CN102557106B - Preparation method of cuprous oxide hollow nanometer cubes - Google Patents
Preparation method of cuprous oxide hollow nanometer cubes Download PDFInfo
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- CN102557106B CN102557106B CN 201210008143 CN201210008143A CN102557106B CN 102557106 B CN102557106 B CN 102557106B CN 201210008143 CN201210008143 CN 201210008143 CN 201210008143 A CN201210008143 A CN 201210008143A CN 102557106 B CN102557106 B CN 102557106B
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Abstract
The invention discloses a preparation method of cuprous oxide hollow nanometer cubes. According to the preparation method, a chemical reducing method is adopted, polyhydric alcohol is used as solvents and reducing agents, cuprous diacetone is reduced at high temperature, the cuprous oxide hollow nanometer cubes are obtained, the edge length of the obtained cuprous oxide hollow nanometer cubes is about 150nm, and the wall thickness is about 20nm. The preparation method has the advantages that the process is simple, any surfactants do not need to be added, the operation is simple and convenient, the cost is low, and the preparation method is suitable for mass production.
Description
Technical field
The present invention relates to the preparation method of Red copper oxide, be specifically related to the cubical preparation method of a kind of Red copper oxide hollow Nano.
Background technology
Hollow material is as a kind of functional materials of novel structure, compare with its body phase material and to have the characteristics such as density is low, surfactivity is high, Surface Permeability is strong, show great potential using value in fields such as biomarker, medicament slow release, artificial cell, photonic crystal and catalytic materials.In addition, hollow material is owing to its special nucleocapsid structure, and hollow space often can hold a large amount of guest molecules: can be used as microreactor on the one hand, for the synthesis of other materials; On the other hand, also can be used for the parcel of medicine, realize the controllable release of medicine.
Red copper oxide (Cu
2O) be a kind of very important p-type metal oxide semiconductor, its energy gap is 2.0 eV.Have a wide range of applications in fields such as photochemical catalysis, novel solar battery, magnetic memory apparatus, bio-sensing and coating.At present, about Cu
2The research of O nano material mainly concentrates on the synthetic of the solid materials such as nano particle, nanofiber, nano thin-film, to Cu
2The research of O hollow material is relatively less.The Cu that has reported
2The preparation method of O hollow material mainly is the auxiliary liquid phase reduction of tensio-active agent.The cluster that forms take polyvinylpyrrolidone and sodium lauryl sulphate such as (CN101041456) such as Fang Yun as soft template, hydrazine hydrate as reductive agent, the cupric ion reduction is obtained Cu
2The O hollow material; Punishment Lan Lan etc. (Hubei University's journal, 2008,30(3): 267-269) take neutralized verdigris as copper source, polyvinylpyrrolidone and sodium hydroxide as additive, glucose prepared Cu as reductive agent
2O open hollow nanometer ball; (J Phys Chem C 2008 112:16769-16773) take cupric chloride as copper source, polyoxyethylene glycol and sodium hydroxide as additive, adopts solvent-thermal method to prepare Cu to Xu etc.
2O hollow Nano cubes; Gou etc. (Nano Letters, 2003,3 (2): 231-234) take copper sulfate as copper source, cetyl trimethylammonium bromide and sodium hydroxide as additive, sodium ascorbate is as reductive agent, prepared Cu
2O hollow Nano cubes.In the multiple synthetic method of bibliographical information, large pogoniasis is used tensio-active agent, such as sodium lauryl sulphate, polyvinylpyrrolidone, cetyl trimethylammonium bromide, polyoxyethylene glycol etc.No matter the amphiphilic structure that tensio-active agent has is in the reunion that prevents nanoparticle or in its pattern regulation and control behavior, has all represented its vital role in the nano material preparation.But also there are some negative issues in the adding of tensio-active agent.The concentration of first tensio-active agent often directly affects the final pattern of product, needs the concentration of accuracy controlling tensio-active agent among the preparation technology, and this has brought a lot of troubles to suitability for industrialized production; It two is surfaces that tensio-active agent very easily is adsorbed on product, makes troubles for the cleaning of product, thereby affects the purity of final product.Therefore developing does not a kind ofly need to add tensio-active agent and the method that operation is simple is synthesized Cu
2The O hollow nano-material is very important.
