CN103922425A - Preparation method of porous cobaltosic oxide nanobelt - Google Patents
Preparation method of porous cobaltosic oxide nanobelt Download PDFInfo
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- CN103922425A CN103922425A CN201410133891.8A CN201410133891A CN103922425A CN 103922425 A CN103922425 A CN 103922425A CN 201410133891 A CN201410133891 A CN 201410133891A CN 103922425 A CN103922425 A CN 103922425A
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Abstract
The invention belongs to the technical field of synthesis of inorganic nano materials and discloses a preparation method of a porous cobaltosic oxide nanobelt. The preparation method of the porous cobaltosic oxide nanobelt comprises the following steps: (1) firstly dissolving cobalt salt and a precipitator into water, so that a mixed solution is formed; (2) placing the mixed solution into a hydrothermal kettle, carrying out a hydrothermal reaction for 5-24 hours at the temperature of 100-250 DEG C; (3) after the hydrothermal reaction is finished, separating and washing reaction products, and then roasting the reaction products at the temperature of 350-800 DEG C, so that the porous cobaltosic oxide nanobelt is obtained. According to the preparation method of the porous cobaltosic oxide nanobelt, no surfactant or organic solvent is adopted in a synthetic process, and a new synthetic method is provided for a multilevel structure copper oxide material; a preparation technology is simple, the whole technological process is carried out in a reaction kettle, no complex equipment is needed, and the preparation method of the porous cobaltosic oxide nanobelt is simple, efficient, low in cost, environmentally friendly and easy for large-scale synthesis.
Description
Technical field
The present invention relates to inorganic nano material synthesis technical field, relate in particular to a kind of preparation method of porous cobaltosic oxide nano band.
Background technology
As a class p-type transition metal oxide, tricobalt tetroxide shows peculiar physics and chemistry performance in fields such as electricity, magnetic, air-sensitive, catalysis, is widely used in the key areas such as lithium ion battery electrode material, magneticsubstance, heterogeneous catalyst.The physics and chemistry performance of tricobalt tetroxide is subject to pattern, size and structure influence.In recent years, the tricobalt tetroxide material with different-shape structure causes people's very big interest, has synthesized cobaltosic oxide nano line, nanometer rod, nanometer sheet, nanotube, nano belt, nano flower, nanometer ball etc.Wherein, nano belt is high surface-area and volume ratio with its unique constitutional features, causes it to have higher active sites, is conducive to improve gas-solid phase reaction speed.Therefore, cobaltosic oxide nano band has higher application prospect in gas sensitive element device material and heterogeneous catalyst field, becomes the study hotspot of tricobalt tetroxide material.At present, tricobalt tetroxide strip material is mainly to adopt organic solvent and water to carry out solvent thermal reaction as mixed solvent to synthesize banded cobalt precursor, then carries out roasting and finally obtains cobaltosic oxide nano band.The people such as Tian are dissolved in neutralized verdigris in the mixed solvent of propylene glycol and water (volume ratio 1:1) and carry out solvent thermal reaction, then carry out roasting and obtained cobaltosic oxide nano band (Tian, H.Zou after reaction finishes, J.Fu, X.Yang, Y.Wang, H.Guo, X.Fu, C.Liang, M.Wu, P.K.ShenandQ.Gao, Adv.Funct.Mater., 2010,20,617.).Cobalt chloride is dissolved in N by the people such as Sasaki, in the mixed solvent of dinethylformamide and water (volume ratio 1:1), carry out solvent thermal reaction using palmityl trimethyl ammonium chloride as tensio-active agent, then carry out roasting and obtained cobaltosic oxide nano band (J.Yang, H.Hyodo, K.Kimura and T.Sasaki, Nanotechnology, 2010,21,045605).From above-mentioned document, can find out, the solvent adopting in cobaltosic oxide nano band building-up process all contains a large amount of organic solvents, has used in addition tensio-active agent, and its disadvantage is that synthetic cost is high, is not easy to large-scale production.Therefore the research that, carry out low cost, is easy to the synthetic cobaltosic oxide nano band its preparation method of mass-producing has important scientific meaning and using value.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide organic solvent-free and tensio-active agent in a kind of building-up reactions and be easy to the preparation method of synthetic four oxidation three nano belt of mass-producing.
