CN105858709A - Method for preparing nano copper oxide - Google Patents
Method for preparing nano copper oxide Download PDFInfo
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- CN105858709A CN105858709A CN201610179583.8A CN201610179583A CN105858709A CN 105858709 A CN105858709 A CN 105858709A CN 201610179583 A CN201610179583 A CN 201610179583A CN 105858709 A CN105858709 A CN 105858709A
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- cupric oxide
- copper carbonate
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- preparing nano
- basic
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention provides a method for preparing nano copper oxide by a one-step synthesis method. The method comprises the steps of adding an insoluble copper salt, i.e., basic copper carbonate and a strong alkali into water, ethanol or a mixed solvent, and carrying out stirring and constant-temperature heating, thereby producing the nano copper oxide. The method has the advantages that the copper source is the insoluble copper salt, the reaction process is simple, the reaction conditions are mild, and the requirements on reaction equipment are simple.
Description
Technical field
The present invention relates to the preparation method of a kind of nano cupric oxide, belong to field of inorganic nonmetallic material.
Background technology
Copper oxide is a kind of main p-type inorganic semiconductor material.The particle diameter of nanosized copper oxide is at 1-100nm
Between, nano level granule is in the transitional region of macro object and microcosmic particle, therefore nano cupric oxide tool
There are bulk effect, quantum size effect, skin effect and macro quanta tunnel effect.With common copper oxide phase
Ratio, the skin effect of nano cupric oxide make it have that specific surface area is big, high adsorption capacity, reactivity high and
The features such as selectivity is good.It addition, the surface atom of nanoparticle is different from granule interior atoms state, surface
The congruent factor of Atomic coordinate makes its surface activity position increase.
Nanosized copper oxide shows in terms of magnetic, light absorption, chemism, thermal resistance, catalyst and fusing point
Go out peculiar process based prediction model.Due to these characteristics, nano cupric oxide is widely used sensor, too
Sun can battery, photodetector, catalyst, increase fluid thermal conductance, nanoelectromechanical systems, Flied emission pole
In field, it has also become purposes widely one of inorganic material.
The preparation method of nano cupric oxide mainly have wet chemistry method, electrochemical process, microwave method, supercritical ultrasonics technology,
The sedimentation method, hydro-thermal method etc..Wherein hydro-thermal method is one of most important method.But hydro-thermal reaction needs at height
Carrying out in pressure still, reaction requires higher, and equipment is complicated, and these all limit the popularization of this technique, difficult
To realize large-scale production.
Summary of the invention
It is an object of the invention to provide a kind of method preparing nano cupric oxide, it is with insoluble mantoquita alkali formula carbon
Acid copper is raw material, and highly basic is precipitant, and cupric oxide powder is prepared in reaction, solves equipment in prior art multiple
Miscellaneous, reaction requires high problem, and the method reaction condition is gentle, and course of reaction is simple.
Preparation process of the present invention comprises the steps:
Step 1, joining in solvent by basic copper carbonate and highly basic, the mass ratio of basic copper carbonate and highly basic is,
Basic copper carbonate: highly basic=1.9:1-3:1, at a temperature of 50 DEG C-80 DEG C, stirs 5-12h, makes reaction fill
Divide and carry out, obtain mixed solution；
Step 2, above-mentioned mixed solution is cooled to room temperature after, be filtrated to get precipitation, with deionized water and anhydrous
Ethanol cyclic washing 2-3 time, is centrifuged and puts in an oven by the precipitation obtained, and dries 1-3h for 50 DEG C-70 DEG C,
Obtain cupric oxide powder.
Described highly basic includes sodium hydroxide and potassium hydroxide, and in reaction system, alkali concn controls 0.025
mol·L-1-4mol·L-1。
Described basic copper carbonate with the mass ratio of solvent is, basic copper carbonate: solvent=1:20-1:30.
Described solvent is in the mixed solvent of water, ethanol or choline chloride and carbamide composition.
In described mixed solvent, the mass ratio of choline chloride and carbamide is, choline chloride: carbamide=2:1.
