CN108975381A - The preparation method of monodisperse uniform morphology Nano balls of cuprous oxide - Google Patents
The preparation method of monodisperse uniform morphology Nano balls of cuprous oxide Download PDFInfo
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- CN108975381A CN108975381A CN201810994064.6A CN201810994064A CN108975381A CN 108975381 A CN108975381 A CN 108975381A CN 201810994064 A CN201810994064 A CN 201810994064A CN 108975381 A CN108975381 A CN 108975381A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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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Abstract
The invention discloses a kind of preparation methods of monodisperse uniform morphology Nano balls of cuprous oxide, belong to field of nano material preparation.By a certain amount of copper source CuSO4Mixed solution is formed in deionized water with alkali source NaF dissolution, appropriate reducing agent ascorbic acid is then added, after reacting a period of time, product obtains monodisperse uniform morphology Nano balls of cuprous oxide through centrifugation, washing, drying.Synthetic method of the invention is not necessarily to pyroreaction kettle without adding highly basic, organic basic solvent and any surfactant, has the characteristics that Nano balls of cuprous oxide pattern at low cost, simple to operation and obtained is uniform, good dispersion.
Description
Technical field
The present invention relates to field of nano material preparation, especially one kind to be restored using NaF as alkali source using ascorbic acid
CuSO4Method obtain monodisperse uniform morphology Nano balls of cuprous oxide method.
Background technique
Cuprous oxide is shown excellent for a kind of important p-type transition metal oxide in fields such as catalysis, air-sensitive, electricity
Different physical and chemical performance is therefore widely used in the key areas such as photochemical catalyst, gas-sensitive sensing element and solar battery.
The application performance of cuprous oxide and its pattern and structure are closely related.Uniform morphology Nano balls of cuprous oxide because its compared with
Good pattern integrity degree, higher performance degree of repeatability and paid close attention to by researcher.The system of uniform morphology Nano balls of cuprous oxide
The standby hot spot for becoming Recent study.For example, Wang Jigan (CN105692679B) is to the copper-bath containing histidine polypeptide
In be slowly added dropwise sodium hydroxide solution, after standing reaction, ascorbic acid solution is added and obtains cuprous oxide after reaction and receives
Rice grain.Zhao Wenjie (CN105621473B) is successively added strong using mantoquita, highly basic, reducing agent as raw material in copper salt solution
Aqueous slkali and reducing agent solution and prepare, the molar ratio of control copper ion, hydroxide ion, reducing agent, hydroxide ion plus
The addition rate for entering rate and reducing agent, has obtained the nano cuprous oxide of uniform particle sizes, regular appearance.He Wei
(CN104591256B) a kind of method that cuprous oxide is prepared under copper chloride system is disclosed, this method is first to adjust copper chloride
The concentration and pH value of solution, then certain density sulphite and villaumite mixed solution are prepared, by copper chloride solution and mixed liquor
Preheating, then mixed liquor is slowly added into copper chloride solution and is reacted, and lye control reacting liquid pH value is added dropwise, after reaction, obtain
To cuprous oxide powder.Wu Ling (CN104477969A) is using copper acetate does raw material, N-N dimethylformamide makees solvent, poly- second
Alkene pyrrolidone does dispersing agent, sodium borohydride makees reducing agent, and regulation reaction temperature prepares spherical cuprous oxide nano particle.
As it can be seen that having the preparation report for monodisperse uniform morphology Nano balls of cuprous oxide in the prior art, but existing
The alkali source added in report is mostly highly basic or the organic basic solvent for relying on high temperature, and needs to add a certain amount of surface-active
Agent.
Summary of the invention
It is an object of the invention to: for the state of the art of above-mentioned monodisperse uniform morphology Nano balls of cuprous oxide, provide
A kind of preparation method of monodisperse uniform morphology Nano balls of cuprous oxide, method is simple, and operation is easy, and production cost is low, is not necessarily to
Highly basic, organic basic solvent and surfactant are added, pyroreaction kettle is not necessarily to.
The technical solution of the invention is as follows: using NaF as alkali source, restoring CuSO using ascorbic acid4Method obtain it is single
Disperse uniform morphology Nano balls of cuprous oxide.
