preparation method of a kind of cobaltous oxide nanoparticle be produced on a large scale.
The present invention includes following steps:
1) in sodium hydroxide solution, add cobalt nitrate solution, then add tensio-active agent, obtain mixed solution;
2) by step 1) mixed solution that obtains is transferred to is furnished with in teflon-lined reactor and seals, and reactor is put into baking oven and reacts, then be cooled to room temperature, eccentric cleaning, abandon supernatant liquor, obtain dense colloidal sol;
3) by step 2) namely obtain cobaltous oxide nanoparticle powder after the dense colloidal sol drying that obtains; Or
In step 2) add dehydrated alcohol in the dense colloidal sol that obtains, obtain cobaltous oxide nanoparticle sol, standing storage at 4 DEG C after sealing.
In step 1) in, the proportioning of described sodium hydroxide solution, cobalt nitrate solution, tensio-active agent can be 7.5mL: 6mL: (0.03 ~ 0.05) g, wherein, sodium hydroxide solution, cobalt nitrate solution are calculated by volume, and tensio-active agent is calculated in mass; The volumetric molar concentration of described sodium hydroxide solution can be 0.5 ~ 1M, and the volumetric molar concentration of described cobalt nitrate solution can be 0.03 ~ 0.2M; Described sodium hydroxide solution and cobalt nitrate solution can adopt dehydrated alcohol to prepare; Described tensio-active agent can be selected from cetyl trimethylammonium bromide powder or tetradecanoic acid powder etc.
In step 2) in, described polytetrafluoroethyllining lining can adopt 25mL polytetrafluoroethyllining lining; The temperature of described baking oven can be 110 ~ 180 DEG C, and the time of reaction can be 4 ~ 13h; Described eccentric cleaning can use dehydrated alcohol centrifuge washing 3 times, centrifugal 10min under described centrifugal condition can be 8000rpm.
In step 3) in, described drying can adopt vacuum-drying, and vacuum drying condition can be 60 DEG C ,-0.1MPa.
The present invention has prepared the good polycrystalline cobaltous oxide nano particle of crystallinity, and particle diameter is about 20nm.The present invention has that preparation flow is simple efficient, favorable reproducibility, product purity are high, good crystallinity, low in raw material price, energy consumption are low, environmental friendliness and the easy advantage such as industrialization amplification, is particularly suitable for the suitability for industrialized production that low cost prepares cobaltous oxide.
Accompanying drawing explanation
Fig. 1 is the TEM figure of the cobaltous oxide nanoparticle of preparation in embodiment 1.
Fig. 2 is the HRTEM figure of the cobaltous oxide nanoparticle of preparation in embodiment 1.
Fig. 3 is the SEAD figure of the cobaltous oxide nanoparticle of preparation in embodiment 1.
Fig. 4 is the XRD figure of the cobaltous oxide nanoparticle of preparation in embodiment 1.
Fig. 5 is the TEM figure of the cobaltous oxide nanoparticle of preparation in embodiment 2.
Fig. 6 is the TEM figure of the cobaltous oxide nanoparticle of preparation in embodiment 3.
Fig. 7 is the SAED figure of the cobaltous oxide nanoparticle of preparation in embodiment 3.
Embodiment
The invention will be further described below by way of embodiments and drawings.
Embodiment 1:
6mL 0.2M cobalt nitrate solution is slowly dripped under continuous stirring in 7.5mL 0.5M sodium hydroxide solution.Property adds 0.03g cetyl trimethylammonium bromide powder again, continues to stir 15min.Then above-mentioned mixed solution is transferred to and is furnished with in 25mL teflon-lined autoclave (Autoclave) and seals, take out after baking oven reactor being put into 180 DEG C reacts 5h.After air cooling to room temperature, with dehydrated alcohol centrifuge washing three times, then gained is precipitated vacuum-drying obtain product.