When described highly basic is sodium hydroxide, course of reaction is as follows:
CuCO3·Cu(OH)2+2NaOH→2Cu(OH)2+Na2CO3 (1)
2Cu(OH)2→2CuO+2H2O (2)
Compared with existing additive method, the present invention has the following advantages:
(1) present invention uses insoluble mantoquita basic copper carbonate to be copper source, and its copper content is higher；
(2) present invention uses low temperature to synthesize copper oxide, should not produce agglomeration under low temperature；
(3) only having sodium carbonate and copper oxide in product of the present invention, the supernatant can be obtained by the method for recrystallization
To sodium carbonate, and sodium carbonate is also the important source material during chemical industry generates；
(4) present invention uses one-step synthesis to prepare nano cupric oxide, and the method is with water, ethanol, choline chloride:
The system of carbamide=2:1 is as solvent, and course of reaction is simple, and reaction condition is gentle.
Accompanying drawing explanation
Fig. 1 is in embodiment 1, X-ray diffraction (XRD) collection of illustrative plates of the nano cupric oxide of preparation.
Fig. 2 is in embodiment 1, scanning electron microscope (SEM) collection of illustrative plates of the nano cupric oxide of preparation.
From the X diffracting spectrum of Fig. 1 it is recognised that products therefrom is copper oxide.
From the image of the scanning electron microscope of Fig. 2 it can be seen that copper oxide is to be assembled life by the nanometer sheet of 13.6nm
Become the microsphere about 12 μm.
Detailed description of the invention
Embodiment 1
Weigh 1.105g basic copper carbonate and 0.4g sodium hydroxide, basic copper carbonate and sodium hydroxide are added
In 40mL deionized water, constant temperature stirring 5h at 50 DEG C.Centrifuge washing after cooling, with distilled water and
Absolute ethanol washing product 2-3 time, puts into powder in baking oven and is dried, obtain cupric oxide nanometer power.
Embodiment 2
Weigh 1.105g basic copper carbonate and 0.4g sodium hydroxide, basic copper carbonate and sodium hydroxide are added
Enter in 100mL deionized water, constant temperature stirring 5h at 50 DEG C.Centrifuge washing after cooling, with distillation
Water and absolute ethanol washing product 2-3 time, put into powder in baking oven and be dried, obtain cupric oxide nanometer power.
Embodiment 3
Weigh 1.105g basic copper carbonate and 0.561g potassium hydroxide, basic copper carbonate and potassium hydroxide are added
Enter in 100mL deionized water, constant temperature stirring 5h at 50 DEG C.Centrifuge washing after cooling, with distillation
Water and absolute ethanol washing product 2-3 time, put into powder in baking oven and be dried, obtain cupric oxide nanometer power.
Embodiment 4
Weigh 0.2762g basic copper carbonate and 0.1402g potassium hydroxide, by basic copper carbonate and potassium hydroxide
Join in 100mL deionized water, constant temperature stirring 5h at 50 DEG C.Centrifuge washing after cooling, with steaming
Distilled water and absolute ethanol washing product 2-3 time, put into powder in baking oven and be dried, obtain cupric oxide nano powder
Body.
Embodiment 5
Step 1, basic copper carbonate and potassium hydroxide are joined in alcohol solvent, basic copper carbonate and hydroxide
The mass ratio of potassium is, basic copper carbonate: potassium hydroxide=3:1, and basic copper carbonate with the mass ratio of alcohol solvent is,
Basic copper carbonate: alcohol solvent=1:30, at a temperature of 80 DEG C, stirs 5h, reacts fully and carry out,
Mixed solution；
Step 2, above-mentioned mixed solution is cooled to room temperature after, be filtrated to get precipitation, with deionized water and anhydrous
Ethanol cyclic washing 2-3 time, is centrifuged and puts in an oven by the precipitation obtained, and dries 3h, obtains for 50 DEG C
Cupric oxide powder.
Embodiment 6
Step 1, basic copper carbonate and sodium hydroxide are added to the water, basic copper carbonate and the matter of sodium hydroxide
Amount ratio is that basic copper carbonate: sodium hydroxide=1.9:1, basic copper carbonate is, alkali formula with the mass ratio of aqueous solvent
Curpic carbonate: aqueous solvent=1:20, at a temperature of 50 DEG C, stirs 12h, reacts fully and carry out, must mix molten
Liquid；
Step 2, above-mentioned mixed solution is cooled to room temperature after, be filtrated to get precipitation, with deionized water and anhydrous
Ethanol cyclic washing 2-3 time, is centrifuged and puts in an oven by the precipitation obtained, and dries 1h, obtains for 70 DEG C
Cupric oxide powder.
