CN102951671A - Preparation method of copper oxide nano particle - Google Patents
Preparation method of copper oxide nano particle Download PDFInfo
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- CN102951671A CN102951671A CN2012104038009A CN201210403800A CN102951671A CN 102951671 A CN102951671 A CN 102951671A CN 2012104038009 A CN2012104038009 A CN 2012104038009A CN 201210403800 A CN201210403800 A CN 201210403800A CN 102951671 A CN102951671 A CN 102951671A
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Abstract
The invention discloses a preparation method of a copper oxide nano particle, which comprises the steps of: firstly, adding a copper salt to a certain volume of distilled water, stirring until completely dissolving, preparing a copper particle solution with a copper particle concentration of 0.20-0.45mol/L, heating to 70-95 DEG C; then transferring the copper particle solution to a three-neck flask, placing the three-neck flask in a refluxing device of a glycerine bath, heating to 95-100 DEG C; subsequently, completely adding the copper particle solution heated to 70-95 DEG C in the step 1 into a sodium hydroxide solution at a stirring speed of 800-1000rpm, generating black precipitate, and refluxing for 4-10h at a stirring speed of 800-1000rpm to obtain a mixture containing the black precipitate; and finally, centrifuging and washing the mixture containing the black precipitate, vacuum-drying to obtain the copper oxide nano particle. The preparation method is simple, safe and pollution-free, and is low in cost and convenient for volume production; and the prepared copper oxide nano particle is of an alpha-Al2O3 structure, has a crystal particle size of 25-35 nanometers, and a specific surface area of 60-90m<2>/g.
Description
Technical field
The present invention relates to a kind of preparations of nanomaterials method, specifically a kind of preparation method of copper oxide nano particle.
Background technology
Cupric oxide powder is a kind of very important Multifunctional fine inorganic materials, be widely used as the tinting material of glass, porcelain, the catalyzer of organic synthesis, the sweetening agent of oils, hydrogenant agent, the also manufacturing through being usually used in artificial silk, gasometry and mensuration organic compound etc., also can be used as the burningrate catalyst of rocket propellant, particularly after copper oxide particle reaches nano level, using can be more wide, this moment, copper oxide nano material need to satisfy two standards: first, the nano cupric oxide size must be in nanometer scale, generally between 1-100nm; Second, the physics of nano cupric oxide, chemical property all changes to some extent, and at this moment particle diameter is little owing to having, specific surface area large, the catalytic activity high makes it show unusual characteristic at aspects such as electricity, magnetic, catalysis, thereby has more wide application prospect.
The method for preparing at present nano cupric oxide mainly contains: chemical precipitation method, solvent thermal or hydro-thermal, sol-gel method, template, solid reaction process, microemulsion method, laser ablation etc.Chemical precipitation method is to obtain precursor with the precipitation agent reaction in mantoquita, precursor is heat-treated obtain nano cupric oxide.This method simple to operate needs high-temperature heat treatment, and energy consumption nanoparticle large and that obtain is easily reunited.Solvent thermal or hydrothermal method need to be carried out in the container of high temperature and high pressure, and be high to equipment requirements.Production efficiency is low, and cost is high.Sol-gel method is reactant to be hydrolyzed under certain condition become gel, and gel is carried out obtaining nanoparticle after drying and the thermal treatment, and this method need to be used organic solvent, cost is high, needs the thermal treatment energy consumption large.Template is that mantoquita is fixed in the limited space, obtains tiny, the finely dispersed nanoparticle of particle diameter thereby add precipitation agent again.This method need to add the template material, gives the separation of back and removes and cause difficulty.The solid phase method reaction is incomplete, and the product yield that obtains is low.Microemulsion method is to utilize two kinds of immiscible solvents to form a uniform microemulsion under the effect of tensio-active agent, synthetic solid phase prepares a kind of method of nanoparticle in less microcell, the tensio-active agent that this method is introduced is difficult for reclaiming, and needs repetitive scrubbing, affects product purity.Laser ablation adopts laser to make light source, condensation is decomposed obtain nano cupric oxide.The present laboratory study of the method and small-scale production stage, the problem that runs in the suitability for industrialized production also lacks research.Above method has synthesis technique relative complex, condition is wayward, environmental pollution is serious, range of application is narrow shortcoming.
