CN112850777B - Preparation method of high-purity nano copper oxide - Google Patents
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Abstract
The invention provides a preparation method of high-purity nano copper oxide, which comprises the following steps: adding a cuprous chloride raw material into hot ammonia water for dissolving, cooling and filtering, adding sodium diisooctyl succinate sulfonate, polyethylene glycol and absolute ethyl alcohol into the obtained filtrate, then adding ethyl acetate for reaction, and filtering to obtain cuprous chloride; preparing a sodium bicarbonate solution, adding cuprous chloride particles, adding sodium diisooctyl succinate sulfonate and polyethylene glycol, then adding urea and hydrogen peroxide, sealing, heating and reacting under high pressure, filtering a reaction product, and drying in vacuum to obtain the high-purity nano copper oxide. The method has simple process and easy operation, and the obtained nano copper oxide has high purity, small crystal grain size, large specific surface area and wide application range.
Description
Technical Field
The invention relates to a preparation method of high-purity nano copper oxide.
Background
The chemical formula of the copper oxide is CuO, the copper oxide is a black oxide of copper, the p-type semiconductor with a narrow band gap of about 1.2 electron volts has the characteristics of good conductivity, photoelectricity, gas sensitivity and the like, and meanwhile, the copper oxide is non-toxic and low in price. The nano copper oxide is different from the conventional copper oxide, and has unique electric, magnetic, optical, chemical and other characteristics due to small grain size and large specific surface area. The nano copper oxide as a novel multifunctional inorganic material has wide application prospect, and can be used for the aspects of high-temperature superconductors, electrochemical sensors, electrode materials, photocatalytic degradation of organic matters, catalytic oxidation of CO, catalytic decomposition of materials such as potassium chlorate, hydrogen peroxide, ammonium perchlorate and the like. The common preparation method of the nano copper oxide powder mainly adopts a liquid phase method and a solid phase method, and the existing preparation method has the disadvantages of complex process, high cost, low production efficiency and poor product dispersibility.
Disclosure of Invention
The invention provides a preparation method of high-purity nano copper oxide, which comprises the following steps: adding a cuprous chloride raw material into hot ammonia water for dissolving, cooling and filtering, adding diisooctyl succinate sodium sulfonate, polyethylene glycol and absolute ethyl alcohol into the obtained filtrate, then adding ethyl acetate, controlling the reaction temperature to be 48+ k1 (the mass fraction of the diisooctyl succinate sodium sulfonate + the mass fraction of the polyethylene glycol) (the volume ratio of the ethyl alcohol to the water), wherein k1 is an adjusting coefficient, carrying out reaction, and filtering to obtain cuprous chloride; preparing a sodium bicarbonate solution, adding cuprous chloride particles, adding sodium diisooctyl succinate sulfonate and polyethylene glycol, then adding urea and hydrogen peroxide, sealing, heating and reacting under high pressure, filtering a reaction product, and drying in vacuum to obtain the high-purity nano copper oxide. The method has simple process and easy operation, and the obtained nano copper oxide has high purity, small crystal grain size, large specific surface area and wide application range.
The specific scheme is as follows:
a preparation method of high-purity nano copper oxide comprises the following steps:
1) adding a cuprous chloride raw material into hot ammonia water for dissolving, cooling to room temperature, filtering, adding diisooctyl succinate sodium sulfonate, polyethylene glycol and absolute ethyl alcohol into the obtained filtrate, wherein the mass ratio of the diisooctyl succinate sodium sulfonate to the polyethylene glycol is 1:1.6, then adding ethyl acetate, controlling the reaction temperature to be 48+ k1 (the mass fraction of the diisooctyl succinate sodium sulfonate + the mass fraction of the polyethylene glycol) (the volume ratio of the ethyl alcohol to the water), wherein k1 is an adjusting coefficient, reacting, and filtering to obtain cuprous chloride;
2) preparing a sodium bicarbonate solution, adding cuprous chloride particles, adding dioctyl sodium sulfosuccinate and polyethylene glycol, then adding urea and hydrogen peroxide, sealing, heating and reacting under high pressure, filtering a reaction product, and drying in vacuum to obtain the high-purity nano copper oxide.
