CN110577234A - Preparation method of nano cuprous oxide - Google Patents
Preparation method of nano cuprous oxide Download PDFInfo
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- CN110577234A CN110577234A CN201911053631.9A CN201911053631A CN110577234A CN 110577234 A CN110577234 A CN 110577234A CN 201911053631 A CN201911053631 A CN 201911053631A CN 110577234 A CN110577234 A CN 110577234A
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- cuprous oxide
- nano cuprous
- methanol
- copper
- alkali
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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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Abstract
A preparation method of nano cuprous oxide comprises the following steps: (1) adding a certain amount of methanol solution into soluble copper salt serving as a raw material, and fully stirring; adding a certain amount of alkali, and continuously and fully stirring; (2) and transferring the liquid and the solid obtained in the last step into a hydrothermal kettle, keeping the temperature for a period of time at a certain temperature, cooling to room temperature, filtering to obtain brick-red precipitates, cleaning the precipitates with distilled water and ethanol, and drying in vacuum to obtain the nano cuprous oxide. The invention prepares the nano cuprous oxide powder by the methanol thermal method, the raw materials are cheap and easy to obtain, the organic product is mainly sodium formate, the unreacted methanol and the corresponding acid salt of the product can be recycled, the production cost is low, and the industrial production is easy to realize.
Description
Technical Field
The invention relates to a preparation method of nano cuprous oxide, belonging to the technical field of nano material preparation.
Background
Cuprous oxide as a p-type semiconductor material has the advantages of narrow band gap, no toxicity and the like, is widely applied to the fields of solar energy conversion, batteries, sensors and the like, and has wide application prospect.
the polyhydric alcohol thermal method is a preparation method of cuprous oxide, and is characterized in that polyhydric alcohol is used as a solvent and a reducing agent, and heating is carried out to a certain temperature to reduce divalent copper ions to prepare nano cuprous oxide. For example, in the publication No. 106315662A, a glucose solution is used as a reducing agent, and the nano cuprous oxide is prepared by heating, and the cuprous oxide can also be prepared by thermal reduction of ethylene glycol (materials chemistry and Physics, 2009,114: 213-; Crystal Growth & Design 2007, 7: 453-.
Disclosure of Invention
The invention aims to provide a method for preparing nano cuprous oxide aiming at the defects of preparing nano cuprous oxide by a polyol thermal method.
The technical scheme of the invention is that the preparation method of the nano cuprous oxide comprises the following specific steps:
(1) Adding a certain amount of methanol solution into soluble copper salt serving as a raw material, and fully stirring; adding a certain amount of alkali, and continuously and fully stirring;
(2) Transferring the liquid and solid obtained in step (1) to a hydrothermal kettle at 100 deg.COC to 150Oand C, keeping the temperature for 2 to 12 hours, cooling to room temperature, filtering to obtain brick red precipitates, cleaning the precipitates with distilled water and ethanol, and drying in vacuum to obtain nano cuprous oxide powder.
The soluble copper salt is one or a mixture of copper sulfate, copper nitrate, copper chloride and copper acetate.
the alkali is one or a mixture of more of sodium hydroxide, potassium hydroxide, sodium carbonate or potassium carbonate.
the mol ratio of the bivalent copper ions in the soluble copper salt to the methanol is 1: 100-1: 5.
The mol ratio of the bivalent copper ions and the alkali in the soluble copper salt is 1: 20-1: 5.
The vacuum drying temperature is 30-60 ℃, and the drying time is as follows: 12-36 h.
The XRD pattern of nano-cuprous oxide prepared by methanothermic process is shown in fig. 2, and diffraction peaks appear at diffraction angles of 29.6, 36.4, 42.3, 61.3, 73.5, and 77.3 degrees, which indicates that the substance prepared by methanothermic process is nano-cuprous oxide.
The method has the beneficial effects that the nano cuprous oxide powder is prepared by the methanol thermal method, the raw materials are cheap and easy to obtain, the organic product is mainly sodium formate, unreacted methanol and the corresponding acid salt of the product can be recycled, and the production cost is low. The generated cuprous oxide is easy to separate and collect, the preparation method and the process are simple, and the industrial production is easy to realize.