Summary of the invention
The present invention seeks to the deficiency for solving the problems of the technologies described above, a kind of preparation method of copper oxide nano particle is provided, the advantages such as the method has that synthesis temperature is low, technique is simple, condition is easily controlled, with low cost, pollution-free, applied range can realize green production.
The present invention solves the problems of the technologies described above the technical scheme that adopts to be:
A kind of preparation method of copper oxide nano particle, its concrete preparation process is:
Step 1, mantoquita is joined in the distilled water of certain volume, be stirred to fully dissolving after, the concentration of preparing copper particle be 0.20-0.45mol/L copper particle solution, be heated to 70 ℃-95 ℃, for subsequent use; Described mantoquita is copper sulfate, cupric chloride or cupric nitrate.
Step 2, sodium hydroxide is joined in the distilled water of certain volume, be stirred to fully dissolving after, prepare the sodium hydroxide solution that concentration is 0.02-3mol/L, for subsequent use.
Step 3, at first, the sodium hydroxide solution that step 2 prepares is transferred in the three-necked flask, the three-necked flask that then sodium hydroxide solution will be housed is placed in the reflux of glycerol bath and is heated to 95-100 ℃, then, under 800-1000 rev/min stirring velocity, step 1 is heated to 70-95 ℃ disposable the joining in the sodium hydroxide solution of copper particle solution, there is the black precipitate material to generate, under 800-1000 rev/min stirring velocity backflow 4-10 hour, obtain containing the mixture of black precipitate material.
Step 4, the mixture with 6000-90000 rev/min rotating speed centrifugal 10 minutes that the step 3 gained is contained the black precipitate material, abandon supernatant, be that the mixed solution that forms of the second alcohol and water of 4:6, the dehydrated alcohol of room temperature wash with 90 ℃ water, 50 ℃ volume ratio successively with gained black precipitate material, then namely getting copper oxide nano particle of the present invention after the vacuum-drying under 50 ℃ of conditions.
Beneficial effect
In preparation process not with an organic solvent and tensio-active agent, can not bring environmental pollution and ecological crisis problem.
2. method is simple, does not need high-temperature roasting, low being convenient to of cost to produce in enormous quantities.
3. prepared cupric oxide is the black nano particle, belongs to monoclinic system, and crystal particle diameter is the 15-20 nanometer, and specific surface area is 80-123m
2/ g.
Description of drawings
Fig. 1 is the X-ray diffracting spectrum of embodiment 1 prepared copper oxide nano particle.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
A kind of preparation method of copper oxide nano particle, its concrete preparation process is:
Step 1, mantoquita is joined in the distilled water, be stirred to fully dissolving after, the concentration of preparing copper particle be 0.20mol/L copper particle solution, be heated to 70 ℃, for subsequent use; Described mantoquita is cupric nitrate.
Step 2, sodium hydroxide is joined in the distilled water, be stirred to fully dissolving after, prepare the sodium hydroxide solution that concentration is 0.02mol/L, for subsequent use.
Step 3, at first, the sodium hydroxide solution that step 2 prepares is transferred in the three-necked flask, the three-necked flask that then sodium hydroxide solution will be housed is placed in the reflux of glycerol bath and is heated to 95 ℃, then, under 800 rev/mins stirring velocity, step 1 is heated to 70 ℃ disposable the joining in the sodium hydroxide solution of copper particle solution, there is the black precipitate material to generate, under 800 rev/mins stirring velocity, refluxed 4 hours, obtain containing the mixture of black precipitate material.
Step 4, the mixture with 6000 rev/mins rotating speed centrifugal 10 minutes that the step 3 gained is contained the black precipitate material, abandon supernatant, be that the mixed solution that forms of the second alcohol and water of 4:6, the dehydrated alcohol of room temperature wash with 90 ℃ water, 50 ℃ volume ratio successively with gained black precipitate material, then namely getting copper oxide nano particle of the present invention after the vacuum-drying under 50 ℃ of conditions, its particle diameter is 18.0nm.Specific surface area is 90m
2/ g.
Embodiment 2
A kind of preparation method of copper oxide nano particle, its concrete preparation process is:
Step 1, mantoquita is joined in the distilled water, be stirred to fully dissolving after, the concentration of preparing copper particle be 0.45mol/L copper particle solution, be heated to 95 ℃, for subsequent use; Described mantoquita is cupric chloride;
Step 2, sodium hydroxide is joined in the distilled water, be stirred to fully dissolving after, prepare the sodium hydroxide solution that concentration is 3mol/L, for subsequent use.