In embodiment 1, the TEM figure of the cobaltous oxide nanoparticle of preparation is see Fig. 1, the HRTEM figure of the cobaltous oxide nanoparticle of preparation is see Fig. 2, the SEAD figure of the cobaltous oxide nanoparticle of preparation is see Fig. 3, and the XRD figure of the cobaltous oxide nanoparticle of preparation is see Fig. 4.
Embodiment 2:
6mL 0.03M cobalt nitrate solution is slowly dripped under continuous stirring in 7.5mL 1M sodium hydroxide solution.Property adds 0.05g tetradecanoic acid powder again, continues to stir 15min.Then above-mentioned mixed solution is transferred to and is furnished with in 25mL teflon-lined autoclave (Autoclave) and seals, take out after baking oven reactor being put into 180 DEG C reacts 4h.After air cooling to room temperature, with dehydrated alcohol centrifuge washing three times, then gained is precipitated vacuum-drying obtain product.
In embodiment 2, the TEM figure of the cobaltous oxide nanoparticle of preparation is see Fig. 5.
Embodiment 3:
6mL 0.03M cobalt nitrate solution is slowly dripped under continuous stirring directly in 7.5mL 1M sodium hydroxide solution.Continue to stir 15min.Then above-mentioned mixed solution is transferred to and is furnished with in 25mL teflon-lined autoclave (Autoclave) and seals, take out after baking oven reactor being put into 110 DEG C reacts 13h.After air cooling to room temperature, with dehydrated alcohol centrifuge washing three times, then gained is precipitated vacuum-drying obtain product.
In embodiment 3, the TEM figure of the cobaltous oxide nanoparticle of preparation is see Fig. 6, and the SAED figure of the cobaltous oxide nanoparticle of preparation is see Fig. 7.
The present invention, by technology such as single step solvent-thermal method, eccentric cleaning, vacuum-dryings, prepares cobaltous oxide nanoparticle simply efficiently, and determines its composition, pattern and crystal property by characterization methods such as XRD, TEM, HRTEM, SAED.Cobaltous oxide nanoparticle prepared by the method is particulate state, and particle diameter is about 20nm, and it is simple that the present invention has preparation flow, and favorable reproducibility, the advantages such as product purity is high, good crystallinity, are suitable for suitability for industrialized production.
Claims (8)
1. a solvothermal preparation method for cobaltous oxide nanoparticle, is characterized in that comprising the following steps:
1) in sodium hydroxide solution, add cobalt nitrate solution, then add tensio-active agent, obtain mixed solution;
2) by step 1) mixed solution that obtains is transferred to is furnished with in teflon-lined reactor and seals, and reactor is put into baking oven and reacts, then be cooled to room temperature, eccentric cleaning, abandon supernatant liquor, obtain dense colloidal sol;
3) by step 2) namely obtain cobaltous oxide nanoparticle powder after the dense colloidal sol drying that obtains; Or
In step 2) add dehydrated alcohol in the dense colloidal sol that obtains, obtain cobaltous oxide nanoparticle sol, standing storage at 4 DEG C after sealing.
2. the solvothermal preparation method of a kind of cobaltous oxide nanoparticle as claimed in claim 1, it is characterized in that in step 1) in, the proportioning of described sodium hydroxide solution, cobalt nitrate solution, tensio-active agent is 7.5mL: 6mL: (0.03 ~ 0.05) g, wherein, sodium hydroxide solution, cobalt nitrate solution are calculated by volume, and tensio-active agent is calculated in mass; The volumetric molar concentration of described sodium hydroxide solution is 0.5 ~ 1M, and the volumetric molar concentration of described cobalt nitrate solution is 0.03 ~ 0.2M.
3. the solvothermal preparation method of a kind of cobaltous oxide nanoparticle as claimed in claim 1, is characterized in that in step 1) in, described sodium hydroxide solution and cobalt nitrate solution all adopt dehydrated alcohol to prepare.
