CN106315662A - Porous cuprous oxide particle and preparation method thereof - Google Patents
Porous cuprous oxide particle and preparation method thereof Download PDFInfo
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- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The preparation method of porous cuprous oxide particle comprises the steps of a, mixing the copper sulfate pentahydrate with water, blending, and acquiring the copper sulfate solution, b, adding certain amount of CTAB and SDS into the copper sulfate solution, blending, heating to 60 to 90 DEG C, continuing the heating and blending for some time to form the mixed solution; c, adding the NaOH solution into the mixing solution to turn the solution into black; d, pouring the mixing solution in step c into glucose solution, blending for some time to turn the solution into orange red; e, processing the solution prepared in step d to acquire the porous cuprous oxide. The preparation method is characterized by simple processing, low cost and short reaction time, averagely distributed density and porous features and can be applied to the field of gas sensitivity requirement, adsorption and photocatalysis and the like.
Description
Technical field
The invention belongs to the preparation of the oxide of copper, relate to the preparation method of the cuprous granule of a kind of porous oxidation.
Background technology
Red copper oxide is as a kind of important p-type semiconductor material, and its band-gap energy is the 2.0-2.2ev suction in visible region
Receiving coefficient higher, energy transformation ratio is in theory up to 12%.In recent years, because of optical, electrical, the magnetic performance of its uniqueness and nontoxic, storage
Amount is abundant, and preparation cost is relatively low, cheap, and its purposes in each field gradually obtains the research and development of people, by
Proof has some and well applies, at aspect tools such as photocatalysis, solaode, sensor, lithium ion battery and magnetic storages
Have broad application prospects.Simultaneous oxidation is cuprous is also the important raw material of industry, in the industry such as boats and ships, water process, electronics and
Agricultural production all has extensive and important purposes.Due to Cu2The pattern of O and structure affect its physics to a great extent
And chemical property, therefore, synthesis controllable appearance and the micro-nano Cu of structure2O has become the focus and emphasis of research.
At present, existing many about Cu2O nano material preparation process controls its pattern and size to optimize its correspondence
Quality Research achievement is reported, such as scientific research person has used magnetron sputtering method, low-temperature solid-phase method, hydro-thermal method, vapour deposition process, solvent
The preparation of the method such as full-boiled process and electrochemical deposition synthesizes Cu2O nanosphere, nano wire, cube, hollow ball, thin film, octahedron and
The patterns such as dodecahedron.Although these methods all prepare Red copper oxide, but seldom can obtain the oxygen of stable performance, uniform particle diameter
Change cuprous, and a lot of comparatively laborious complexity of preparation method, as complicated in magnetron sputtering method not only method and also to equipment requirements very
High；Red copper oxide prepared by solid phase method is often without uniform morphology；Hydro-thermal method is temperature required higher and the response time is long, and controllability is relatively
Low；And existing method to prepare cellular granule less, preparation method is complicated, it may be necessary to high temperature or expensive device, as existing
Technology CN201410457696, needs high temperature and complicated reaction condition to make, also have impact on its application.
Therefore, how to utilize simple method, relatively low cost, it is not necessary to high temperature, prepare morphology controllable, porous C u2O
Grain is significant, its application expansible, is beneficial to the application in catalysis, air-sensitive, solar energy etc. field.
Summary of the invention
Primary technical problem to be solved by this invention is to provide that a kind of technique is simple, low cost, reaction time are short, equal
Even, the preparation method of porous Red copper oxide granule.
A kind of cuprous preparation method of porous oxidation, comprises the following steps: a. is soluble in water by copper sulphate pentahydrate, stirring, shape
Become copper-bath；
B. described copper-bath will add a certain amount of CTAB and SDS, stir under room temperature condition, be heated to 60-90
DEG C, heated and stirred certain time, form mixed solution；
C., in described mixed solution, NaOH solution, solution blackening are added；
D. by adding glucose solution in the solution of step c, stirring certain time, solution slowly becomes Chinese red；
E. by the solution post processing of step d, porous oxidation is i.e. obtained cuprous.
Further, the copper-bath concentration of described step a is 2.5 × 10-6mol/mL-1×10-5Mol/mL, described
The water of step a is deionized water.
