CN110642285A - Preparation method of nano cuprous oxide powder - Google Patents
Preparation method of nano cuprous oxide powder Download PDFInfo
- Publication number
- CN110642285A CN110642285A CN201910937939.3A CN201910937939A CN110642285A CN 110642285 A CN110642285 A CN 110642285A CN 201910937939 A CN201910937939 A CN 201910937939A CN 110642285 A CN110642285 A CN 110642285A
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- CN
- China
- Prior art keywords
- cuprous oxide
- oxide powder
- nano cuprous
- steps
- following
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Classifications
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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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- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention relates to a preparation method of nano cuprous oxide powder, which comprises the following steps: adjusting the pH value of a copper salt solution obtained by dissolving soluble copper salt to 7-8, preheating, adding a reducing agent for reaction, adding a dispersing agent to obtain cuprous oxide powder, cleaning the cuprous oxide powder by using a coating agent solution, and drying to obtain the nano cuprous oxide.
Description
Technical Field
The invention relates to preparation of nano oxides, in particular to a preparation method of nano cuprous oxide powder.
Background
The nano cuprous oxide powder has excellent physical and chemical properties and some special properties, so that the application potential is large and the added value is high. The nano cuprous oxide powder is mainly applied to the fields of powder metallurgy, electronic materials, friction materials, oil-retaining bearings, conductive materials, medicines, diamond products, mechanical parts and the like. The function of the capacitor is more indispensable in the field of capacitors.
However, the traditional method for preparing nano-copper oxide powder, such as electrolysis or atomization, produces a product with a large particle size, even up to several microns, which is not suitable for preparing superfine copper powder.
Meanwhile, the existing preparation method of the nano cuprous oxide powder has poor reproducibility, unstable reaction and easy oxidation in the washing process.
Disclosure of Invention
The invention aims to solve the technical problem of avoiding the defects of the prior art and provides a method for preparing nano copper powder, which is stable and suitable for industrial production.
The invention relates to a preparation method of nano cuprous oxide powder, which comprises the following steps:
adjusting the pH value of a copper salt solution obtained by dissolving soluble copper salt to 7-8, preheating, adding a reducing agent for reaction, adding a dispersing agent to obtain cuprous oxide powder, cleaning the cuprous oxide powder by using a coating agent solution, and drying to obtain the nano cuprous oxide;
the dispersant is an onium salt.
The concentration of the onium salt is 5-8 g/L.
The soluble copper salt is one selected from copper sulfate, copper chloride, copper nitrate or copper bromide.
The concentration of copper ions in the copper salt solution is 0.1-3.0 mol/L.
The preheating temperature is 30-120 ℃.
Adjusting the pH value of the copper salt solution to 7-8 by using an alkali solution; the alkali solution is one selected from ammonia water, sodium hydroxide and potassium hydroxide; the depth of the alkali liquor is 10-45 wt%; the mass ratio of the alkali liquor to the copper salt solution is 1: 3-6.
The reducing agent is selected from one of hydrazine hydrate, ascorbic acid or malic acid; the concentration of the reducing agent is 60-90 wt%; the mass ratio of the reducing agent to the copper salt solution is 1: 3-8.
The coating agent is 2, 6-di-tert-butyl-4-methylphenol. The concentration of the coating agent is 1-4 g/L.
The drying is vacuum drying.
The onium salt is one selected from alkyl trimethyl ammonium salt, pyridinium salt or dialkyl dimethyl ammonium salt.
The grain size of the nano cuprous oxide is 20-100 nm.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method has good reproducibility and stable reaction process, and the prepared nano cuprous oxide powder has stable structure, narrow particle size distribution range and uniform particles.
