CN109095492B - Preparation method of octahedral cuprous oxide micron crystal with uniform morphology - Google Patents
Preparation method of octahedral cuprous oxide micron crystal with uniform morphology Download PDFInfo
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- CN109095492B CN109095492B CN201810995205.6A CN201810995205A CN109095492B CN 109095492 B CN109095492 B CN 109095492B CN 201810995205 A CN201810995205 A CN 201810995205A CN 109095492 B CN109095492 B CN 109095492B
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- cuprous oxide
- boric acid
- ascorbic acid
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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
- 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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/41—Particle morphology extending in three dimensions octahedron-like
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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
Abstract
The invention discloses a preparation method of cuprous oxide microcrystals with uniform octahedron morphology, and belongs to the field of micro-nano material preparation. Dissolving a certain amount of cupric salt and boric acid serving as a structure directing agent in deionized water to form a mixed solution, then adding a proper amount of ascorbic acid serving as a reducing agent, and centrifuging, washing and drying a product to obtain the cuprous oxide micron crystal with the uniform octahedron morphology. The synthesis method provided by the invention is simple to operate and short in reaction time, and the prepared octahedral cuprous oxide is uniform in particle size and good in dispersibility.
Description
Technical Field
The invention relates to the field of micro-nano material preparation, in particular to a preparation method for synthesizing octahedral cuprous oxide microcrystals with uniform morphology by using boric acid as a structure directing agent.
Background
Cuprous oxide is an important p-type transition metal oxide, and shows excellent physical and chemical properties in the fields of catalysis, gas sensitivity, electricity and the like, so the cuprous oxide is widely applied to important fields of photocatalysts, gas-sensitive sensing elements, solar cells and the like.
The application performance of the cuprous oxide is closely related to the shape and the structure of the cuprous oxide. In recent years, the synthesis of cuprous oxide materials with different morphologies, especially cuprous oxide materials with a polyhedral structure, has received wide attention from people. Dissolving inorganic copper salt in a solvent, adding an additive, adding an alkaline substance, adding a reducing agent, reacting for 0.5-6h at the temperature of 30-90 ℃, and washing and drying the obtained product to obtain the hexacosanhedral cuprous oxide material. The method comprises the steps of taking copper acetate as a copper source and tartaric acid as a reducing agent, adding the copper acetate and the tartaric acid into an acetic acid/sodium acetate buffer solution with a proper concentration, adding a potassium carbonate solution with a certain concentration while stirring, stirring at room temperature for 3-9 hours, filtering, and standing and evaporating at room temperature by using a normal-temperature crystallization technology to obtain the octahedral cuprous oxide crystal. Dissolving copper oxide powder in ammonia water and ammonium salt solution by using Liu' ei Feng (CN 105536791B), mixing the solution with ethylene glycol, carrying out solvothermal reaction under the action of strong alkali, separating and washing a product, and carrying out vacuum drying treatment to obtain the octahedral cuprous oxide. Therefore, the technical process is more complex and fussy in the report of the polyhedral cuprous oxide crystal in the prior art.
Disclosure of Invention
The invention aims to: the preparation method of the cuprous oxide micron crystal with the octahedron uniform morphology is provided, the production conditions are simplified, the cost is low, the process is simple, the reaction time is short, and the large-scale industrial production of the cuprous oxide micron crystal with the octahedron uniform morphology is realized.
The technical solution of the invention is as follows: boric acid is used as a structure directing agent, and cuprous oxide micron crystals with octahedron uniform morphology are obtained by using a method of reducing divalent copper salt by ascorbic acid.
The preparation method of the cuprous oxide micron crystal with the octahedral uniform morphology comprises the following specific steps:
(1) adding boric acid into a cupric salt aqueous solution with a certain concentration at a set reaction temperature, and stirring to obtain a clear mixed solution;
(2) ascorbic acid is added into the mixed solution at one time, the molar ratio of the boric acid, the cupric salt and the ascorbic acid is controlled, and the whole reaction process is carried out under the stirring of 300 r/min; after reacting for a period of time, centrifuging, washing and drying the obtained product to obtain the cuprous oxide micron crystal with the octahedron uniform appearance.
Wherein, in the step (1), the set reaction temperature range is 20-50 ℃.
Wherein in the step (1), the cupric salt is copper sulfate, copper chloride, copper acetate or copper nitrate.
Wherein, in the step (1), the concentration of the cupric salt aqueous solution is 0.01-0.02 mol/L.
In the step (2), the molar ratio of the boric acid to the cupric salt to the ascorbic acid is 2-8: 1: 2.5.
Wherein in the step (2), the reaction time is 20-60 min.
The invention has the beneficial effects that:
1. cheap boric acid is used as a structure directing agent, and a simple ascorbic acid reduction process is adopted to obtain the octahedral cuprous oxide micron crystal with uniform morphology in one step, and the octahedral cuprous oxide micron crystal has uniform particle size, high product purity and good dispersibility.
2. The method has simple process and required production equipment, is simple and convenient to operate, and is suitable for large-scale industrial production.
Drawings
FIG. 1 is a scanning electron microscope picture of cuprous oxide microcrystals with octahedron uniform morphology.
Detailed Description
The following structural examples further illustrate the technical solution of the present invention, but are not to be understood as limiting the technical solution.
