CN104003433A - Preparation method of nano copper oxide material - Google Patents
Preparation method of nano copper oxide material Download PDFInfo
- Publication number
- CN104003433A CN104003433A CN201410176824.4A CN201410176824A CN104003433A CN 104003433 A CN104003433 A CN 104003433A CN 201410176824 A CN201410176824 A CN 201410176824A CN 104003433 A CN104003433 A CN 104003433A
- Authority
- CN
- China
- Prior art keywords
- preparation
- mantoquita
- solution
- cupric
- ammoniacal liquor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention provides a preparation method of a nano copper oxide material. The preparation method includes the steps: weighing and taking a copper salt, measuring and taking aqua ammonia, wherein the aqua ammonia mass fraction is 25-28%, and the molar ratio of the copper salt to aqua ammonia is 1:(6-10); then completely dissolving the copper salt in deionized water, adding aqua ammonia, fully stirring, and making into a cupric tetramminohydroxide solution; putting the cupric tetramminohydroxide solution into a microwave oven, and carrying out microwave heating reflux until no ammonia gas is released; and filtering the mixed liquid, remaining the filter cake, washing, drying at the temperature of 120-150 DEG C in a drying oven for overnight, and thus obtaining copper oxide. The preparation method has the advantages of simple synthetic process, easily obtained raw materials and low cost, the obtained product is high in purity and good in uniformity, and the particle size of the CuO powder can reach about 20 nm.
Description
Technical field
The invention belongs to chemical field, relate in particular to a kind of cupric oxide, is a kind of preparation method of nano oxidized copper product specifically.
Background technology
Cupric oxide is a kind of important inorganic materials, and people are growing on and on to its research in recent years.At catalytic field, it all has higher catalytic activity to the complete oxidation of the thermolysis of ammoniumper chlorate, carbon monoxide, ethanol, ethyl acetate and toluene etc., as can be for the scavenging material of vehicle exhaust, and the selective oxidation of CO in fuel cell.In addition, it can also deposit equipment etc. as high temperature superconducting materia, photochromics, gas sensor, magnetic.Aspect sensor, with cupric oxide, make the coating film of sensor, can greatly improve sensor to the selectivity of CO and sensitivity.Nano cupric oxide makes it in fields such as electricity, magnetic, catalysis, show uncommon characteristic because having surface effects, quantum size effect and Kub o effect.As surface effects makes its catalytic activity, greatly strengthen, quantum size effect makes infrared spectra broadening, blue shift and the division of nano cupric oxide.Therefore, the preparation of nanometer CuO and applied research are subject to extensive concern in recent years.
The preparation method of nano cupric oxide generally has: sol-gel method, solid reaction process, the liquid-phase precipitation method of control dual-jet, spray pyrolysis, the hot method of alcohol, sonochemistry method, the precipitator method, hydrothermal method, laser ablation etc.In actual nano cupric oxide preparation process, often above-mentioned several method is carried out to Integrated using.The present invention adopts strong hydrothermal decomposition method to form suspension liquid, and ageing produces precipitation and prepares nano cupric oxide.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nano oxidized copper product, the technical problem such as it is complicated that the preparation method of described this nano oxidized copper product will solve preparation method of the prior art, and cost is high, cupric oxide particle diameter is inhomogeneous.
The invention provides a kind of preparation method of nano oxidized copper product, comprise a step that takes mantoquita, also comprise a step that measures ammoniacal liquor, the massfraction of described ammoniacal liquor is 25-28%, described mantoquita and the mol ratio of ammoniacal liquor are 1: (6～10), then mantoquita is dissolved in deionized water completely, add ammoniacal liquor, fully stir, be prepared into cupric tetramminohydroxide solution, cupric tetramminohydroxide solution is put into microwave oven and carry out microwave heating backflow, until there is no ammonia, do not emit, mixed solution is filtered, retain filter cake, washing, 120～150 ℃ of dried overnight in baking oven, obtain cupric oxide.
Further, described mantoquita is Cu (NO
3)
2, or CuCl
2, or CuSO
4, or (CH
3cOO)
2cu.
Further, described microwave heating power is 500-900W.
Further, the ammonia producing in microwave heating process is by deionized water recovery.
Further, mantoquita is dissolved in the process in deionized water completely, the concentration of mantoquita is less than 0.5mol/L.
