CN104787807B - A kind of solvothermal preparation method of cobalt protoxide nanoparticle - Google Patents
A kind of solvothermal preparation method of cobalt protoxide nanoparticle Download PDFInfo
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- CN104787807B CN104787807B CN201510224938.6A CN201510224938A CN104787807B CN 104787807 B CN104787807 B CN 104787807B CN 201510224938 A CN201510224938 A CN 201510224938A CN 104787807 B CN104787807 B CN 104787807B
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Abstract
The solvothermal preparation method of a kind of cobalt protoxide nanoparticle, relates to cobalt protoxide nanoparticle.1) in sodium hydroxide solution, add cobalt nitrate solution, add surfactant, obtain mixed liquor；2) by step 1) mixed liquor that obtains is transferred to is furnished with in teflon-lined reactor and seals, and reactor is put in baking oven and react, be cooled to room temperature, eccentric cleaning, abandon supernatant, obtain dense colloidal sol；3) by step 2) the dense colloidal sol that obtains the most i.e. obtains cobalt protoxide nanoparticle powder；Or in step 2) the dense colloidal sol that obtains adds dehydrated alcohol, obtain cobalt protoxide nanoparticle sol, long term storage at 4 DEG C after sealing.The advantages such as preparation flow is simply efficiently, favorable reproducibility, product purity height, good crystallinity, low in raw material price, energy consumption be low, environmental friendliness and easy industrialization amplification, are particularly suitable for low cost and prepare the industrialized production of cobalt protoxide.
Description
Technical field
The present invention relates to cobalt protoxide nanoparticle, especially relate to cabaltous nitrate hexahydrate as cobalt source, by single step solvent thermal
A kind of solvothermal preparation method of the cobalt protoxide nanoparticle of the techniques such as method, eccentric cleaning and vacuum drying.
Background technology
CoO is a kind of material extremely with application prospect, receives significant attention because of its magnetic property, chemical property, has
As the great potential of anode cell material, it is at lithium ion battery, gas sensor, electrochromic device and ultracapacitor
All play an important role Deng in electronic product.
(He X M, the Shi H G.Synthesis and anomalous magnetic properties of such as He
Hexagonal CoO nanoparticles [J], Mater Res Bull, 2011,46 (10): 1692) use simply
Thermal decomposition method is prepared for CoO granule, and distribution of sizes is in the range of 38～93nm, and experimental data shows that they are pyramids
Shape, and there is close-packed hexagonal structure.Finding after tested, it has unusual magnetic property, is in particular in following several respects: (1)
When about 300K, antiferromagnetic transition can disappear；(2) less than 6～the blocking temperature electric capacity of 11K is 1090F/g,
Now, sweep speed is 10mV/s.These nano-particle have prominent super when testing as the cathode material of ultracapacitor
Capacitance characteristic and cycle life.
Solvent-thermal process be carry out in high-temperature high-pressure reaction kettle and use organic solvent as the transmission medium of pressure and mineralizer,
By reaction system is heated, produce the environment of a High Temperature High Pressure wherein, thus carry out prepared by Inorganic synthese and material one
Plant effective ways.It can effectively stop predecessor, being smoothed out of the hydrolysis oxidation of product, beneficially synthetic reaction；Also may be used
With the new chemical reaction that is difficult under other normal condition of realization, moreover it is possible to obtain various new thing phase, metastable phase, no
Daltonide and multiple elements design nano material；Solvent-thermal process also helps generation and has crystal formation perfection, the material of rule orientating
Material, and the product purity of synthesis is higher, by selecting and adjusting reaction temperature, solvent, surfactant etc., can be to nanometer
The shape of material, size and structure etc. are controlled, thus for new material lay a solid foundation (Lie group. the system of nano material
Standby with application technology [M]. Beijing: Chemical Industry Press, 2008).Solvent-thermal method is synthesis cobalt/cobalt oxide nanoparticle
Common method.
Summary of the invention
It is an object of the invention to provide simple, efficient, prepared by the solvent thermal of a kind of cobalt protoxide nanoparticle being produced on a large scale
Method.