Summary of the invention
The object of the invention is to: provide a kind of Red copper oxide hollow Nano cubical preparation method, this preparation method disobeys the abutment surface promoting agent, and operation is simple.
Technical solution of the present invention is: it is to mix with polyvalent alcohol with acetylacetone copper, prepares Red copper oxide hollow Nano cubes, and concrete steps are as follows:
(1) acetylacetone copper is joined in the polyvalent alcohol, under 1000-1500 rev/min agitation condition, be warming up to temperature of reaction with certain temperature rise rate;
(2) after reaction for some time, mentioned solution left standstill be cooled to room temperature, with ethanol and deionized water product is repeatedly washed, obtain light yellow precipitate, this throw out is obtained Red copper oxide hollow Nano cubes 70 ℃ of dryings.
Wherein, described polyvalent alcohol and acetylacetone copper weight ratio are 1:0.0005-0.020.
Wherein, polyvalent alcohol is a kind of in ethylene glycol, sorbyl alcohol, glycerol, the triethylene glycol etc.
Wherein, described temperature rise rate is 2-5 ℃/second.
Wherein, described temperature of reaction is 180-240 ℃.
Wherein, the described reaction times is 1-6 hour.
The invention has the beneficial effects as follows:
1, reaction system is simple, only uses acetylacetone copper (copper source) and two kinds of raw materials of polyvalent alcohol (solvent and reductive agent), does not add the tensio-active agent of control pattern, and synthesis technique and required production unit are simple, are fit to suitability for industrialized production.
2, the Red copper oxide hollow Nano cubes that is synthesized, size and pattern homogeneous, the length of side is about 150 nm, and wall thickness is about 20 nm.
Description of drawings
Fig. 1 is Red copper oxide hollow Nano cubes transmission electron microscope photo.
The cubical X-ray diffractogram of Fig. 2 Red copper oxide hollow Nano.
Embodiment
Further specify technical solution of the present invention below in conjunction with specific embodiment, these embodiment can not be interpreted as it is restriction to technical solution.
Embodiment 1: prepare Red copper oxide hollow Nano cubes according to following steps
(1) acetylacetone copper is joined in the polyvalent alcohol, be warming up to temperature of reaction with certain temperature rise rate under 1000 rev/mins agitation condition, wherein, described polyvalent alcohol and acetylacetone copper weight ratio are 1:0.0005; Wherein, polyvalent alcohol is ethylene glycol; Wherein, described temperature rise rate is 2 ℃/second; Wherein, described temperature of reaction is 180 ℃;
(2) react after 6 hours, mentioned solution is left standstill be cooled to room temperature, with ethanol and deionized water product is repeatedly washed, obtain light yellow precipitate, this throw out is obtained Red copper oxide hollow Nano cubes 70 ℃ of dryings.
Embodiment 2: prepare Red copper oxide hollow Nano cubes according to following steps
(1) acetylacetone copper is joined in the polyvalent alcohol, be warming up to temperature of reaction with certain temperature rise rate under 1100 rev/mins agitation condition, wherein, described polyvalent alcohol and acetylacetone copper weight ratio are 1:0.001; Wherein, polyvalent alcohol is sorbyl alcohol; Wherein, described temperature rise rate is 3 ℃/second; Wherein, described temperature of reaction is 200 ℃;
(2) react after 5 hours, mentioned solution is left standstill be cooled to room temperature, with ethanol and deionized water product is repeatedly washed, obtain light yellow precipitate, this throw out is obtained Red copper oxide hollow Nano cubes 70 ℃ of dryings.