Embodiment 7
Step 1, basic copper carbonate and highly basic sodium hydroxide are joined choline chloride and carbamide composition mixing molten
In agent, in described mixed solvent, the mass ratio of choline chloride and carbamide is, choline chloride: carbamide=2:1,
The mass ratio of basic copper carbonate and highly basic sodium hydroxide is, basic copper carbonate: highly basic sodium hydroxide=2.5:1,
Basic copper carbonate with the mass ratio of solvent is, basic copper carbonate: solvent=1:25, at a temperature of 65 DEG C, and stirring
8h, reacts fully and carries out, obtain mixed solution；
Step 2, above-mentioned mixed solution is cooled to room temperature after, be filtrated to get precipitation, with deionized water and anhydrous
Ethanol cyclic washing 2-3 time, is centrifuged and puts in an oven by the precipitation obtained, and dries 2h, obtains for 60 DEG C
Cupric oxide powder.
In reaction system, alkali concn controls at 0.025mol L-1-4mol·L-1。
When described highly basic is sodium hydroxide, course of reaction is as follows:
CuCO3·Cu(OH)2+2NaOH→2Cu(OH)2+Na2CO3 (1)
2Cu(OH)2→2CuO+2H2O (2)
Claims (6)
1. the method preparing nano cupric oxide, it is characterised in that preparation process comprises the steps:
Step 1, joining in solvent by basic copper carbonate and highly basic, the mass ratio of basic copper carbonate and highly basic is,
Basic copper carbonate: highly basic=1.9:1-3:1, at a temperature of 50 DEG C-80 DEG C, stirs 5-12h, makes reaction fill
Divide and carry out, obtain mixed solution；
Step 2, above-mentioned mixed solution is cooled to room temperature after, be filtrated to get precipitation, with deionized water and anhydrous
Ethanol cyclic washing 2-3 time, is centrifuged and puts in an oven by the precipitation obtained, and dries 1-3h for 50 DEG C-70 DEG C,
Obtain cupric oxide powder.
A kind of method preparing nano cupric oxide the most according to claim 1, it is characterised in that described
In step 1, highly basic includes sodium hydroxide and potassium hydroxide, and in reaction system, alkali concn controls 0.025
mol·L-1-4mol·L-1。
A kind of method preparing nano cupric oxide the most according to claim 1, it is characterised in that described
In step 1, described basic copper carbonate with the mass ratio of solvent is, basic copper carbonate: solvent=1:20-1:30.
A kind of method preparing nano cupric oxide the most according to claim 1 and 2, it is characterised in that institute
In the step 1 stated, described solvent is in the mixed solvent of water, ethanol or choline chloride and carbamide composition.
A kind of method preparing nano cupric oxide the most according to claim 4, it is characterised in that described
In step 1, in described mixed solvent, the mass ratio of choline chloride and carbamide is, choline chloride: carbamide=2:1.
A kind of method preparing nano cupric oxide the most according to claim 2, it is characterised in that described
In step 1, when described highly basic is sodium hydroxide, course of reaction is as follows:
CuCO3·Cu(OH)2+2NaOH→2Cu(OH)2+Na2CO3 (1)
2Cu(OH)2→2CuO+2H2O (2)
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610179583.8A CN105858709A (en) | 2016-03-25 | 2016-03-25 | Method for preparing nano copper oxide |
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| CN201610179583.8A CN105858709A (en) | 2016-03-25 | 2016-03-25 | Method for preparing nano copper oxide |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007238388A (en) * | 2006-03-09 | 2007-09-20 | Tsurumi Soda Co Ltd | Copper oxide and its producing method |
| JP2008143737A (en) * | 2006-12-08 | 2008-06-26 | Furukawa Co Ltd | Cupric oxide powder and its manufacturing method |
| CN104528801A (en) * | 2014-12-18 | 2015-04-22 | 中国科学院深圳先进技术研究院 | Preparation method of nano copper oxide and printing method of metal-matrix printing ink |
-
2016
- 2016-03-25 CN CN201610179583.8A patent/CN105858709A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007238388A (en) * | 2006-03-09 | 2007-09-20 | Tsurumi Soda Co Ltd | Copper oxide and its producing method |
| JP2008143737A (en) * | 2006-12-08 | 2008-06-26 | Furukawa Co Ltd | Cupric oxide powder and its manufacturing method |
| CN104528801A (en) * | 2014-12-18 | 2015-04-22 | 中国科学院深圳先进技术研究院 | Preparation method of nano copper oxide and printing method of metal-matrix printing ink |
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Application publication date: 20160817 |
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