The present invention comprises the following steps:
1) in sodium hydroxide solution, add cobalt nitrate solution, add surfactant, obtain mixed liquor；
2) by step 1) mixed liquor that obtains is transferred to is furnished with in teflon-lined reactor and seals, by reactor
Put in baking oven and react, be cooled to room temperature, eccentric cleaning, abandon supernatant, obtain dense colloidal sol；
3) by step 2) the dense colloidal sol that obtains the most i.e. obtains cobalt protoxide nanoparticle powder；Or
In step 2) the dense colloidal sol that obtains adds dehydrated alcohol, obtain cobalt protoxide nanoparticle sol, after sealing
Long term storage at 4 DEG C.
In step 1) in, described sodium hydroxide solution, cobalt nitrate solution, the proportioning of surfactant can be 7.5mL: 6
ML: (0.03～0.05) g, wherein, in terms of volume, surfactant is with matter for sodium hydroxide solution, cobalt nitrate solution
Amount calculates；The molar concentration of described sodium hydroxide solution can be 0.5～1M, and the molar concentration of described cobalt nitrate solution can be
0.03～0.2M；Described sodium hydroxide solution and cobalt nitrate solution can use dehydrated alcohol to prepare；Described surfactant is optional
From cetyl trimethylammonium bromide powder or myristic acid powder etc..
In step 2) in, described polytetrafluoroethyllining lining can use 25mL polytetrafluoroethyllining lining；The temperature of described baking oven can
Being 110～180 DEG C, the time of reaction can be 4～13h；Described eccentric cleaning can use dehydrated alcohol centrifuge washing 3 times,
Described centrifugal condition can be centrifugal 10min under 8000rpm.
In step 3) in, described being dried can use vacuum drying, and vacuum drying condition can be 60 DEG C ,-0.1MPa.
The present invention is prepared for the polycrystalline cobalt protoxide nano-particle that crystallinity is good, particle diameter about 20nm.The present invention has preparation stream
Journey is simply efficiently, favorable reproducibility, product purity height, good crystallinity, low in raw material price, energy consumption be low, environmental friendliness and Yi work
The advantages such as industry amplification, are particularly suitable for low cost and prepare the industrialized production of cobalt protoxide.
Accompanying drawing explanation
Fig. 1 is the TEM figure of the cobalt protoxide nanoparticle of preparation in embodiment 1.
Fig. 2 is the HRTEM figure of the cobalt protoxide nanoparticle of preparation in embodiment 1.
Fig. 3 is the SEAD figure of the cobalt protoxide nanoparticle of preparation in embodiment 1.
Fig. 4 is the XRD figure of the cobalt protoxide nanoparticle of preparation in embodiment 1.
Fig. 5 is the TEM figure of the cobalt protoxide nanoparticle of preparation in embodiment 2.
Fig. 6 is the TEM figure of the cobalt protoxide nanoparticle of preparation in embodiment 3.
Fig. 7 is the SAED figure of the cobalt protoxide nanoparticle of preparation in embodiment 3.
Detailed description of the invention
The invention will be further described below by way of embodiments and drawings.
Embodiment 1:
6mL 0.2M cobalt nitrate solution it is slowly added dropwise under continuous stirring in 7.5mL 0.5M sodium hydroxide solution.Again
The disposable 0.03g cetyl trimethylammonium bromide powder that adds, continuation stirring 15min.Then above-mentioned mixed liquor is turned
Move to be furnished with in 25mL teflon-lined autoclave (Autoclave) and seal, reactor is put into
Take out after the baking oven of 180 DEG C reacts 5h.After air cooling to room temperature, with dehydrated alcohol centrifuge washing three times, then by gained
Precipitation vacuum drying obtains product.
In embodiment 1, the TEM figure of the cobalt protoxide nanoparticle of preparation sees Fig. 1, the cobalt protoxide nanoparticle of preparation
HRTEM figure sees Fig. 2, and the SEAD figure of the cobalt protoxide nanoparticle of preparation sees Fig. 3, the cobalt protoxide nanometer of preparation
The XRD figure of particle sees Fig. 4.
Embodiment 2:
6mL 0.03M cobalt nitrate solution it is slowly added dropwise under continuous stirring in 7.5mL 1M sodium hydroxide solution.Again
The disposable 0.05g myristic acid powder that adds, continuation stirring 15min.Then above-mentioned mixed liquor is transferred to be furnished with 25
In mL teflon-lined autoclave (Autoclave) and seal, reactor is put in the baking oven of 180 DEG C
Take out after reaction 4h.After air cooling to room temperature, with dehydrated alcohol centrifuge washing three times, then gained precipitation is vacuum dried
To product.