Embodiment 3: prepare Red copper oxide hollow Nano cubes according to following steps
(1) acetylacetone copper is joined in the polyvalent alcohol, be warming up to temperature of reaction with certain temperature rise rate under 1250 rev/mins agitation condition, wherein, described polyvalent alcohol and acetylacetone copper weight ratio are 1:0.01; Wherein, polyvalent alcohol is glycerol; Wherein, described temperature rise rate is 4 ℃ of degree/seconds; Wherein, described temperature of reaction is 220 ℃ of degree;
(2) react after 3 hours, mentioned solution is left standstill be cooled to room temperature, with ethanol and deionized water product is repeatedly washed, obtain light yellow precipitate, this throw out is obtained Red copper oxide hollow Nano cubes 70 ℃ of dryings.
Embodiment 4: prepare Red copper oxide hollow Nano cubes according to following steps
(1) acetylacetone copper is joined in the polyvalent alcohol, be warming up to temperature of reaction with certain temperature rise rate under 1500 rev/mins agitation condition, wherein, described polyvalent alcohol and acetylacetone copper weight ratio are 1:0.020; Wherein, polyvalent alcohol is triethylene glycol; Wherein, described temperature rise rate is 5 ℃/second; Wherein, described temperature of reaction is 240 ℃;
(2) react after 1 hour, mentioned solution is left standstill be cooled to room temperature, with ethanol and deionized water product is repeatedly washed, obtain light yellow precipitate, this throw out is obtained Red copper oxide hollow Nano cubes 70 ℃ of dryings.
Claims (5)
1. the cubical preparation method of Red copper oxide hollow Nano, it is to mix with polyvalent alcohol with acetylacetone copper, prepares Red copper oxide hollow Nano cubes; Concrete steps are as follows:
(1) acetylacetone copper is joined in the polyvalent alcohol, under 1000-1500 rev/min agitation condition, be warming up to temperature of reaction with certain temperature rise rate;
(2) after reaction for some time, mentioned solution left standstill be cooled to room temperature, with ethanol and deionized water product is repeatedly washed, obtain light yellow precipitate, this throw out is obtained Red copper oxide hollow Nano cubes 70 ℃ of lower dryings; It is characterized in that: described polyvalent alcohol and acetylacetone copper weight ratio are 1:0.0005-0.020.
2. the cubical preparation method of Red copper oxide hollow Nano according to claim 1 is characterized in that: wherein, polyvalent alcohol is a kind of in ethylene glycol, sorbyl alcohol, glycerol, the triethylene glycol.
3. the cubical preparation method of Red copper oxide hollow Nano according to claim 1, it is characterized in that: wherein, described temperature rise rate is 2-5 ℃/second.
4. the cubical preparation method of Red copper oxide hollow Nano according to claim 1, it is characterized in that: wherein, described temperature of reaction is 180-240 ℃.
5. the cubical preparation method of Red copper oxide hollow Nano according to claim 1, it is characterized in that: wherein, the described reaction times is 1-6 hour.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102849778A (en) * | 2012-09-21 | 2013-01-02 | 中国科学院过程工程研究所 | Octahedron cuprous oxide crystal and preparation method thereof |
| CN103043703B (en) * | 2013-01-05 | 2014-06-11 | 河北工业大学 | Preparation method of hollow Cu2O cubic box |
| CN103387258B (en) * | 2013-08-07 | 2015-05-27 | 武汉理工大学 | Cuprous oxide nano hollow spheres as well as synthetic method and application method thereof |
| CN105565362A (en) * | 2015-12-21 | 2016-05-11 | 江苏大学 | Preparation method of reduced graphene oxide/cuprous oxide nano composite material |
| CN105771996B (en) * | 2016-04-08 | 2018-08-10 | 江苏大学 | A kind of preparation method of hexagonal phase nickel/redox graphene electrocatalysis material |
| CN106040234B (en) * | 2016-06-07 | 2019-01-15 | 苏州大学 | A kind of platinum gallium composite nano-catalyst and preparation method thereof |
| CN106241854B (en) * | 2016-09-05 | 2017-09-29 | 南通大学 | The method that nano cuprous oxide is prepared in glycerine and the positive dibutyl ester mixture system of adipic acid |
| CN111482175B (en) * | 2020-05-09 | 2022-10-28 | 中国科学技术大学 | Preparation method of copper/cuprous oxide heterojunction nanosheet catalyst |
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