Specifically, the CTAB in described step b and the amount of the material of copper sulphate pentahydrate are than being (0.69-11): 1.
As preferably, the SDS in described step b is (0.87-13.85) with the amount ratio of the material of copper sulphate pentahydrate: 1.
Further, the concentration of the NaOH solution in described step c is 1.25 × 10-3mol/mL-7.5×10-3mol/
ML, described NaOH are (1-37.5) with the amount ratio of the material of copper sulphate pentahydrate: 1.
Further, the heated and stirred certain time in described step b is 10-25 minute.
Further, in described step d the amount of glucose and the material of copper sulphate pentahydrate than for (2.32-83.5): 1；Institute
The stirring certain time stating step d is 30 minutes-60 minutes.
Further, the post processing of described step d is for naturally cool to room temperature by solution, centrifugal, washing, dried.
Present invention additionally comprises, a kind of cuprous granule of porous oxidation, use porous prepared by the preparation method of any of the above-described
Red copper oxide granule.
Beneficial effects of the present invention: the preparation method of the cuprous granule of porous oxidation of the present invention, it is not necessary to valuable instrument and equipment.
By rational technology controlling and process, it is achieved the preparation of the cuprous granule of porous oxidation, this Red copper oxide microsphere size is uniform, it is good to disperse
Good, there is preferable porous, can be applicable to the fields such as air-sensitive, absorption, photocatalysis.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) photo of the cuprous granule of porous oxidation prepared by example 2.
Fig. 2 is scanning electron microscope (SEM) photo of the cuprous granule of porous oxidation prepared by example 2.
Fig. 3 is the X ray diffracting spectrum of the cuprous granule of porous oxidation prepared by example 2.
Detailed description of the invention
Below by way of specific embodiment for further illustrating the method that the present invention describes, it is not intended that the present invention
It is confined to these embodiments.
Embodiment 1:
A kind of cuprous preparation method of porous oxidation, comprises the following steps:
A. 0.05g copper sulphate pentahydrate is dissolved in 80ml deionized water, stirs 20 minutes, form copper-bath, sulphuric acid
The concentration of copper solution is 6.25 × 10-6mol/mL；
B., copper-bath in step a will add the SDS of CTAB and 0.8g of 0.3g, stirring, it is heated to 60 DEG C, heating
Stir 10 minutes, form mixed solution；The amount of the material of described CTAB is 8.23 × 10-4Mol, described CTAB and copper sulphate pentahydrate
The amount ratio of material be 4.12: 1；The amount of the material of described SDS is 2.77 × 10-3Mol, described SDS and the thing of copper sulphate pentahydrate
The amount ratio of matter is 13.85: 1.
C. adding 1ml concentration is 1.25 × 10-3The material of the NaOH solution of mol/m, described NaOH and copper sulphate pentahydrate
Amount ratio is 6.25: 1, solution blackening；
D. by adding 0.5g glucose solution in the solution of step c, stirring 30 minutes, solution slowly becomes Exocarpium Citri Rubrum
Color；Described glucose is 13.9: 1 with the amount ratio of the material of copper sulphate pentahydrate；
E. by the solution post processing of step d, i.e. take out, naturally cool to room temperature, centrifugal, clean, dried, obtain many
Hole Red copper oxide.
Embodiment 2
A kind of cuprous preparation method of porous oxidation, comprises the following steps:
A. 0.1g copper sulphate pentahydrate is dissolved in 100ml deionized water, stirs 20 minutes, form copper-bath, described
Copper-bath concentration is 4 × 10-6mol/mL；
B. will add the SDS of CTAB and 0.43g of 0.54g in step a, stirring forms mixed solution, is heated to 60 DEG C, stirs
Mix 10 minutes；The amount of the material of described CTAB is 1.48 × 10-3The amount of the material of mol, described CTAB and copper sulphate pentahydrate
Ratio is 3.7: 1；The amount of the material of described SDS is 1.49 × 10-3Mol, described SDS with the amount ratio of the material of copper sulphate pentahydrate are
3.73∶1。
C. adding 1ml concentration is 2 × 10-3The NaOH solution of mol/mL, solution blackening；Described NaOH and copper sulphate pentahydrate
The amount ratio of material is 5: 1；
D. by adding 1g glucose solution in the solution of step c, stirring 35 minutes, solution slowly becomes Chinese red；
Described glucose is 13.9: 1 with the amount ratio of the material of copper sulphate pentahydrate；
E. the solution of step d is taken out, naturally cool to room temperature, centrifugal, clean, dried, obtain porous oxidation sub-
Copper.