In embodiment 2, the TEM figure of the cobalt protoxide nanoparticle of preparation sees Fig. 5.
Embodiment 3:
Directly in 7.5mL 1M sodium hydroxide solution, it is slowly added dropwise 6mL 0.03M cobalt nitrate under continuous stirring molten
Liquid.Continue stirring 15min.Then above-mentioned mixed liquor being transferred to is furnished with 25mL teflon-lined autoclave
(Autoclave) in and seal, reactor is put into and takes out after the baking oven of 110 DEG C reacts 13h.Treat that air cooling is to room temperature
After, with dehydrated alcohol centrifuge washing three times, then gained is precipitated vacuum drying obtain product.
In embodiment 3, the TEM figure of the cobalt protoxide nanoparticle of preparation sees Fig. 6, the cobalt protoxide nanoparticle of preparation
SAED figure sees Fig. 7.
The present invention, by technology such as single step solvent-thermal method, eccentric cleaning, vacuum drying, simply and efficiently prepares cobalt protoxide and receives
Rice corpuscles, and determine its composition, pattern and crystal property by characterization methods such as XRD, TEM, HRTEM, SAED.The method
The cobalt protoxide nanoparticle of preparation is in granular form, particle diameter about 20nm, and it is simple that the present invention has preparation flow, favorable reproducibility,
The advantages such as product purity height, good crystallinity, are suitable to industrialized production.
Claims (7)
1. the solvothermal preparation method of a cobalt protoxide nanoparticle, it is characterised in that comprise the following steps:
1) in sodium hydroxide solution, add cobalt nitrate solution, add surfactant, obtain mixed liquor；Described sodium hydroxide
Solution, cobalt nitrate solution, the proportioning of surfactant are 7.5mL: 6mL: (0.03～0.05) g, wherein, and hydrogen-oxygen
Changing sodium solution, cobalt nitrate solution in terms of volume, surfactant is calculated by mass；The molar concentration of described sodium hydroxide solution
Being 0.5～1M, the molar concentration of described cobalt nitrate solution is 0.03～0.2M；
2) by step 1) mixed liquor that obtains is transferred to is furnished with in teflon-lined reactor and seals, reactor is put
Enter in baking oven and react, be cooled to room temperature, eccentric cleaning, abandon supernatant, obtain dense colloidal sol；
3) by step 2) the dense colloidal sol that obtains the most i.e. obtains cobalt protoxide nanoparticle powder；Or
In step 2) the dense colloidal sol that obtains adds dehydrated alcohol, obtain cobalt protoxide nanoparticle sol, at 4 DEG C after sealing
Lower long term storage.
The solvothermal preparation method of a kind of cobalt protoxide nanoparticle the most as claimed in claim 1, it is characterised in that in step 1)
In, described sodium hydroxide solution and cobalt nitrate solution all use dehydrated alcohol to prepare.
The solvothermal preparation method of a kind of cobalt protoxide nanoparticle the most as claimed in claim 1, it is characterised in that in step 1)
In, described surfactant is selected from cetyl trimethylammonium bromide powder or myristic acid powder.
The solvothermal preparation method of a kind of cobalt protoxide nanoparticle the most as claimed in claim 1, it is characterised in that in step 2)
In, described polytetrafluoroethyllining lining uses 25mL polytetrafluoroethyllining lining.
The solvothermal preparation method of a kind of cobalt protoxide nanoparticle the most as claimed in claim 1, it is characterised 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.
The solvothermal preparation method of a kind of cobalt protoxide nanoparticle the most as claimed in claim 1, it is characterised in that in step 2)
In, described eccentric cleaning is to use dehydrated alcohol centrifuge washing 3 times, and described centrifugal condition is centrifugal 10min under 8000rpm.
The solvothermal preparation method of a kind of cobalt protoxide nanoparticle the most as claimed in claim 1, it is characterised in that in step 3)
In, described dry employing is vacuum dried, and vacuum drying condition is 60 DEG C ,-0.1MPa.
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