Specific step is as follows for the preparation method of monodisperse uniform morphology Nano balls of cuprous oxide of the invention:
(1) room temperature configures certain density CuSO4Aqueous solution；According to preset NaF, ascorbic acid and CuSO4Mole
Than to CuSO4NaF and ascorbic acid are added in aqueous solution, stirs to get clarification mixed solution, mixing speed be set as 300 turns/
Point；
(2) above-mentioned mixed solution is heated to certain reaction temperature, and after being kept for one section of reaction time, by products therefrom carry out from
The heart, washing, drying are to get monodisperse uniform morphology Nano balls of cuprous oxide.
Wherein, in step (1), the CuSO4The concentration of aqueous solution is 0. 005 ~ 0.015 mol/L.
Wherein, in step (1), the preset NaF, ascorbic acid and CuSO4Molar ratio be (3 ~ 6): 2.5:
1。
Wherein, in step (2), the reaction temperature is 30 ~ 70 DEG C.
Wherein, in step (2), the reaction time is 0.5 ~ 2 h.
The principle of the present invention is: at room temperature, NaF, ascorbic acid and CuSO4After solution mixing, because lacking alkali in system
Degree, ascorbic acid do not have CuSO4It is reduced into the ability of cuprous oxide, so clarification mixed solution is formed after three's mixing；
In a heated condition, with the raising of reaction temperature, F in NaF-Slowly hydrolysis shape goes out OH-, step up the alkali in mixed solution
Degree just forms the cuprous nucleus of the initial oxidation being reduced out after basicity is more than certain critical value in the solution；Because of NaF
Hydrolysis rate is slow, the OH that sequential hydrolysis is formed-With CuSO4In conjunction with rear, the cuprous oxide atom being reduced into just is deposited on initial oxygen
Change the surface of cuprous nucleus；With the extension of reaction time, the cuprous nucleus of initial oxidation is gradually grown up, and it is equal to ultimately form monodisperse
One pattern Nano balls of cuprous oxide.
The beneficial effects of the present invention are:
1, using NaF as alkali source, using simple ascorbic acid reducing process, a step just obtains monodisperse uniform morphology cuprous oxide
Nanosphere, uniform particle diameter, about 800 nm, product purity is high, good dispersion.
2, synthetic method of the invention simplifies working condition, living without adding highly basic, organic basic solvent and any surface
Property agent, be not necessarily to pyroreaction kettle, production cost is low, operation be easy, realize monodisperse uniform morphology Nano balls of cuprous oxide rule
Modelling industrial production.
Detailed description of the invention
The scanning electron microscopic picture of Fig. 1 monodisperse uniform morphology Nano balls of cuprous oxide.
Specific embodiment
Technical solution of the invention is further illustrated below with reference to embodiment, but is not to be construed as to technical solution
Limitation.
Embodiment 1: monodisperse uniform morphology Nano balls of cuprous oxide is prepared according to following steps
(1) room temperature, configuration concentration are the CuSO of 0. 005mol/L4Aqueous solution；According to preset NaF, ascorbic acid and
CuSO4Molar ratio 3:2.5:1, to CuSO4NaF and ascorbic acid are added in aqueous solution, stirs to get clarification mixed solution, stirs
It mixes speed and is set as 300 revs/min；
(2) above-mentioned mixed solution is heated to 30 DEG C of reaction temperature, and after keeping 2 h of reaction time, by products therefrom carry out from
The heart, washing, drying are to get monodisperse uniform morphology Nano balls of cuprous oxide.
Embodiment 2: monodisperse uniform morphology Nano balls of cuprous oxide is prepared according to following steps
(1) room temperature, configuration concentration are the CuSO of 0.01mol/L4Aqueous solution；According to preset NaF, ascorbic acid and
CuSO4Molar ratio 4.5:2.5:1, to CuSO4NaF and ascorbic acid are added in aqueous solution, stirs to get clarification mixed solution,
Mixing speed is set as 300 revs/min；
(2) above-mentioned mixed solution is heated to 50 DEG C of reaction temperature, and after keeping 1.25 h of reaction time, products therefrom is carried out
Centrifugation, washing, drying are to get monodisperse uniform morphology Nano balls of cuprous oxide.
Embodiment 3: monodisperse uniform morphology Nano balls of cuprous oxide is prepared according to following steps
(1) room temperature, configuration concentration are the CuSO of 0.015 mol/L4Aqueous solution；According to preset NaF, ascorbic acid and
CuSO4Molar ratio 6:2.5:1, to CuSO4NaF and ascorbic acid are added in aqueous solution, stirs to get clarification mixed solution, stirs
It mixes speed and is set as 300 revs/min；
(2) above-mentioned mixed solution is heated to 70 DEG C of reaction temperature, and after keeping reaction time 0.5h, by products therefrom carry out from
The heart, washing, drying are to get monodisperse uniform morphology Nano balls of cuprous oxide.