Further, the ammonia water in the step 1 is at a temperature of 45 ℃, the concentration of the ammonia water is 5.0mol/L, and the molar ratio of cuprous chloride in the cuprous chloride raw material to ammonia in the ammonia water is 1: 5.
Further, the mass fraction of the diisooctyl succinate sodium sulfonate in the mixed solution in the step 1 is 0.05-0.06%, the mass fraction of the polyethylene glycol is 0.08-0.096%, and the molecular weight of the polyethylene glycol is 40000-60000.
Further, the volume ratio of the water to the ethanol in the mixed solution in the step 1 is 67:33-70: 30.
Further, the molar ratio of the ethyl acetate to the cuprous ions in the mixed solution in the step 1 is 3.5: 1.
Further, wherein k1 of step 1 is 4.25 x 104。
Further, the mass fraction of the diisooctyl sulfosuccinate in the mixed solution in the step 2 is 0.15%, and the mass fraction of the polyethylene glycol is 0.25%.
Further, the mole number of the urea, the hydrogen peroxide and the cuprous chloride in the mixed solution in the step 2 is 1.2:1.5: 1.
Further, the reaction temperature in the step 2 is 135 ℃, and the pressure is 2.5 atmospheric pressures.
The invention has the following beneficial effects:
1) industrial cuprous chloride is used as a raw material, the raw material is cheap and easy to obtain, the raw material is dissolved by preparing strong ammonia water, then ethyl acetate is utilized to decompose under a heating environment to form acetic acid and ethanol, the acetic acid is combined with ammonium radicals to enable the cuprous chloride to precipitate again, and the concentration of the ethanol and the surfactant in the solution is controlled to control the particle structure of the cuprous chloride to form, so that precursor particles with nanometer size and short rod shape are obtained; under the high-temperature action of sodium bicarbonate, urea and hydrogen peroxide, the urea is used for stabilizing the pH value of the solution, and the hydrogen peroxide oxidizes the cupric oxide under the action of the sodium bicarbonate to form copper oxide particles with consistent appearance;
2) the inventors have found that when the temperature of the hydrothermal reaction and the concentrations of the surfactant and ethanol satisfy a specific relationship, precursor particles having a uniform particle size distribution can be obtained, and copper oxide particles having a uniform particle size distribution and a low impurity content can be obtained.
Drawings
FIG. 1 is a low-magnification SEM electron micrograph of example 1.
FIG. 2 is a high-magnification SEM electron micrograph of example 1.
Detailed Description
The present invention will be described in more detail below with reference to specific examples, but the scope of the present invention is not limited to these examples.
Example 1
(1) Adding cuprous chloride raw material into ammonia water, stirring and dissolving for 1 hour at the temperature of 45 ℃, wherein the concentration of the ammonia water is 5.0mol/L, the molar ratio of cuprous chloride in the cuprous chloride raw material to ammonia in the ammonia water is 1:5, then cooling to 25 ℃, filtering, adding diisooctyl succinate sodium sulfonate, polyethylene glycol with the molecular weight of 50000 and absolute ethyl alcohol into obtained filtrate, so that the mass fraction of the diisooctyl succinate sodium sulfonate in the mixed solution is 0.05%, the mass fraction of the polyethylene glycol is 0.08%, and the volume ratio of water to ethyl alcohol in the mixed solution is 67: 33; then adding ethyl acetate, wherein the molar ratio of the ethyl acetate to the cuprous ions in the mixed solution is 3.5: 1; heating the mixed solution in a hydrothermal device, and controlling the reaction temperature to be 48+4.25 x 104(mass fraction of sodium diisooctyl sulfosuccinate + mass fraction of polyethylene glycol) ((volume ratio of ethanol to water)): 75.2 deg.C, performing hydrothermal reflux reaction for 2 hr, filtering to obtain filter residue, and washing the filter residue with deionized water to obtain cuprous chloride particles;
(2) preparing a sodium bicarbonate solution, adding cuprous chloride particles, pulping, adding diisooctyl succinate sodium sulfonate and polyethylene glycol to enable the mass fraction of the diisooctyl succinate sodium sulfonate in the mixed solution to be 0.15% and the mass fraction of the polyethylene glycol to be 0.25%, then adding urea and hydrogen peroxide, enabling the mole number of the added urea, hydrogen peroxide and cuprous chloride to be 1.2:1.5:1, putting the mixed solution into a sealed kettle, heating to 135 ℃, enabling the pressure to be 2.5 atmospheres, stirring and reacting for 2.5 hours, filtering a reaction product, and washing with deionized water to obtain copper oxide filter residues; and drying the copper oxide filter residue in vacuum to obtain the nano copper oxide.