Above-mentioned reaction can cupric nitrate be raw material, and its chemical equation is:
Adopt microwave heating treatment, thereby the energy that microwave radiation produces can realize with electromagnetic form transmission the object that stirring on molecular level reaches homogeneous heating by water, due to glassware for drinking water, there is the dielectric characteristics of strong absorption microwave simultaneously, with the fierce collision friction of microwave frequency, produce a large amount of heat, thereby aqueous solvent is sharply volatilized and produces vapour pressure to be extruded as extraneous explosion by raw material inside, this sharply effect is risen rapidly water temperature, the cupric tetramminohydroxide solute being dissolved in water is decomposed, the CuO molecule producing is just suspended in solvent, with nanoparticle, exist in water.Obviously, copper ammon solution concentration used is less, decomposes and the CuO intermolecular distance that suspends is large and be not easy to assemble in water, and the CuO particle being prepared into is more tiny, has avoided picture solid Cu (OH)
2when pyrolytic decomposition is CuO because CuO packing of molecules is conducive to the defect that CuO particle is grown up.
The present invention decomposes cupric ammine complex to emit ammonia under strong hydrothermal condition, and in the aqueous solution, constantly produce nanometer CuO fine particle and be suspended in liquid phase, through ageing, filtration, washing and dry, and then preparation nanometer CuO.
The present invention compares with prior art, and its technical progress is significant.The present invention's raw material used is cheap and easy to get, and preparation method is simple, and gained cupric oxide particle diameter homogeneous and be nano level can obtain the CuO powder that particle diameter can reach 20nm left and right.And a large amount of ammonias that produce in thermal degradation process can adopt deionized water to absorb, the ammonia soln of gained again can be again for the preparation of cupric tetramminohydroxide solution.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum (XRD) of embodiment 1 prepared sample.
Fig. 2 is the X ray diffracting spectrum (XRD) of embodiment 2 prepared samples.
Embodiment
Below in conjunction with concrete embodiment, the present invention will be further described, so that those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
Embodiment 1
By 9.664gCu (NO
3)
23H
2o(0.04mol) be dissolved in completely in the deionized water of 400ml, adding 18ml massfraction is 25% ammoniacal liquor, fully stirs, and is prepared into Cu (NH
3)
4(OH)
2solution.Copper ammon solution is put into microwave oven, and microwave power is transferred to 800W, carries out microwave heating backflow, until do not have ammonia to emit.Mixed solution is filtered, retain filter cake, washing, in baking oven, 120 ℃ of dried overnight, obtain CuO black powder.As shown in Figure 1, the median size of calculating CuO with Scherrer formula is 19.3nm to its XRD figure spectrum.
Embodiment 2
By 9.664gCu (NO
3)
23H
2o (0.04mol) is dissolved in the deionized water of 300ml completely, and adding 25ml massfraction is 25% ammoniacal liquor, fully stirs, and is prepared into Cu (NH
3)
4(OH)
2solution.Copper ammon solution is put into microwave oven, and microwave power is transferred to 900W, carries out microwave heating backflow, until do not have ammonia to emit.Mixed solution is filtered, retain filter cake, washing, in baking oven, 140 ℃ of dried overnight, obtain CuO black powder.As shown in Figure 2, the median size of calculating CuO with Scherrer formula is 22.2nm to its XRD figure spectrum.
Embodiment 3
By 6.82gCuCl
22H
2o(0.04mol) be dissolved in completely in the deionized water of 300ml, all the other steps are with embodiment 2.Mixed solution after microwave heating is filtered, and repeatedly washing, by filter cake 130 ℃ of dried overnight in baking oven, obtains CuO black powder.
Embodiment 4
By 9.9872g CuSO
45H
2o(0.04mol) be dissolved in completely in the deionized water of 300ml, all the other steps are with embodiment 2.Mixed solution after microwave heating is filtered, and washing, by gained filter cake 120 ℃ of dried overnight in baking oven, obtains CuO black powder.
Embodiment 5
By 7.986g Cu (CH
3cOO)
2h
2o(0.04mol) be dissolved in completely in the deionized water of 300ml, all the other steps are with embodiment 2.Gained mixed solution is filtered, and washing, by filter cake 140 ℃ of dried overnight in baking oven, obtains CuO black powder.
Claims (4)
1. the preparation method of a nano oxidized copper product, it is characterized in that: comprise a step that takes mantoquita, also comprise a step that measures ammoniacal liquor, the massfraction of described ammoniacal liquor is 25-28%, described mantoquita and the mol ratio of ammoniacal liquor are 1: (6～10), then mantoquita is dissolved in deionized water completely, add ammoniacal liquor, fully stir, be prepared into cupric tetramminohydroxide solution, cupric tetramminohydroxide solution is put into microwave oven and carry out microwave heating backflow, until there is no ammonia, do not emit, mixed solution is filtered, retain filter cake, washing, 120～150 ℃ of dried overnight in baking oven, obtain cupric oxide.