Step 3, at first, the sodium hydroxide solution that step 2 prepares is transferred in the three-necked flask, the three-necked flask that then sodium hydroxide solution will be housed is placed in the reflux of glycerol bath and is heated to 100 ℃, then, under 1000 rev/mins stirring velocity, step 1 is heated to 95 ℃ disposable the joining in the sodium hydroxide solution of copper particle solution, there is the black precipitate material to generate, under 1000 rev/mins stirring velocity, refluxed 10 hours, obtain containing the mixture of black precipitate material.
Step 4, the mixture with 90000 rev/mins rotating speed centrifugal 10 minutes that the step 3 gained is contained the black precipitate material, abandon supernatant, be that the mixed solution that forms of the second alcohol and water of 4:6, the dehydrated alcohol of room temperature wash with 90 ℃ water, 50 ℃ volume ratio successively with gained black precipitate material, then namely getting copper oxide nano particle of the present invention after the vacuum-drying under 50 ℃ of conditions, its particle diameter is 15.0nm, and specific surface area is 121m
2/ g.
Embodiment 3
A kind of preparation method of copper oxide nano particle, its concrete preparation process is:
Step 1, mantoquita is joined in the distilled water, be stirred to fully dissolving after, the concentration of preparing copper particle be 0.35mol/L copper particle solution, be heated to 80 ℃, for subsequent use; Described mantoquita is copper sulfate.
Step 2, sodium hydroxide is joined in the distilled water, be stirred to fully dissolving after, prepare the sodium hydroxide solution that concentration is 0.10mol/L, for subsequent use.
Step 3, at first, the sodium hydroxide solution that step 2 prepares is transferred in the three-necked flask, the three-necked flask that then sodium hydroxide solution will be housed is placed in the reflux of glycerol bath and is heated to 97 ℃, then, under 900 rev/mins stirring velocity, step 1 is heated to 80 ℃ disposable the joining in the sodium hydroxide solution of copper particle solution, there is the black precipitate material to generate, under 900 rev/mins stirring velocity, refluxed 8 hours, obtain containing the mixture of black precipitate material.
Step 4, the mixture with 50000 rev/mins rotating speed centrifugal 10 minutes that the step 3 gained is contained the black precipitate material, abandon supernatant, be that the mixed solution that forms of the second alcohol and water of 4:6, the dehydrated alcohol of room temperature wash with 90 ℃ water, 50 ℃ volume ratio successively with gained black precipitate material, then namely getting copper oxide nano particle of the present invention after the vacuum-drying under 50 ℃ of conditions, particle diameter is 17.0nm, and specific surface area is 101m
2/ g.
Embodiment 4
A kind of preparation method of copper oxide nano particle, its concrete preparation process is:
Step 1, the 5.0g cupric sulfate pentahydrate is joined in the 75mL distilled water, be stirred to fully dissolving after, the concentration of preparing copper particle be 0.266mol/L copper particle solution, be heated to 80 ℃, for subsequent use;
Step 2,1.6g sodium hydroxide is joined in the 75mL distilled water, be stirred to fully dissolving after, prepare concentration and be 0.533 sodium hydroxide solution, for subsequent use.
Step 3, at first, the sodium hydroxide solution that step 2 prepares is transferred in the three-necked flask, the three-necked flask that then sodium hydroxide solution will be housed is placed in the reflux of glycerol bath and is heated to 96 ℃, then, under 950 rev/mins stirring velocity, step 1 is heated to 97 ℃ disposable the joining in the sodium hydroxide solution of copper particle solution, there is the black precipitate material to generate, under 950 rev/mins stirring velocity backflow 4-10 hour, obtains containing the mixture of black precipitate material.
Step 4, the mixture with 60000 rev/mins rotating speed centrifugal 10 minutes that the step 3 gained is contained the black precipitate material, abandon supernatant, be that the mixed solution that forms of the second alcohol and water of 4:6, the dehydrated alcohol of room temperature wash with 90 ℃ water, 50 ℃ volume ratio successively with gained black precipitate material, then namely getting copper oxide nano particle of the present invention after the vacuum-drying under 50 ℃ of conditions.