Example 2
(1) Adding cuprous chloride raw material into ammonia water, stirring and dissolving for 1 hour at the temperature of 45 ℃, wherein the concentration of the ammonia water is 5.0mol/L, the molar ratio of cuprous chloride in the cuprous chloride raw material to ammonia in the ammonia water is 1:5, then cooling to 25 ℃, filtering, adding diisooctyl succinate sodium sulfonate, polyethylene glycol with the molecular weight of 50000 and absolute ethyl alcohol into obtained filtrate, so that the mass fraction of the diisooctyl succinate sodium sulfonate in the mixed solution is 0.06%, the mass fraction of the polyethylene glycol is 0.096%, and the volume ratio of water to ethanol in the mixed solution is 70: 30; then adding ethyl acetate, wherein the molar ratio of the ethyl acetate to the cuprous ions in the mixed solution is 3.5: 1; heating the mixed solution in a hydrothermal device, and controlling the reaction temperature to be 48+4.25 x 104(mass fraction of sodium diisooctyl sulfosuccinate + mass fraction of polyethylene glycol) ((volume ratio of ethanol to water)): 76.4 deg.C, performing hydrothermal reflux reaction for 2 hours, filtering to obtain filter residue, and washing the filter residue with deionized water to obtain cuprous chloride particles;
(2) preparing a sodium bicarbonate solution, adding cuprous chloride particles, pulping, adding diisooctyl succinate sodium sulfonate and polyethylene glycol to ensure that the mass fraction of the diisooctyl succinate sodium sulfonate in the mixed solution is 0.15 percent and the mass fraction of the polyethylene glycol is 0.25 percent after pulping is finished, then adding urea and hydrogen peroxide, wherein the mole number of the added urea, hydrogen peroxide and cuprous chloride is 1.2:1.5:1, placing the mixed solution into a sealed kettle, heating to 135 ℃, keeping the pressure at 2.5 atmospheric pressures, stirring and reacting for 2.5 hours, filtering a reaction product, and washing with deionized water to obtain copper oxide filter residues; and drying the copper oxide filter residue in vacuum to obtain the nano copper oxide.
Example 3
(1) Adding cuprous chloride raw material into ammonia water, stirring and dissolving at 45 ℃ for 1 hour, wherein the concentration of the ammonia water is 5.0mol/L, the molar ratio of cuprous chloride in the cuprous chloride raw material to ammonia in the ammonia water is 1:5, cooling to 25 ℃, filtering, adding the obtained filtrate into sodium diisooctyl sulfosuccinatePolyethylene glycol with the molecular weight of 50000 and absolute ethyl alcohol, so that the mass fraction of the diisooctyl succinate sodium sulfonate in the mixed solution is 0.055%, the mass fraction of the polyethylene glycol is 0.088%, and the volume ratio of water to the ethyl alcohol in the mixed solution is 68: 32; then adding ethyl acetate, wherein the molar ratio of the ethyl acetate to the cuprous ions in the mixed solution is 3.5: 1; heating the mixed solution in a hydrothermal device, and controlling the reaction temperature to be 48+4.25 x 104(mass fraction of sodium diisooctyl sulfosuccinate + mass fraction of polyethylene glycol) ((volume ratio of ethanol to water)): 76.6 deg.C, performing hydrothermal reflux reaction for 2 hours, filtering to obtain filter residue, and washing the filter residue with deionized water to obtain cuprous chloride particles;
(2) preparing a sodium bicarbonate solution, adding cuprous chloride particles, pulping, adding diisooctyl succinate sodium sulfonate and polyethylene glycol to enable the mass fraction of the diisooctyl succinate sodium sulfonate in the mixed solution to be 0.15% and the mass fraction of the polyethylene glycol to be 0.25%, then adding urea and hydrogen peroxide, enabling the mole number of the added urea, hydrogen peroxide and cuprous chloride to be 1.2:1.5:1, putting the mixed solution into a sealed kettle, heating to 135 ℃, enabling the pressure to be 2.5 atmospheres, stirring and reacting for 2.5 hours, filtering a reaction product, and washing with deionized water to obtain copper oxide filter residues; and drying the copper oxide filter residue in vacuum to obtain the nano copper oxide.