Accompanying drawing 1-3 is SEM figure and the XRD figure of the cuprous granule of porous oxidation prepared by the method, accompanying drawing understand and successfully make
For having gone out cuprous oxide crystal, and granule is uniform, and is loose structure.
Embodiment 3
A kind of cuprous preparation method of porous oxidation, comprises the following steps:
A. 0.1g copper sulphate pentahydrate is dissolved in 100ml deionized water, stirs 20 minutes, form copper-bath, described
Copper-bath concentration is 4 × 10-6mol/mL；
B. will add the SDS of CTAB and 0.3g of 0.8g in step a, stirring forms mixed solution, is heated to 60 DEG C, stirring
10 minutes；The amount of the material of described CTAB is 2.2 × 10-3Mol, described CTAB with the amount ratio of the material of copper sulphate pentahydrate are
5.5∶1；The amount of the material of described SDS is 1.04 × 10-3Mol, described SDS are 2.6: 1 with the amount ratio of the material of copper sulphate pentahydrate.
C., in described mixed solution, adding 1ml concentration is 2 × 10-3The NaOH solution of mol/mL, solution blackening；Described
NaOH is 5: 1 with the amount ratio of the material of copper sulphate pentahydrate；
D. by adding 1g glucose solution in the solution of step c, stirring 35 minutes, solution slowly becomes Chinese red；
Described glucose is 13.9: 1 with the amount ratio of the material of copper sulphate pentahydrate；
E. the solution of step d is taken out, naturally cool to room temperature, centrifugal, clean, dried, i.e. obtain porous oxidation
Cuprous.
Embodiment 4
A kind of cuprous preparation method of porous oxidation, comprises the following steps:
A. 0.1g copper sulphate pentahydrate is dissolved in 100ml deionized water, stirs 20 minutes, form copper-bath, described
Copper-bath concentration is 4 × 10-6mol/mL；
B. will add the SDS of CTAB and 0.43g of 0.54g in step a, stirring forms mixed solution, is heated to 70 DEG C, adds
Thermal agitation 10 minutes；The amount of the material of described CTAB is 1.48 × 10-3Mol, described CTAB and the material of copper sulphate pentahydrate
Amount ratio be 3.7: 1；The amount of the material of described SDS is 1.49 × 10-3The amount ratio of mol, described SDS and the material of copper sulphate pentahydrate
It is 3.73: 1.
C. adding 1ml concentration is 2 × 10-3The NaOH solution of mol/mL, solution blackening；Described NaOH and copper sulphate pentahydrate
The amount ratio of material is 5: 1；
D. by adding 1g glucose solution in the solution of step c, stirring 35 minutes, solution slowly becomes Chinese red；
Described glucose is 13.9: 1 with the amount ratio of the material of copper sulphate pentahydrate；
E. the solution of step d is taken out, naturally cool to room temperature, centrifugal, clean, dried, obtain porous oxidation sub-
Copper.
Embodiment 5
A kind of cuprous preparation method of porous oxidation, comprises the following steps:
A. 0.1g copper sulphate pentahydrate is dissolved in 100ml deionized water, stirs 20 minutes, form copper-bath, described
Copper-bath concentration is 4 × 10-6mol/mL；
B. will add the SDS of CTAB and 0.43g of 0.54g in step a, stirring forms mixed solution, is heated to 80 DEG C, adds
Thermal agitation 10 minutes；The amount of the material of described CTAB is 1.48 × 10-3Mol, described CTAB and the material of copper sulphate pentahydrate
Amount ratio be 3.7: 1；The amount of the material of described SDS is 1.49 × 10-3The amount ratio of mol, described SDS and the material of copper sulphate pentahydrate
It is 3.73: 1.