The present invention adopts following technical scheme:
The preparation method's of porous cobaltosic oxide nano band of the present invention concrete steps are as follows:
(1) first by soluble in water to cobalt salt and precipitation agent, form mixing solutions, the mol ratio of cobalt salt and precipitation agent is 1:1～1:10;
(2) then mixing solutions is put in water heating kettle, carried out hydro-thermal reaction at 100～250 DEG C, the reaction times is 5～24h;
(3) after hydro-thermal reaction finishes, reaction product is separated, washed, then reaction product roasting 1～10h at 350～800 DEG C is obtained to porous cobaltosic oxide nano band.
In step (1), described cobalt salt is Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, and precipitation agent is Dyhard RU 100, and the concentration of described cobalt salt is 5～200mmol/l; The concentration of preferred described cobalt salt is 10～150mmol/l; More preferably the concentration of described cobalt salt is 30～100mmol/l.
In step (1), the mol ratio of described cobalt salt and precipitation agent is preferably 1:1～1:7, more preferably 1:3～1:5.
In step (2), preferably at 130～200 DEG C, carry out hydro-thermal reaction, the reaction times is 8～20h; More preferably at 160～190 DEG C, carry out hydro-thermal reaction, the reaction times is 10～15h.
In step (3), preferably 400～700 DEG C of maturing temperatures; Be more preferably 450～600 DEG C.
In step (3), roasting time is 1～10h
Positively effect of the present invention is as follows:
1) the present invention has realized surfactant-free in building-up process, organic solvent-free, provides a new synthetic method for having multilevel hierarchy copper oxide material.
2) the present invention is by regulating mol ratio, hydrothermal temperature and the time of cobalt salt concentration, cobalt salt and precipitation agent to regulate and control the pattern of tricobalt tetroxide, and control condition and means are easy to implement.
3) preparation technology of the present invention is succinct, and whole technological process is carried out in reactor, without any complex apparatus, is a kind of simple and effective, cheap, environmental friendliness, is easy to the synthetic preparation method who prepares cobaltosic oxide nano band of mass-producing.
Brief description of the drawings
Fig. 1 is the XRD spectra of the cobaltosic oxide nano band that obtains of embodiment 1;
Fig. 2 is the SEM figure of the cobaltosic oxide nano band that obtains of embodiment 1;
Fig. 3 is the TEM figure of the cobaltosic oxide nano band that obtains of embodiment 1;
Fig. 4 is nitrogen adsorption/desorption isotherm figure of the cobaltosic oxide nano band that obtains of embodiment 1;
Fig. 5 is the graph of pore diameter distribution of the cobaltosic oxide nano band that obtains of embodiment 1.
Embodiment
The following examples are to describe in further detail of the present invention.
Embodiment 1
(1) first by soluble in water to Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and Dyhard RU 100, form mixing solutions, the concentration of Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is 50mmol/l, the mol ratio of Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and Dyhard RU 100 is 1:4;
(2) then mixing solutions is put in water heating kettle, carried out hydro-thermal reaction at 180 DEG C, the reaction times is 12h;
(3) after hydro-thermal reaction finishes, reaction product is separated, washed, then reaction product roasting 2h at 500 DEG C is obtained to porous cobaltosic oxide nano band.
On the X ' PertPROMPD type Multi-functional X ray diffractometer that the black powder product of above-mentioned preparation is produced in Dutch Panalytical company (PANalytical), carry out XRD test.Fig. 1 is the XRD spectra of the black powder product that obtains of embodiment 1, and the diffraction peak in spectrogram is typical spinel structure tricobalt tetroxide characteristic diffraction peak, and according to standard powdery diffractometry card (JCPDSNo.42-1467), its crystalline structure is isometric system.XRD spectra confirms that gained black product is tricobalt tetroxide.
The JSM-7001F model field emission scanning electron microscope observation surface topography that the black tricobalt tetroxide of above-mentioned preparation is produced in NEC company.Fig. 2 is the SEM figure of the black tricobalt tetroxide that obtains of embodiment 1, and tricobalt tetroxide pattern is banded as seen from the figure, and its width is at 100nm～300nm, and has vesicular structure on nano belt surface.
The JEM-2100 lanthanum hexaborane transmission electron microscopy observation particle information that the black tricobalt tetroxide of above-mentioned preparation is produced in NEC company.Fig. 3 is the TEM figure of the black tricobalt tetroxide that obtains of embodiment 1, and black cobaltosic oxide nano band size is about 200nm as seen from the figure, is formed, and formed the vesicular structure of the about 30nm in aperture by the nanoparticle assembling that is of a size of 50nm～100nm.