Detailed Description
Examples
40g of CuSO4·5H2And O, preparing 250ml of copper sulfate solution with the concentration of 0.5mol/L, and preheating the solution to 30 ℃ in a 500ml water bath kettle. Then, 20 wt% of ammonia water is dripped under the condition of stirring to form a blue turbid liquid with a certain concentration, and the mass ratio of the ammonia water to the copper salt is 1: 3. And slowly dropwise adding a reducing agent hydrazine hydrate solution with the weight percent of 80 percent, wherein the molar ratio of the hydrazine hydrate to the copper salt is 1: 6. Then adding 30ml of 6g/L tetramethyl ammonium hydroxide solution, and then preserving the temperature for 2h to obtain brick red powder. And (3) cleaning the brick red powder with 2, 6-di-tert-butyl-4-methylphenol ethanol solution with the concentration of 2.5g/L, and drying in vacuum to obtain the cuprous hydroxide powder.
Claims (10)
1. The preparation method of the nano cuprous oxide powder is characterized by comprising the following steps of:
adjusting the pH value of a copper salt solution obtained by dissolving soluble copper salt to 7-8, preheating, adding a reducing agent for reaction, adding a dispersing agent to obtain cuprous oxide powder, cleaning the cuprous oxide powder by using a coating agent solution, and drying to obtain the nano cuprous oxide;
the dispersant is an onium salt.
2. The method for preparing nano cuprous oxide powder according to claim 1, wherein said method comprises the following steps: the soluble copper salt is one selected from copper sulfate, copper chloride, copper nitrate or copper bromide.
3. The method for preparing nano cuprous oxide powder according to claim 1, wherein said method comprises the following steps: the concentration of copper ions in the copper salt solution is 0.1-3.0 mol/L.
4. The method for preparing nano cuprous oxide powder according to claim 1, wherein said method comprises the following steps: the preheating temperature is 30-120 ℃.
5. The method for preparing nano cuprous oxide powder according to claim 1, wherein said method comprises the following steps: adjusting the pH value of the copper salt solution to 7-8 by using an alkali solution; the alkali solution is one selected from ammonia water, sodium hydroxide and potassium hydroxide; the depth of the alkali liquor is 10-45 wt%; the mass ratio of the alkali liquor to the copper salt solution is 1: 3-6.
6. The method for preparing nano cuprous oxide powder according to claim 1, wherein said method comprises the following steps: the reducing agent is selected from one of hydrazine hydrate, sodium hypophosphite, borohydride, formaldehyde, ascorbic acid or malic acid; the concentration of the reducing agent is 60-90 wt%; the mass ratio of the reducing agent to the copper salt solution is 1: 3-8.
7. The method for preparing nano cuprous oxide powder according to claim 1, wherein said method comprises the following steps: the coating agent is 2, 6-di-tert-butyl-4-methylphenol; the concentration of the coating agent is 1-4 g/L.
8. The method for preparing nano cuprous oxide powder according to claim 1, wherein said method comprises the following steps: the drying is vacuum drying.
9. The method for preparing nano cuprous oxide powder according to claim 1, wherein said method comprises the following steps: the onium salt is one selected from alkyl trimethyl ammonium salt, pyridinium salt or dialkyl dimethyl ammonium salt, and the concentration of the onium salt is 5-8 g/L.
10. The method for preparing nano cuprous oxide powder according to claim 1, wherein said method comprises the following steps: the grain size of the nano cuprous oxide is 20-100 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910937939.3A CN110642285A (en) | 2019-09-30 | 2019-09-30 | Preparation method of nano cuprous oxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910937939.3A CN110642285A (en) | 2019-09-30 | 2019-09-30 | Preparation method of nano cuprous oxide powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110642285A true CN110642285A (en) | 2020-01-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910937939.3A Pending CN110642285A (en) | 2019-09-30 | 2019-09-30 | Preparation method of nano cuprous oxide powder |
Country Status (1)
| Country | Link |
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| CN (1) | CN110642285A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1490439A (en) * | 2003-07-11 | 2004-04-21 | 华中师范大学 | Method for preparing stable nanometer cuprous oxide whiskers with chemical precipitation method |
-
2019
- 2019-09-30 CN CN201910937939.3A patent/CN110642285A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1490439A (en) * | 2003-07-11 | 2004-04-21 | 华中师范大学 | Method for preparing stable nanometer cuprous oxide whiskers with chemical precipitation method |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200103 |