C. adding 1ml concentration is 2 × 10-3The NaOH solution of mol/mL, solution blackening；Described NaOH and copper sulphate pentahydrate
The amount ratio of material is 5: 1；
D. by adding 1g glucose solution in the solution of step c, stirring 35 minutes, solution slowly becomes Chinese red；
Described glucose is 13.9: 1 with the amount ratio of the material of copper sulphate pentahydrate；
E. the solution of step d is taken out, naturally cool to room temperature, centrifugal, clean, dried, obtain porous oxidation sub-
Copper.
Embodiment 6
A kind of cuprous preparation method of porous oxidation, comprises the following steps:
A. 0.1g copper sulphate pentahydrate is dissolved in 100ml deionized water, stirs 20 minutes, form copper-bath, described
Copper-bath concentration is 4 × 10-6mol/mL；
B. will add the SDS of CTAB and 0.43g of 0.54g in step a, stirring forms mixed solution, is heated to 90 DEG C, adds
Thermal agitation 10 minutes；The amount of the material of described CTAB is 1.48 × 10-3Mol, described CTAB and the material of copper sulphate pentahydrate
Amount ratio be 3.7: 1；The amount of the material of described SDS is 1.49 × 10-3The amount ratio of mol, described SDS and the material of copper sulphate pentahydrate
It is 3.73: 1.
C. adding 1ml concentration is 2 × 10-3The NaOH solution of mol/mL, solution blackening；Described NaOH and copper sulphate pentahydrate
The amount ratio of material is 5: 1；
D. by adding 1g glucose solution in the solution of step c, stirring 35 minutes, solution slowly becomes Chinese red；
Described glucose is 13.9: 1 with the amount ratio of the material of copper sulphate pentahydrate；
E. the solution of step d is taken out, naturally cool to room temperature, centrifugal, clean, dried, obtain porous oxidation sub-
Copper.
Embodiment 7
A kind of cuprous preparation method of porous oxidation, comprises the following steps:
A. 0.1g copper sulphate pentahydrate is dissolved in 100ml deionized water, stirs 15 minutes, form copper-bath, described
Copper-bath concentration is 4 × 10-6mol/mL；
B. will add the SDS of CTAB and 0.43g of 0.54g in step a, stirring forms mixed solution, is heated to 60 DEG C, adds
Thermal agitation 25 minutes；The amount of the material of described CTAB is 1.48 × 10-3Mol, described CTAB and the material of copper sulphate pentahydrate
Amount ratio be 3.7: 1；The amount of the material of described SDS is 1.49 × 10-3The amount ratio of mol, described SDS and the material of copper sulphate pentahydrate
It is 3.73: 1.
C. adding 1ml concentration is 2 × 10-3The NaOH solution of mol/mL, solution blackening；Described NaOH and copper sulphate pentahydrate
The amount ratio of material is 5: 1；
D. by adding 1g glucose solution in the solution of step c, stirring 60 minutes, solution slowly becomes Chinese red；
Described glucose is 13.9: 1 with the amount ratio of the material of copper sulphate pentahydrate；
E. the solution of step d is taken out, naturally cool to room temperature, centrifugal, clean, dried, obtain porous oxidation sub-
Copper.
Embodiment 8
A kind of cuprous preparation method of porous oxidation, comprises the following steps:
A. 0.1g copper sulphate pentahydrate is dissolved in 100ml deionized water, stirs 20 minutes, form copper-bath, described
Copper-bath concentration is 4 × 10-6mol/mL；
B. will add the SDS of CTAB and 0.43g of 0.54g in step a, stirring forms mixed solution, is heated to 60 DEG C, adds
Thermal agitation 10 minutes；The amount of the material of described CTAB is 1.48 × 10-3Mol, described CTAB and the material of copper sulphate pentahydrate
Amount ratio be 3.7: 1；The amount of the material of described SDS is 1.49 × 10-3The amount ratio of mol, described SDS and the material of copper sulphate pentahydrate
It is 3.73: 1.