Embodiment 5
A kind of preparation method of copper oxide nano particle, its concrete preparation process is:
Step 1, the 3.4g copper chloride dihydrate is joined in the distilled water of 75mL, be stirred to fully dissolving after, the concentration of preparing copper particle be 0.20-0.45mol/L copper particle solution, be heated to 70 ℃-95 ℃, for subsequent use.
Step 2,1.6g sodium hydroxide is joined in the 75mL distilled water, be stirred to fully dissolving after, prepare the sodium hydroxide solution that concentration is 0.533mol/L, for subsequent use.
Step 3, at first, the sodium hydroxide solution that step 2 prepares is transferred in the three-necked flask, the three-necked flask that then sodium hydroxide solution will be housed is placed in the reflux of glycerol bath and is heated to 95-100 ℃, then, under 800 rev/mins stirring velocity, step 1 is heated to 70-95 ℃ disposable the joining in the sodium hydroxide solution of copper particle solution, there is the black precipitate material to generate, under 960 rev/mins stirring velocity, refluxed 7 hours, obtain containing the mixture of black precipitate material.
Step 4, the mixture with 40000 rev/mins rotating speed centrifugal 10 minutes that the step 3 gained is contained the black precipitate material, abandon supernatant, be that the mixed solution that forms of the second alcohol and water of 4:6, the dehydrated alcohol of room temperature wash with 90 ℃ water, 50 ℃ volume ratio successively with gained black precipitate material, then namely getting copper oxide nano particle of the present invention after the vacuum-drying under 50 ℃ of conditions.
Claims (1)
1. the preparation method of a copper oxide nano particle, it is characterized in that: its concrete preparation process is:
Step 1, mantoquita is joined in the distilled water, be stirred to fully dissolving after, the concentration of preparing copper particle be 0.20-0.45mol/L copper particle solution, be heated to 70 ℃-95 ℃, for subsequent use; Described mantoquita is copper sulfate, cupric chloride or cupric nitrate;
Step 2, sodium hydroxide is joined in the distilled water, be stirred to fully dissolving after, prepare the sodium hydroxide solution that concentration is 0.02-3mol/L, for subsequent use;
Step 3, at first, the sodium hydroxide solution that step 2 prepares is transferred in the three-necked flask, the three-necked flask that then sodium hydroxide solution will be housed is placed in the reflux of glycerol bath and is heated to 95-100 ℃, then, under 800-1000 rev/min stirring velocity, step 1 is heated to 70-95 ℃ disposable the joining in the sodium hydroxide solution of copper particle solution, there is the black precipitate material to generate, under 800-1000 rev/min stirring velocity backflow 4-10 hour, obtain containing the mixture of black precipitate material;
Step 4, the mixture with 6000-90000 rev/min rotating speed centrifugal 10 minutes that the step 3 gained is contained the black precipitate material, abandon supernatant, be that the mixed solution that forms of the second alcohol and water of 4:6, the dehydrated alcohol of room temperature wash with 90 ℃ water, 50 ℃ volume ratio successively with gained black precipitate material, then namely getting copper oxide nano particle of the present invention after the vacuum-drying under 50 ℃ of conditions.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435088A (en) * | 2013-06-07 | 2013-12-11 | 江苏大学 | Method for preparing nano copper oxide in liquid phase by lignosulfonate template 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 |
| CN105036174A (en) * | 2015-07-10 | 2015-11-11 | 安鹏九 | Production method for submicron electronic-grade copper oxide powder |
| CN113968588A (en) * | 2021-11-19 | 2022-01-25 | 吴江市威士达铜业科技有限公司 | Production method of copper oxide |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435088A (en) * | 2013-06-07 | 2013-12-11 | 江苏大学 | Method for preparing nano copper oxide in liquid phase by lignosulfonate template method |
| CN103435088B (en) * | 2013-06-07 | 2016-04-06 | 江苏大学 | Sulfonated lignin template liquid phase prepares the method for nano cupric oxide |
| 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 |
| WO2016095520A1 (en) * | 2014-12-18 | 2016-06-23 | 中国科学院深圳先进技术研究院 | Method for preparing nano copper oxide and method for printing with metal-based ink |
| CN105036174A (en) * | 2015-07-10 | 2015-11-11 | 安鹏九 | Production method for submicron electronic-grade copper oxide powder |
| CN113968588A (en) * | 2021-11-19 | 2022-01-25 | 吴江市威士达铜业科技有限公司 | Production method of copper oxide |
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