Drawings
FIG. 1 is a flow chart of the preparation method of nano cuprous oxide of the present invention;
Fig. 2 is an XRD pattern of nano-cuprous oxide prepared by methanothermic process, which shows diffraction peaks at diffraction angles of 29.6, 36.4, 42.3, 61.3, 73.5, and 77.3 degrees, indicating that the substance prepared by methanothermic process is nano-cuprous oxide.
Detailed Description
The specific embodiment of the present invention is shown in fig. 1.
Example 1:
(1) 0.01mol of blue vitriol is taken and added into 80ml of methanol, and the mixture is fully stirred for 0.5h, added with 3.0g of NaOH and stirred for 1 h.
(2) The mixed liquid and solid obtained above are transferred to a hydrothermal kettle in an oven 140OAnd C, keeping for 8 hours, and cooling to the normal temperature.
(3) Filtering the mixed liquid and solid in the reaction kettle to obtain brick red solid, washing with water and ethanol, and purifying by 40Oand C, vacuum drying for 24 hours to obtain the nano cuprous oxide powder.
Example 2:
(1) 0.01mol of copper acetate is taken and added into 60ml of methanol, and the mixture is fully stirred for 0.5h, added with 2.0 g of NaOH and stirred for 1 h.
(2) The mixed liquid and solid obtained above were transferred to a hydrothermal kettle in an oven 150OAnd C, keeping for 2 hours, and cooling to the normal temperature.
(3) Filtering the mixed liquid and solid in the reaction kettle to obtain brick red solid, washing with water and ethanol, and washing with 50% ethanolOAnd C, vacuum drying for 12 hours to obtain the nano cuprous oxide powder.
Example 3:
(1) 0.01mol of copper chloride is taken and added into 50ml of methanol, the mixture is fully stirred for 0.5h, 1.5 g of NaOH is added, and the mixture is stirred for 1 h.
(2) the mixed liquid and solid obtained above are transferred to a hydrothermal kettle and placed in an oven 130OKeeping the temperature for 10 hours under the condition C, and cooling to the normal temperature.
(3) Filtering the mixed liquid and solid in the reaction kettle to obtain brick red solid, washing with water and ethanol, and washing with ethanol for 30 daysOAnd C, vacuum drying for 36 hours to obtain nano cuprous oxide powder.
Example 4:
(1) 0.01mol of copper nitrate is taken and added into 40ml of methanol, the mixture is fully stirred for 0.5h, 1.0g of NaOH is added, and the mixture is stirred for 1 h.
(2) The mixed liquid and solid obtained above are transferred to a hydrothermal kettle and placed in an oven 120OKeeping the temperature for 10 hours under the condition C, and cooling to the normal temperature.
(3) filtering the mixed liquid and solid in the reaction kettle to obtain brick red solid, washing with water and ethanol, and purifying by 40OAnd C, vacuum drying for 24 hours to obtain the nano cuprous oxide powder.
Example 5:
(1) 0.005mol of copper chloride and 0.005mol of copper sulfate are taken and added into 70ml of methanol, and the mixture is fully stirred for 0.5h, added with 2.5g of NaOH and stirred for 1 h.
(2) The mixed liquid and solid obtained above are transferred to a hydrothermal kettle in an oven 140Oand C, keeping for 8 hours, and cooling to the normal temperature.
(3) filtering the mixed liquid and solid in the reaction kettle to obtain brick red solid, washing with water and ethanol, and washing with ethanol for 30 daysOAnd C, vacuum drying for 36 hours to obtain nano cuprous oxide powder.
Example 6:
(1) 0.005mol of copper chloride and 0.005mol of copper acetate are taken and added into 50ml of methanol, and the mixture is fully stirred for 0.5h, added with 1.8g of NaOH and stirred for 1 h.
(2) The mixed liquid and solid obtained above are transferred to a hydrothermal kettle and placed in an oven 130OAnd C, keeping for 12 hours, and cooling to the normal temperature.
(3) Filtering the mixed liquid and solid in the reaction kettle to obtain brick red solid, washing with water and ethanol, and purifying by 40OAnd C, vacuum drying for 30 hours to obtain the nano cuprous oxide powder.
Example 7:
(1) 0.005mol of copper nitrate and 0.005mol of copper sulfate were added to 50ml of methanol, and stirred sufficiently for 0.5 hour, 2.4g of NaOH was added thereto, and stirred for 1 hour.
(2) The mixed liquid and solid obtained above were transferred to a hydrothermal kettle in an oven 150OAnd C, keeping for 4 hours, and cooling to the normal temperature.