C. adding 1ml concentration is 2 × 10-3The NaOH solution of mol/mL, solution blackening；Described NaOH and copper sulphate pentahydrate
The amount ratio of material is 5: 1；
D. by adding 1g glucose solution in the solution of step c, stirring 30 minutes, solution slowly becomes Chinese red；
Described glucose is 13.9: 1 with the amount ratio of the material of copper sulphate pentahydrate；
E. the solution of step d is taken out, naturally cool to room temperature, centrifugal, clean, dried, obtain porous oxidation sub-
Copper.
Embodiment 9
A kind of cuprous preparation method of porous oxidation, comprises the following steps:
A. 0.2g copper sulphate pentahydrate is incorporated in 110ml deionized water, stir 20 minutes, form copper-bath, described
Copper-bath concentration is 7.27 × 10-6mol/mL；
B. will add the SDS of CTAB and 0.5g of 0.7g in the copper-bath of step a, stirring forms mixed solution, adds
Heat, to 60 DEG C, stirs 10 minutes；The amount of the material of described CTAB is 1.92 × 10-3Mol, described CTAB and copper sulphate pentahydrate
The amount ratio of material be 2.4: 1；The amount of the material of described SDS is 1.73 × 10-3Mol, described SDS and the material of copper sulphate pentahydrate
Amount ratio be 2.2: 1.
C. adding 1ml concentration is 3.75 × 10-3The NaOH solution of mol/mL, solution blackening；Described NaOH and five water sulphuric acid
The amount ratio of the material of copper is 4.7: 1；
D. adding 2g glucose solution, stir 35 minutes, solution slowly becomes Chinese red；Described glucose and five water
The amount ratio of the material of copper sulfate is 13.8: 1；
E. the solution of step d is taken out, naturally cool to room temperature, centrifugal, clean, dried.
Embodiment 10
A kind of cuprous preparation method of porous oxidation, comprises the following steps:
A. 0.3g copper sulphate pentahydrate is incorporated in 120ml deionized water, stir 20 minutes；Form copper-bath, described
Copper-bath concentration is 1 × 10-5mol/mL；
B. will add the SDS of CTAB and 0.8g of 0.8g in step a, stirring forms mixed solution, is heated to 60 DEG C, stirring
10 minutes；The amount of the material of described CTAB is 2.2 × 10-3Mol, described CTAB with the amount ratio of the material of copper sulphate pentahydrate are
1.83∶1；The amount of the material of described SDS is 2.77 × 10-3Mol, described SDS are 2.3 with the amount ratio of the material of copper sulphate pentahydrate:
1。
C. adding 1ml concentration is 7.5 × 10-5The NaOH solution of mol/mL, solution blackening；Described NaOH and copper sulphate pentahydrate
The amount ratio of material be 6.25: 1；
D. adding 3g glucose solution, stir 60 minutes, solution slowly becomes Chinese red；Described glucose and five water
The amount ratio of the material of copper sulfate is 13.9: 1；
(5) solution of step d is taken out, naturally cool to room temperature, centrifugal, clean, dried.
Embodiment 11
A kind of cuprous preparation method of porous oxidation, comprises the following steps:
A. 0.05g copper sulphate pentahydrate is dissolved in 80ml deionized water, stirs 20 minutes, form copper-bath, described
Copper-bath concentration is 2.5 × 10-6mol/mL；
B. will add the SDS of CTAB and 0.8g of 0.8g in step a, stirring forms mixed solution, is heated to 90 DEG C, stirring
25 minutes；The amount of the material of described CTAB is 2.2 × 10-3Mol, described CTAB with the amount ratio of the material of copper sulphate pentahydrate are
11∶1；The amount of the material of described SDS is 2.77 × 10-3Mol, described SDS are 13.85 with the amount ratio of the material of copper sulphate pentahydrate:
1。
C. adding 1ml concentration is 7.5 × 10-3The NaOH solution of mol/mL, solution blackening；Described NaOH and copper sulphate pentahydrate
The amount ratio of material be 37.5: 1；
D. by adding 3g glucose solution in the solution of step c, stirring 60 minutes, solution slowly becomes Chinese red；
Described glucose is 83.5: 1 with the amount ratio of the material of copper sulphate pentahydrate；
E. the solution of step d is taken out, naturally cool to room temperature, centrifugal, clean, dried, obtain porous oxidation sub-
Copper.