Example 1: the octahedral cuprous oxide micron crystal with uniform morphology is prepared according to the following steps
(1) Setting the reaction temperature to be 20 ℃, adding boric acid into a copper sulfate aqueous solution with the concentration of 0.01 mol/L, and stirring to obtain a clear mixed solution;
(2) ascorbic acid is added into the mixed solution at one time, the molar ratio of the boric acid to the cupric salt to the ascorbic acid is controlled to be 2:1:2.5, and the whole reaction process is carried out under the stirring of 300 r/min; after reacting for 60 min, centrifuging, washing and drying the obtained product to obtain the cuprous oxide micron crystal with the octahedron uniform appearance.
Example 2: the octahedral cuprous oxide micron crystal with uniform morphology is prepared according to the following steps
(1) Setting the reaction temperature to be 30 ℃, adding boric acid into a copper chloride aqueous solution with the concentration of 0.015 mol/L, and stirring to obtain a clear mixed solution;
(2) ascorbic acid is added into the mixed solution at one time, the molar ratio of the boric acid to the cupric salt to the ascorbic acid is controlled to be 5:1:2.5, and the whole reaction process is carried out under the stirring of 300 r/min; after reacting for 40 min, centrifuging, washing and drying the obtained product to obtain the cuprous oxide micron crystal with the octahedron uniform appearance.
Example 3: the octahedral cuprous oxide micron crystal with uniform morphology is prepared according to the following steps
(1) Setting the reaction temperature to 40 ℃, adding boric acid into a copper acetate aqueous solution with the concentration of 0.02 mol/L, and stirring to obtain a clear mixed solution;
(2) ascorbic acid is added into the mixed solution at one time, the molar ratio of the boric acid to the cupric salt to the ascorbic acid is controlled to be 8:1:2.5, and the whole reaction process is carried out under the stirring of 300 r/min; after reacting for 20min, centrifuging, washing and drying the obtained product to obtain the cuprous oxide micron crystal with the octahedron uniform appearance.
Example 4: the octahedral cuprous oxide micron crystal with uniform morphology is prepared according to the following steps
(1) Setting the reaction temperature to 50 ℃, adding boric acid into a copper nitrate aqueous solution with the concentration of 0.018 mol/L, and stirring to obtain a clear mixed solution;
(2) ascorbic acid is added into the mixed solution at one time, the molar ratio of the boric acid to the cupric salt to the ascorbic acid is controlled to be 6:1:2.5, and the whole reaction process is carried out under the stirring of 300 r/min; after reacting for 50 min, centrifuging, washing and drying the obtained product to obtain the cuprous oxide micron crystal with the octahedron uniform appearance.
The scanning electron microscope pictures of the octahedral cuprous oxide micro-crystals with uniform morphology obtained in examples 1-4 are shown in FIG. 1.
Claims (1)
1. The preparation method of the cuprous oxide micron crystal with the octahedron uniform morphology is characterized by comprising the following steps of: boric acid is used as a structure directing agent, and cuprous oxide micron crystals with octahedral uniform morphology are obtained by using a method of reducing divalent copper salt by ascorbic acid; the method comprises the following specific steps:
step (1), adding boric acid into a cupric salt aqueous solution with a certain concentration at a set reaction temperature, and stirring to obtain a clear mixed solution; the set reaction temperature is 20-50 ℃; the cupric salt is copper sulfate, copper chloride, copper acetate or copper nitrate; the concentration of the cupric salt water solution is 0.01-0.02 mol/L;
step (2), ascorbic acid is added into the mixed solution at one time, the molar ratio of the boric acid, the cupric salt and the ascorbic acid is controlled, and the whole reaction process is carried out under the stirring of 300 r/min; after reacting for a period of time, centrifuging, washing and drying the obtained product to obtain cuprous oxide micron crystals with octahedron uniform morphology; the molar ratio of the boric acid to the cupric salt to the ascorbic acid is 2-8: 1: 2.5; the reaction time is 20-60 min.
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| CN103172104B (en) * | 2013-04-03 | 2015-05-13 | 浙江理工大学 | Preparation method of nano cuprous oxide |
| WO2016020759A1 (en) * | 2014-08-04 | 2016-02-11 | King Abdullah University Of Science And Technology | Catalytic structures and methods of generating hydrogen gas |
| CN105621473B (en) * | 2014-11-06 | 2017-11-14 | 中国科学院宁波材料技术与工程研究所 | The preparation method and pattern and size control method of nano cuprous oxide particle |
| CN105536791B (en) * | 2015-12-30 | 2018-06-29 | 河北工程大学 | The preparation method of the octahedra cuprous oxide catalysis agent of synthesizing methyl-chloro-silane monomer |
| CN105731518B (en) * | 2016-01-19 | 2017-05-10 | 湖南城市学院 | Normal-temperature crystallization preparation method of octahedron cuprous oxide crystal |
| CN105866098B (en) * | 2016-04-13 | 2019-03-08 | 吉林师范大学 | A kind of Cu2Compound micro particles surface-enhanced Raman scattering activity substrate of O-Au and preparation method thereof |
| CN106673051B (en) * | 2017-01-22 | 2018-04-20 | 郑州轻工业学院 | A kind of preparation method of the super crystalline material of cuprous oxide |
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