Comparative example 1
(1) Adding cuprous chloride raw material into ammonia water, stirring and dissolving for 1 hour at the temperature of 45 ℃, wherein the concentration of the ammonia water is 5.0mol/L, the molar ratio of cuprous chloride in the cuprous chloride raw material to ammonia in the ammonia water is 1:5, then cooling to 25 ℃, filtering, adding diisooctyl succinate sodium sulfonate, polyethylene glycol with the molecular weight of 50000 and absolute ethyl alcohol into obtained filtrate, so that the mass fraction of the diisooctyl succinate sodium sulfonate in the mixed solution is 0.055%, the mass fraction of the polyethylene glycol is 0.088%, and the volume ratio of water to ethyl alcohol in the mixed solution is 68: 32; then adding ethyl acetate, wherein the molar ratio of the ethyl acetate to the cuprous ions in the mixed solution is 3.5: 1; placing the mixed solution in a hydrothermal device, heating the mixed solution, controlling the reaction temperature to be 75.5 ℃, carrying out hydrothermal reflux reaction for 2 hours, then filtering to obtain filter residue, and washing the filter residue with deionized water to obtain cuprous chloride particles;
(2) preparing a sodium bicarbonate solution, adding cuprous chloride particles, pulping, adding diisooctyl succinate sodium sulfonate and polyethylene glycol to enable the mass fraction of the diisooctyl succinate sodium sulfonate in the mixed solution to be 0.15% and the mass fraction of the polyethylene glycol to be 0.25%, then adding urea and hydrogen peroxide, enabling the mole number of the added urea, hydrogen peroxide and cuprous chloride to be 1.2:1.5:1, putting the mixed solution into a sealed kettle, heating to 135 ℃, enabling the pressure to be 2.5 atmospheres, stirring and reacting for 2.5 hours, filtering a reaction product, and washing with deionized water to obtain copper oxide filter residues; and drying the copper oxide filter residue in vacuum to obtain the nano copper oxide.
Comparative example 2
(1) Adding cuprous chloride raw material into ammonia water, stirring and dissolving for 1 hour at the temperature of 45 ℃, wherein the concentration of the ammonia water is 5.0mol/L, the molar ratio of cuprous chloride in the cuprous chloride raw material to ammonia in the ammonia water is 1:5, then cooling to 25 ℃, filtering, adding diisooctyl succinate sodium sulfonate, polyethylene glycol with the molecular weight of 50000 and absolute ethyl alcohol into obtained filtrate, so that the mass fraction of the diisooctyl succinate sodium sulfonate in the mixed solution is 0.055%, the mass fraction of the polyethylene glycol is 0.088%, and the volume ratio of water to ethyl alcohol in the mixed solution is 68: 32; then adding ethyl acetate, wherein the molar ratio of the ethyl acetate to the cuprous ions in the mixed solution is 3.5: 1; placing the mixed solution in a hydrothermal device, heating the mixed solution, controlling the reaction temperature to be 78.0 ℃, carrying out hydrothermal reflux reaction for 2 hours, then filtering to obtain filter residue, and washing the filter residue with deionized water to obtain cuprous chloride particles;
(2) preparing a sodium bicarbonate solution, adding cuprous chloride particles, pulping, adding diisooctyl succinate sodium sulfonate and polyethylene glycol to enable the mass fraction of the diisooctyl succinate sodium sulfonate in the mixed solution to be 0.15% and the mass fraction of the polyethylene glycol to be 0.25%, then adding urea and hydrogen peroxide, enabling the mole number of the added urea, hydrogen peroxide and cuprous chloride to be 1.2:1.5:1, putting the mixed solution into a sealed kettle, heating to 135 ℃, enabling the pressure to be 2.5 atmospheres, stirring and reacting for 2.5 hours, filtering a reaction product, and washing with deionized water to obtain copper oxide filter residues; and drying the copper oxide filter residue in vacuum to obtain the nano copper oxide.