The scanning electron microscopic picture of the resulting monodisperse uniform morphology Nano balls of cuprous oxide of embodiment 1-3 is as shown in Figure 1.
Claims (6)
1. the preparation method of monodisperse uniform morphology Nano balls of cuprous oxide, it is characterised in that: using NaF as alkali source, using anti-bad
Hematic acid restores CuSO4Method obtain monodisperse uniform morphology Nano balls of cuprous oxide.
2. the preparation method of monodisperse uniform morphology Nano balls of cuprous oxide according to claim 1, it is characterised in that it
Specific step is as follows:
Room temperature configures certain density CuSO4Aqueous solution；According to preset NaF, ascorbic acid and CuSO4Molar ratio,
To CuSO4NaF and ascorbic acid are added in aqueous solution, stirs to get clarification mixed solution, mixing speed is set as 300 revs/min；
Above-mentioned mixed solution is heated to certain reaction temperature, and after being kept for one section of reaction time, by gained product carry out from
The heart, washing, drying are to get monodisperse uniform morphology Nano balls of cuprous oxide.
3. the preparation method of monodisperse uniform morphology Nano balls of cuprous oxide according to claim 2, it is characterised in that: step
Suddenly in (1), the CuSO4The concentration of aqueous solution is 0. 005 ~ 0.015 mol/L.
4. the preparation method of monodisperse uniform morphology Nano balls of cuprous oxide according to claim 2, it is characterised in that: step
Suddenly in (1), the preset NaF, ascorbic acid and CuSO4Molar ratio be (3 ~ 6): 2.5:1.
5. the preparation method of monodisperse uniform morphology Nano balls of cuprous oxide according to claim 2, it is characterised in that: step
Suddenly in (2), the reaction temperature is 30 ~ 70 DEG C.
6. the preparation method of monodisperse uniform morphology Nano balls of cuprous oxide according to claim 2, it is characterised in that: step
Suddenly in (2), the reaction time is 0.5 ~ 2 h.
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| CN201810994064.6A CN108975381B (en) | 2018-08-29 | 2018-08-29 | Preparation method of monodisperse cuprous oxide nanospheres with uniform morphology |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805010A (en) * | 2010-04-02 | 2010-08-18 | 青岛科技大学 | Method for preparing hollow sphere made from cuprous oxide |
| JP2010534186A (en) * | 2007-07-25 | 2010-11-04 | エルジー・ケム・リミテッド | Spherical cuprous oxide aggregate particle composition and method for producing the same |
| CN107473257A (en) * | 2016-06-07 | 2017-12-15 | 中国科学院化学研究所 | Controllable cuprous nano crystalline substance of a kind of pattern, size and its preparation method and application |
| WO2018119543A1 (en) * | 2016-12-29 | 2018-07-05 | Pontificia Universidad Catolica De Chile | Method for producing a cu2o/tio2 nanoparticle catalyst, and cu2o/tio2 nanoparticle catalyst |
-
2018
- 2018-08-29 CN CN201810994064.6A patent/CN108975381B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010534186A (en) * | 2007-07-25 | 2010-11-04 | エルジー・ケム・リミテッド | Spherical cuprous oxide aggregate particle composition and method for producing the same |
| CN101805010A (en) * | 2010-04-02 | 2010-08-18 | 青岛科技大学 | Method for preparing hollow sphere made from cuprous oxide |
| CN107473257A (en) * | 2016-06-07 | 2017-12-15 | 中国科学院化学研究所 | Controllable cuprous nano crystalline substance of a kind of pattern, size and its preparation method and application |
| WO2018119543A1 (en) * | 2016-12-29 | 2018-07-05 | Pontificia Universidad Catolica De Chile | Method for producing a cu2o/tio2 nanoparticle catalyst, and cu2o/tio2 nanoparticle catalyst |
Non-Patent Citations (2)
| Title |
|---|
| 张迎迎 等: "不同形貌纳米Cu2O的制备", 《淮阴师范学院学报（自然科学版）》 * |
| 王正远: "《化工产品购销手册》", 28 February 2002, 中国物资出版社出版发行 * |
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