The specific surface of the NOVA3200e model that the black tricobalt tetroxide of above-mentioned preparation is produced in Kang Ta company of the U.S. and lacunarity analysis instrument test specific surface and pore size distribution.Figure 4 and 5 are respectively nitrogen adsorption/desorption isotherm figure and the graph of pore diameter distribution of the black tricobalt tetroxide that embodiment 1 obtains.Hysteresis loop shows that at the IV type thermoisopleth at relative dividing potential drop approximately 0.8～1.0 place cobaltosic oxide nano band has the secondary meso-hole structure that particle packing forms, and BET specific surface is 31.6m
2/ g, can and aperture be 28.6nm.
Embodiment 2
(1) first by soluble in water to Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and Dyhard RU 100, form mixing solutions, the concentration of Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is 10mmol/l, the mol ratio of Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and Dyhard RU 100 is 1:1;
(2) then mixing solutions is put in water heating kettle, carried out hydro-thermal reaction at 130 DEG C, the reaction times is 20h;
(3) after hydro-thermal reaction finishes, reaction product is separated, washed, then reaction product roasting 10h at 400 DEG C is obtained to porous cobaltosic oxide nano band.
XRD spectra assay products is isometric system tricobalt tetroxide.SEM photo shows that tricobalt tetroxide pattern presents porous zonal structure, its width 150nm～200nm.TEM photo shows that cobaltosic oxide nano band size is about 200nm, is formed by the nanoparticle assembling that is of a size of 30nm～50nm, and aperture is about 25nm.It is 37.9m that nitrogen adsorption instrument is measured specific surface
2/ g, can and aperture be about 24.3nm.
Embodiment 3
(1) first by soluble in water to Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and Dyhard RU 100, form mixing solutions, the concentration of Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is 150mmol/l, the mol ratio of Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and Dyhard RU 100 is 1:7;
(2) then mixing solutions is put in water heating kettle, carried out hydro-thermal reaction at 200 DEG C, the reaction times is 8h;
(3) after hydro-thermal reaction finishes, reaction product is separated, washed, then reaction product roasting 1h at 700 DEG C is obtained to porous cobaltosic oxide nano band.
XRD spectra assay products is isometric system tricobalt tetroxide.SEM photo shows that tricobalt tetroxide pattern presents porous zonal structure, its width 100nm～500nm.TEM photo shows that cobaltosic oxide nano band size is about 250nm, is formed by the nanoparticle assembling that is of a size of 40nm～60nm, and aperture is about 25nm.It is 33.1m that nitrogen adsorption instrument is measured specific surface
2/ g, can and aperture be about 25.7nm.
Embodiment 4
(1) first by soluble in water to Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and Dyhard RU 100, form mixing solutions, the concentration of Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is 100mmol/l, the mol ratio of Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and Dyhard RU 100 is 1:3;
(2) then mixing solutions is put in water heating kettle, carried out hydro-thermal reaction at 190 DEG C, the reaction times is 10h;
(3) after hydro-thermal reaction finishes, reaction product is separated, washed, then reaction product roasting 3h at 600 DEG C is obtained to porous cobaltosic oxide nano band.
XRD spectra assay products is isometric system tricobalt tetroxide.SEM photo shows that tricobalt tetroxide pattern presents porous zonal structure, its width 100nm～500nm.TEM photo shows that cobaltosic oxide nano band size is about 310nm, is formed by the nanoparticle assembling that is of a size of 50nm～60nm, and aperture is about 28nm.It is 30.2m that nitrogen adsorption instrument is measured specific surface
2/ g, can and aperture be about 27.5nm.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, amendment, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (10)
1. a preparation method for porous cobaltosic oxide nano band, is characterized in that: the concrete steps of described method are as follows:
(1) first by soluble in water to cobalt salt and precipitation agent, form mixing solutions, the mol ratio of cobalt salt and precipitation agent is 1:1～1:10;
(2) then mixing solutions is put in water heating kettle, carried out hydro-thermal reaction at 100～250 DEG C, the reaction times is 5～24h;
(3) after hydro-thermal reaction finishes, reaction product is separated, washed, then reaction product roasting 1～10h at 350～800 DEG C is obtained to porous cobaltosic oxide nano band.
2. preparation method as claimed in claim 1, is characterized in that: in step (1), described cobalt salt is Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, and precipitation agent is Dyhard RU 100, and the concentration of described cobalt salt is 5～200mmol/l.
3. preparation method as claimed in claim 2, is characterized in that: the concentration of described cobalt salt is 10～150mmol/l.
4. preparation method as claimed in claim 2, is characterized in that: the concentration of described cobalt salt is 30～100mmol/l.
5. preparation method as claimed in claim 1, is characterized in that: in step (1), the mol ratio of described cobalt salt and precipitation agent is 1:1～1:7.