Test and results
The indexes of copper oxide obtained in test examples 1 to 3 and comparative examples 1 to 3 are shown in Table 1. It can be seen that when the reaction temperature does not satisfy the relationship of the present invention, the particle size distribution is not uniform, the tap density is low, or the average particle size is too large, and it is difficult to obtain nano copper oxide having a uniform particle size and a small average particle size.
TABLE 1
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention.
Claims (5)
1. A preparation method of high-purity nano copper oxide comprises the following steps:
1) adding cuprous chloride raw material into hot ammonia water for dissolving, cooling to room temperature, filtering, adding sodium diisooctyl succinate sulfonate, polyethylene glycol and absolute ethyl alcohol into obtained filtrate, wherein the mass ratio of the sodium diisooctyl succinate sulfonate to the polyethylene glycol is 1:1.6, then adding ethyl acetate, controlling the reaction temperature to be 48+ k1 (the mass fraction of the sodium diisooctyl succinate sulfonate + the mass fraction of the polyethylene glycol) (the volume ratio of the ethyl alcohol to the water), wherein k1 is an adjustment coefficient, and k1 to be 4.25 to 104Reacting, and filtering to obtain cuprous chloride;
2) preparing a sodium bicarbonate solution, adding cuprous chloride particles, adding diisooctyl succinate sodium sulfonate and polyethylene glycol, wherein the mass fraction of the diisooctyl succinate sodium sulfonate in the mixed solution is 0.15%, the mass fraction of the polyethylene glycol is 0.25%, then adding urea and hydrogen peroxide, wherein the mole number of the urea, the hydrogen peroxide and the cuprous chloride in the mixed solution is 1.2:1.5:1, sealing, heating and reacting at high pressure, wherein the reaction temperature is 135 ℃ and the pressure is 2.5 atmospheres, filtering the reaction product, and drying in vacuum to obtain the high-purity nano copper oxide.
2. The process of claim 1, wherein the temperature of the aqueous ammonia in step 1 is 45 ℃, the concentration of the aqueous ammonia is 5.0mol/L, and the molar ratio of cuprous chloride in the cuprous chloride feed to ammonia in the aqueous ammonia is 1: 5.
3. The method as set forth in claim 1, wherein the mass fraction of sodium diisooctyl sulfosuccinate in the mixed solution of step 1 is 0.05-0.06%, the mass fraction of polyethylene glycol is 0.08-0.096%, and the molecular weight of polyethylene glycol is 40000-60000.
4. The method according to claim 1, wherein the volume ratio of water to ethanol in the mixed solution of step 1 is 67:33 to 70: 30.
5. The method of claim 1, wherein the molar ratio of ethyl acetate to cuprous ions in the mixed solution of step 1 is 3.5: 1.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103537284A (en) * | 2013-11-01 | 2014-01-29 | 长沙理工大学 | Preparation method of nano-copper oxide catalyst for degrading organic dye wastewater |
| CN105084408A (en) * | 2015-08-07 | 2015-11-25 | 电子科技大学 | Preparing method for copper oxide powder |
| CN108069455A (en) * | 2018-01-12 | 2018-05-25 | 蒋央芳 | A kind of preparation method of nano cupric oxide |
| CN111747440A (en) * | 2020-07-13 | 2020-10-09 | 泰兴冶炼厂有限公司 | Method for preparing high-purity active copper oxide by alkali etching solution secondary ammonia evaporation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103537284A (en) * | 2013-11-01 | 2014-01-29 | 长沙理工大学 | Preparation method of nano-copper oxide catalyst for degrading organic dye wastewater |
| CN105084408A (en) * | 2015-08-07 | 2015-11-25 | 电子科技大学 | Preparing method for copper oxide powder |
| CN108069455A (en) * | 2018-01-12 | 2018-05-25 | 蒋央芳 | A kind of preparation method of nano cupric oxide |
| CN111747440A (en) * | 2020-07-13 | 2020-10-09 | 泰兴冶炼厂有限公司 | Method for preparing high-purity active copper oxide by alkali etching solution secondary ammonia evaporation method |
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