Embodiment 12
A kind of cuprous preparation method of porous oxidation, comprises the following steps:
A. 0.3g copper sulphate pentahydrate is dissolved in 120ml deionized water, stirs 20 minutes, form copper-bath, described
Copper-bath concentration is 1 × 10-5mol/mL；
B. will add the SDS of CTAB and 0.3g of 0.3g in step a, stirring forms mixed solution, is heated to 60 DEG C, stirring
10 minutes；The amount of the material of described CTAB is 8.23 × 10-4The amount ratio of mol, described CTAB and the material of copper sulphate pentahydrate
It is 0.69: 1；The amount of the material of described SDS is 1.04 × 10-3Mol, described SDS with the amount ratio of the material of copper sulphate pentahydrate are
0.87∶1。
C. adding 1ml concentration is 1.25 × 10-3The NaOH solution of mol/mL, solution blackening；Described NaOH and five water sulphuric acid
The amount ratio of the material of copper is 1: 1；
D. by adding 0.5g glucose solution in the solution of step c, stirring 30 minutes, solution slowly becomes Exocarpium Citri Rubrum
Color；Described glucose is 2.32: 1 with the amount ratio of the material of copper sulphate pentahydrate；
E. the solution of step d is taken out, naturally cool to room temperature, centrifugal, clean, dried, obtain porous oxidation sub-
Copper.
Embodiment 13
The cuprous granule of porous oxidation, uses the cuprous granule of porous oxidation prepared by the preparation method of embodiment 1-12.
Claims (9)
1. the cuprous preparation method of porous oxidation, it is characterised in that: comprise the following steps:
A. copper sulphate pentahydrate is soluble in water, stirring, form copper-bath；
B. described copper-bath will add a certain amount of CTAB and SDS, stirring, it is heated to 60-90 DEG C, heated and stirred is certain
Time, form mixed solution；
C., in described mixed solution, NaOH solution, solution blackening are added；
D. by adding glucose solution in the solution of step c, stirring certain time, solution slowly becomes Chinese red；
E. by the solution post processing of step d, porous oxidation is i.e. obtained cuprous.
A kind of cuprous preparation method of porous oxidation the most according to claim 1, it is characterised in that: the sulphuric acid of described step a
Copper solution concentration is 2.5 × 10-6mol/mL-1×10-5Mol/mL, the water of described step a is deionized water.
A kind of cuprous preparation method of porous oxidation the most according to claim 1, it is characterised in that: in described step b
CTAB is (0.69-11) with the amount ratio of the material of copper sulphate pentahydrate: 1.
4. according to the cuprous preparation method of a kind of porous oxidation described in claim 1 or 2 or 3, it is characterised in that: described step b
In the amount of SDS and the material of copper sulphate pentahydrate than for (0.87-13.85): 1.
A kind of cuprous preparation method of porous oxidation the most according to claim 1, it is characterised in that: in described step c
The concentration of NaOH solution is 1.25 × 10-3mol/mL-7.5×10-3The material of mol/mL, described NaOH and copper sulphate pentahydrate
Amount ratio is (1-37.5): 1.
A kind of cuprous preparation method of porous oxidation the most according to claim 1, it is characterised in that: adding in described step b
Thermal agitation certain time is 10-25 minute.
A kind of cuprous preparation method of porous oxidation the most according to claim 1, it is characterised in that: Fructus Vitis viniferae in described step d
Sugar is (2.32-83.5) with the amount ratio of the material of copper sulphate pentahydrate: 1；The stirring certain time of described step d is 30 minutes-60
Minute.
8. according to the cuprous preparation method of a kind of porous oxidation described in claim 1, it is characterised in that: the post processing of described step d
For solution is naturally cooled to room temperature, centrifugal, washing, dried.
9. the cuprous granule of porous oxidation, it is characterised in that use the preparation method of any one of the claims 1-8 to prepare
The cuprous granule of porous oxidation.
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