6. preparation method as claimed in claim 1, is characterized in that: in step (1), the mol ratio of described cobalt salt and precipitation agent is 1:3～1:5.
7. preparation method as claimed in claim 1, is characterized in that: in step (2), carry out hydro-thermal reaction at 130～200 DEG C, the reaction times is 8～20h.
8. preparation method as claimed in claim 1, is characterized in that: in step (2), carry out hydro-thermal reaction at 160～190 DEG C, the reaction times is 10～15h.
9. preparation method as claimed in claim 1, is characterized in that: in step (3), maturing temperature is 400～700 DEG C.
10. preparation method as claimed in claim 1, is characterized in that: in step (3), maturing temperature is 450～600 DEG C.
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Cited By (11)
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| CN104478006A (en) * | 2015-01-06 | 2015-04-01 | 南京工业大学 | Preparation method of tricobalt tetraoxide mesoporous nanosheets |
| CN104609479A (en) * | 2015-02-11 | 2015-05-13 | 天津理工大学 | Method for preparing Co3O4 nanoribbon |
| WO2016095670A1 (en) * | 2014-12-17 | 2016-06-23 | 江苏合志锂硫电池技术有限公司 | Method for preparing cobaltosic oxide |
| CN105870439A (en) * | 2016-04-22 | 2016-08-17 | 济南大学 | Preparation method and application of porous Co3O4 |
| CN108046341A (en) * | 2018-01-11 | 2018-05-18 | 燕山大学 | A kind of preparation method of hollow coralliform cobaltosic oxide nanoparticles |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2016095670A1 (en) * | 2014-12-17 | 2016-06-23 | 江苏合志锂硫电池技术有限公司 | Method for preparing cobaltosic oxide |
| CN104478006A (en) * | 2015-01-06 | 2015-04-01 | 南京工业大学 | Preparation method of tricobalt tetraoxide mesoporous nanosheets |
| CN104609479A (en) * | 2015-02-11 | 2015-05-13 | 天津理工大学 | Method for preparing Co3O4 nanoribbon |
| CN105870439A (en) * | 2016-04-22 | 2016-08-17 | 济南大学 | Preparation method and application of porous Co3O4 |
| CN105870439B (en) * | 2016-04-22 | 2018-03-16 | 济南大学 | A kind of preparation method and applications of porous cobaltosic oxide |
| CN108046341B (en) * | 2018-01-11 | 2019-09-10 | 燕山大学 | A kind of preparation method of hollow coralliform cobaltosic oxide nanoparticles |
| CN108046341A (en) * | 2018-01-11 | 2018-05-18 | 燕山大学 | A kind of preparation method of hollow coralliform cobaltosic oxide nanoparticles |
| CN108611659A (en) * | 2018-05-03 | 2018-10-02 | 山东大学 | A kind of Co of efficient stable3O4Nano-band array analyses chloride electrode |
| CN108611659B (en) * | 2018-05-03 | 2019-12-17 | 山东大学 | High-efficiency stable Co3O4Nanoribbon array chlorine evolution electrode |
| CN108918603A (en) * | 2018-07-11 | 2018-11-30 | 山东大学 | A kind of g-C of porous zinc bloom nanometer sheet carrying transition metal doping3N4The synthetic method of composite air-sensitive material |
| CN110479274A (en) * | 2018-11-05 | 2019-11-22 | 吉林大学 | It is a kind of by aluminium powder be sacrifice agent Co3O4-CuCoO2The preparation method of nanometer net materials |
| CN110479274B (en) * | 2018-11-05 | 2021-06-22 | 吉林大学 | Co taking aluminum powder as sacrificial agent3O4-CuCoO2Preparation method of nano net material |
| CN110357171A (en) * | 2019-05-07 | 2019-10-22 | 淮阴师范学院 | A kind of preparation method of band-like porous cobaltosic oxide |
| CN110357171B (en) * | 2019-05-07 | 2021-11-02 | 淮阴师范学院 | Preparation method of strip-shaped porous cobaltosic oxide |
| CN113600194A (en) * | 2021-07-21 | 2021-11-05 | 西安近代化学研究所 | Nano photocatalyst containing cobalt in different valence states, preparation method and application thereof |
| CN113600194B (en) * | 2021-07-21 | 2023-10-20 | 西安近代化学研究所 | Nanometer photocatalyst containing cobalt with different valence states, preparation method and application thereof |
| CN114887579A (en) * | 2022-05-28 | 2022-08-12 | 昆明理工大学 | Preparation and application of vanadium-based material for adsorbing and recovering organic cationic dye in wastewater |
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