2. the preparation method of a kind of nano oxidized copper product according to claim 1, is characterized in that: described mantoquita is Cu (NO
3)
2, or CuCl
2, or CuSO
4, or (CH
3cOO)
2cu.
3. the preparation method of a kind of nano oxidized copper product according to claim 1, is characterized in that: described microwave heating power is 500-900W.
4. the preparation method of a kind of nano oxidized copper product according to claim 1, is characterized in that: mantoquita is dissolved in the process in deionized water completely, and the concentration of mantoquita is less than 0.5mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410176824.4A CN104003433A (en) | 2014-04-30 | 2014-04-30 | Preparation method of nano copper oxide material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410176824.4A CN104003433A (en) | 2014-04-30 | 2014-04-30 | Preparation method of nano copper oxide material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104003433A true CN104003433A (en) | 2014-08-27 |
Family
ID=51364378
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410176824.4A Pending CN104003433A (en) | 2014-04-30 | 2014-04-30 | Preparation method of nano copper oxide material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104003433A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105129837A (en) * | 2015-09-09 | 2015-12-09 | 上海应用技术学院 | Preparation method of nano-cuprous oxide |
| CN105714356A (en) * | 2016-04-26 | 2016-06-29 | 临朐鹏博环保科技有限公司 | Sealant for aluminum alloy anode oxide film and preparing method for sealant |
| CN105821405A (en) * | 2016-03-25 | 2016-08-03 | 奇瑞汽车股份有限公司 | Preparation method and application of low-valence metal nano-structure thin film |
| CN109279654A (en) * | 2018-12-06 | 2019-01-29 | 盐城工学院 | A kind of preparation method of copper wolframic acid |
| CN110144479A (en) * | 2019-05-15 | 2019-08-20 | 内蒙古工业大学 | The method that fabricated in situ has the aluminum matrix composite of hierarchical structure |
| CN111517358A (en) * | 2020-06-16 | 2020-08-11 | 盐城工学院 | Synthetic method and application of flower-shaped copper oxide nanospheres |
| CN115304093A (en) * | 2022-08-10 | 2022-11-08 | 李晓清 | Continuous production process of high-purity copper oxide based on ammonia circulation system |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306832A (en) * | 2008-07-03 | 2008-11-19 | 上海交通大学 | Method for preparing hollow multilevel copper oxide nano material |
| CN101829579A (en) * | 2010-05-25 | 2010-09-15 | 上海应用技术学院 | Preparation method and application of cerium-zirconium composite oxide catalyst loaded with copper oxide |
| CN102614888A (en) * | 2012-03-12 | 2012-08-01 | 上海应用技术学院 | Method for preparing loaded CuO/CeO2 catalyst |
-
2014
- 2014-04-30 CN CN201410176824.4A patent/CN104003433A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306832A (en) * | 2008-07-03 | 2008-11-19 | 上海交通大学 | Method for preparing hollow multilevel copper oxide nano material |
| CN101829579A (en) * | 2010-05-25 | 2010-09-15 | 上海应用技术学院 | Preparation method and application of cerium-zirconium composite oxide catalyst loaded with copper oxide |
| CN102614888A (en) * | 2012-03-12 | 2012-08-01 | 上海应用技术学院 | Method for preparing loaded CuO/CeO2 catalyst |
Non-Patent Citations (4)
| Title |
|---|
| 李冬梅等: ""络合沉淀法合成纳米氧化铜粉体及其性能表征"", 《无机材料学报》 * |
| 袁芳芳等: ""微波辅助合成纳米氧化铜"", 《广州化工》 * |
| 陈根等: ""氧化铜微球的微波辅助液相合成与表征"", 《第七届中国功能材料及其应用学术会议论文集》 * |
| 雷涛等: ""纳米氧化铜粉体的制备及应用研究进展"", 《化工进展》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105129837A (en) * | 2015-09-09 | 2015-12-09 | 上海应用技术学院 | Preparation method of nano-cuprous oxide |
| CN105821405A (en) * | 2016-03-25 | 2016-08-03 | 奇瑞汽车股份有限公司 | Preparation method and application of low-valence metal nano-structure thin film |
| CN105821405B (en) * | 2016-03-25 | 2019-01-25 | 奇瑞汽车股份有限公司 | A kind of preparation method and application of low-valent metal nano structure membrane |
| CN105714356A (en) * | 2016-04-26 | 2016-06-29 | 临朐鹏博环保科技有限公司 | Sealant for aluminum alloy anode oxide film and preparing method for sealant |