4. the solvothermal preparation method of a kind of cobaltous oxide nanoparticle as claimed in claim 1, is characterized in that in step 1) in, described tensio-active agent is selected from cetyl trimethylammonium bromide powder or tetradecanoic acid powder.
5. the solvothermal preparation method of a kind of cobaltous oxide nanoparticle as claimed in claim 1, is characterized in that in step 2) in, described polytetrafluoroethyllining lining adopts 25mL polytetrafluoroethyllining lining.
6. the solvothermal preparation method of a kind of cobaltous oxide nanoparticle as claimed in claim 1, is characterized in that in step 2) in, the temperature of described baking oven is 110 ~ 180 DEG C, and the time of reaction is 4 ~ 13h.
7. the solvothermal preparation method of a kind of cobaltous oxide nanoparticle as claimed in claim 1, is characterized in that in step 2) in, described eccentric cleaning is that described centrifugal condition is centrifugal 10min under 8000rpm with dehydrated alcohol centrifuge washing 3 times.
8. the solvothermal preparation method of a kind of cobaltous oxide nanoparticle as claimed in claim 1, is characterized in that in step 3) in, described drying adopts vacuum-drying, and vacuum drying condition is 60 DEG C ,-0.1MPa.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110305249A (en) * | 2019-07-12 | 2019-10-08 | 广西民族大学 | A kind of preparation method of the abietyl thermal polymerization corrosion prevention film of the cobalt protoxide nanoparticle doped of high pitting potential |
| CN110305571A (en) * | 2019-07-12 | 2019-10-08 | 广西民族大学 | A kind of preparation method of high performance alkyd resin corrosive enamel |
| CN114380338A (en) * | 2022-01-25 | 2022-04-22 | 重庆邮电大学 | Preparation method of magnetic cobalt oxide mesoporous nanospheres, products and applications thereof |
| CN114804221A (en) * | 2022-04-28 | 2022-07-29 | 荆门市格林美新材料有限公司 | Cobaltous oxide and preparation method and application thereof |
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| CN101800302A (en) * | 2010-04-15 | 2010-08-11 | 上海交通大学 | Graphene nanometer sheet-cobaltous oxide composite negative electrode material of lithium ion battery and preparation method thereof |
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| CN103771540A (en) * | 2013-12-26 | 2014-05-07 | 青岛永通电梯工程有限公司 | Cobaltous oxide material preparation method |
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| CN1891635A (en) * | 2005-07-08 | 2007-01-10 | 中南大学 | Method for preparing nano cobaltous oxide |
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| CN101800302A (en) * | 2010-04-15 | 2010-08-11 | 上海交通大学 | Graphene nanometer sheet-cobaltous oxide composite negative electrode material of lithium ion battery and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110305249A (en) * | 2019-07-12 | 2019-10-08 | 广西民族大学 | A kind of preparation method of the abietyl thermal polymerization corrosion prevention film of the cobalt protoxide nanoparticle doped of high pitting potential |
| CN110305571A (en) * | 2019-07-12 | 2019-10-08 | 广西民族大学 | A kind of preparation method of high performance alkyd resin corrosive enamel |
| CN110305571B (en) * | 2019-07-12 | 2023-03-07 | 广西民族大学 | Preparation method of high-performance alkyd resin anticorrosive enamel |
| CN114380338A (en) * | 2022-01-25 | 2022-04-22 | 重庆邮电大学 | Preparation method of magnetic cobalt oxide mesoporous nanospheres, products and applications thereof |
| CN114380338B (en) * | 2022-01-25 | 2023-11-03 | 重庆邮电大学 | Preparation method of magnetic cobalt oxide mesoporous nanospheres, product and application thereof |
| CN114804221A (en) * | 2022-04-28 | 2022-07-29 | 荆门市格林美新材料有限公司 | Cobaltous oxide and preparation method and application thereof |
| CN114804221B (en) * | 2022-04-28 | 2023-11-03 | 荆门市格林美新材料有限公司 | Cobalt oxide and preparation method and application thereof |
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