(3) Filtering the mixed liquid and solid in the reaction kettle to obtain brick red solid, washing with water and ethanol, and purifying by 40OAnd C, vacuum drying for 24 hours to obtain the nano cuprous oxide powder.
Example 8:
(1) 0.005mol of copper chloride, 0.005mol of copper sulfate and 0.005mol of copper acetate are taken and added into 80ml of methanol, and the mixture is fully stirred for 0.5h, added with 3.0g of NaOH and stirred for 1 h.
(2) The mixed liquid and solid obtained above are transferred to a hydrothermal kettle in an oven 140OAnd C, keeping for 12 hours, and cooling to the normal temperature.
(3) Filtering the mixed liquid and solid in the reaction kettle to obtain brick red solid, washing with water and ethanol, and washing with 45% ethanolOAnd C, vacuum drying for 30 hours to obtain the nano cuprous oxide powder.
Claims (5)
1. The preparation method of nano cuprous oxide is characterized by preparing nano cuprous oxide by a methanol thermal method, and comprises the following steps:
(1) Adding a certain amount of methanol solution into soluble copper salt serving as a raw material, and fully stirring; adding a certain amount of alkali, and continuously and fully stirring;
(2) Transferring the liquid and solid obtained in step (1) to a hydrothermal kettle at 100 deg.COC to 150OAnd C, keeping the temperature for 2 to 12 hours, cooling to room temperature, filtering to obtain brick red precipitates, cleaning the precipitates with distilled water and ethanol, and drying in vacuum to obtain the nano cuprous oxide.
2. the method for preparing nano cuprous oxide according to claim 1, wherein said soluble copper salt is one or more selected from copper sulfate, copper nitrate, copper chloride and copper acetate.
3. The method for preparing nano cuprous oxide according to claim 1, wherein said alkali is one or more of sodium hydroxide, potassium hydroxide, sodium carbonate or potassium carbonate.
4. The method for preparing nano cuprous oxide according to claim 1, wherein the mole ratio of cupric ion in said soluble cupric salt to methanol is 1: 100-1: 5.
5. The method for preparing nano cuprous oxide according to claim 1, wherein the mole ratio of cupric ion to alkali in said cupric salt is 1: 20-1: 5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811317995.9A CN109133146A (en) | 2018-11-07 | 2018-11-07 | A kind of preparation method of nano cuprous oxide |
| CN2018113179959 | 2018-11-07 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113403134A (en) * | 2021-06-23 | 2021-09-17 | 江西省科学院能源研究所 | Copper wire drawing oil waste liquid treatment method |
| CN113683115A (en) * | 2021-09-01 | 2021-11-23 | 深圳市动盈先进材料有限公司 | Preparation method of semiconductor material for 5G signal transmission |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110039069B (en) * | 2019-05-30 | 2021-05-14 | 江西省科学院能源研究所 | Spongy micron copper powder and preparation method thereof |
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- 2018-11-07 CN CN201811317995.9A patent/CN109133146A/en active Pending
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2019
- 2019-10-31 CN CN201911053631.9A patent/CN110577234A/en active Pending
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| WO2014109722A1 (en) * | 2013-01-14 | 2014-07-17 | Kaya Cengiz | A method for production and coating of antibacterial copper (ii) oxide (cuo) nano-tube |
| CN103435089A (en) * | 2013-07-16 | 2013-12-11 | 上海应用技术学院 | Spherical cuprous oxide micro-nano particles with roughness surface and preparation method thereof |
| CN105439191A (en) * | 2014-09-28 | 2016-03-30 | 天津工业大学 | Method for preparing core-shell-like cuprous oxide microspheres |
| CN104760988A (en) * | 2015-03-11 | 2015-07-08 | 白晓光 | Environmental-protective preparation method of Cu2O and CuCl |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113403134A (en) * | 2021-06-23 | 2021-09-17 | 江西省科学院能源研究所 | Copper wire drawing oil waste liquid treatment method |
| CN113403134B (en) * | 2021-06-23 | 2022-05-20 | 江西省科学院能源研究所 | Copper wire drawing oil waste liquid treatment method |
| CN113683115A (en) * | 2021-09-01 | 2021-11-23 | 深圳市动盈先进材料有限公司 | Preparation method of semiconductor material for 5G signal transmission |
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