| CN105714356B (en) * | 2016-04-26 | 2018-02-13 | 临朐鹏博环保科技有限公司 | A kind of aluminium alloy anode oxide film hole sealing agent and preparation method thereof |
| CN109279654A (en) * | 2018-12-06 | 2019-01-29 | 盐城工学院 | A kind of preparation method of copper wolframic acid |
| CN110144479A (en) * | 2019-05-15 | 2019-08-20 | 内蒙古工业大学 | The method that fabricated in situ has the aluminum matrix composite of hierarchical structure |
| CN111517358A (en) * | 2020-06-16 | 2020-08-11 | 盐城工学院 | Synthetic method and application of flower-shaped copper oxide nanospheres |
| CN111517358B (en) * | 2020-06-16 | 2021-11-02 | 盐城工学院 | Synthetic method and application of flower-shaped copper oxide nanospheres |
| CN115304093A (en) * | 2022-08-10 | 2022-11-08 | 李晓清 | Continuous production process of high-purity copper oxide based on ammonia circulation system |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104003433A (en) | Preparation method of nano copper oxide material | |
| Sajid et al. | Preparation and characterization of Vanadium pentoxide (V2O5) for photocatalytic degradation of monoazo and diazo dyes | |
| Ismael | A review and recent advances in solar-to-hydrogen energy conversion based on photocatalytic water splitting over doped-TiO2 nanoparticles | |
| Sun et al. | Synthesis and photocatalytic activity of nano-cobalt ferrite catalyst for the photo-degradation various dyes under simulated sunlight irradiation | |
| Zhao et al. | CeO2/3D g-C3N4 heterojunction deposited with Pt cocatalyst for enhanced photocatalytic CO2 reduction | |
| Chen et al. | Room temperature synthesized BaTiO3 for photocatalytic hydrogen evolution | |
| Nagabhushana et al. | Synthesis of bismuth vanadate: its application in H 2 evolution and sunlight-driven photodegradation | |
| Singh et al. | The role of pH and nitrate concentration in the wet chemical growth of nano-rods shaped ZnO photocatalyst | |
| Li et al. | Nature of catalytic activities of CoO nanocrystals in thermal decomposition of ammonium perchlorate | |
| CN103889898B (en) | It is enclosed in the preparation method of the particle of porous silica and porous silica and is enclosed in the particle of porous silica | |
| CN105233850A (en) | Magnetic nanometer composite photocatalysis material, and preparation method thereof | |
| Sulaeman et al. | Visible light photocatalytic activity induced by the carboxyl group chemically bonded on the surface of SrTiO3 | |
| CN104190423B (en) | A kind of spherical shape α-Fe2O3Preparation method | |
| Siddique et al. | Solution combustion synthesis: the relevant metrics for producing advanced and nanostructured photocatalysts | |
| Arumugam et al. | Solvent effects on the properties of Bi 2 S 3 nanoparticles: Photocatalytic application | |
| CN101993111B (en) | Method for preparing nanometer vanadous oxide | |
| Wang et al. | Z-scheme Cu2O/Bi/BiVO4 nanocomposite photocatalysts: synthesis, characterization, and application for CO2 photoreduction | |
| Yu et al. | Ultrasound-assisted construction of a Z-scheme heterojunction with g-C3N4 nanosheets and flower-like Bi2WO6 microspheres and the photocatalytic activity in the coupling reaction between alcohols and amines under visible light irradiation | |
| CN105540663A (en) | Controllable preparation method of CuSbS2 nanocrystalline material | |
| CN103664723B (en) | The preparation method of metal dithiocarbamate solution and nano metal sulfide material | |
| Lou et al. | A facility synthesis of bismuth-iron bimetal MOF composite silver vanadate applied to visible light photocatalysis | |
| Kang et al. | Photothermal reduction of 4-nitrophenol using rod-shaped core–shell structured catalysts | |
| Yan et al. | Molten salt pyrolysis synthesis of magnetic FeNCN nanorods and their visible-light-driven photocatalytic properties | |
| CN103440947A (en) | One-dimensional magnetic metal/carbon nano-composite material and preparation method thereof | |
| Dave et al. | NiCoZn Ferrite: burn rate enhancer for AP/HTPB based propellant and its catalytic study on the decomposition of ammonium perchlorate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140827 |