CN111482175B - Preparation method of copper/cuprous oxide heterojunction nanosheet catalyst - Google Patents
Preparation method of copper/cuprous oxide heterojunction nanosheet catalyst Download PDFInfo
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- CN111482175B CN111482175B CN202010387369.8A CN202010387369A CN111482175B CN 111482175 B CN111482175 B CN 111482175B CN 202010387369 A CN202010387369 A CN 202010387369A CN 111482175 B CN111482175 B CN 111482175B
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000010949 copper Substances 0.000 title claims abstract description 36
- 239000003054 catalyst Substances 0.000 title claims abstract description 34
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 33
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229940112669 cuprous oxide Drugs 0.000 title claims abstract description 33
- 229910000431 copper oxide Inorganic materials 0.000 title claims abstract description 30
- 239000002135 nanosheet Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 33
- 238000006243 chemical reaction Methods 0.000 claims description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- ZKXWKVVCCTZOLD-UHFFFAOYSA-N copper;4-hydroxypent-3-en-2-one Chemical compound [Cu].CC(O)=CC(C)=O.CC(O)=CC(C)=O ZKXWKVVCCTZOLD-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- 230000001476 alcoholic effect Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 239000012752 auxiliary agent Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 16
- 239000001569 carbon dioxide Substances 0.000 description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 description 8
- 238000003917 TEM image Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000005431 greenhouse gas Substances 0.000 description 2
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 150000005677 organic carbonates Chemical class 0.000 description 1
- 238000005832 oxidative carbonylation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- B01J35/30—
-
- B01J35/39—
Abstract
The invention provides a preparation method of a copper/cuprous oxide heterojunction nanosheet catalyst, wherein the copper/cuprous oxide heterojunction nanosheet catalyst is composed of copper and cuprous oxide. The invention greatly increases the catalytic activity of copper by selecting cuprous oxide as a new auxiliary agent to modify the traditional copper catalyst and forming a heterojunction with copper. According to the invention, the morphology of the catalyst is limited to nanosheets by a hydrothermal synthesis method, so that the specific surface area is increased, the molar ratio of copper to cuprous oxide can be changed and adjusted by adjusting the feeding composition, and the catalytic activity of the catalyst can be effectively regulated and controlled.
Description
Technical Field
The invention relates to a preparation method of a copper/cuprous oxide heterojunction nanosheet catalyst, and belongs to the field of preparation of inorganic materials.
Background
Since the 21 st century, the demand of people for traditional fossil energy such as petroleum and coal is increasing due to the development of economy and the improvement of living standard of people, so that greenhouse gases such as carbon dioxide are discharged in large quantity, the content of carbon dioxide in the atmosphere is increasing, the greenhouse effect is obvious day by day, and the living environment of people is deteriorating day by day. Therefore, the resource utilization of carbon dioxide and the development of a carbon dioxide green utilization technology have become important to research. Although carbon dioxide is a greenhouse gas, carbon dioxide is also a cheap, clean and effective carbon resource; if it can be effectively utilized, it can not only solve the related environmental problems, but also reduce the dependence on other kinds of carbon resources.
Dimethyl carbonate, as a simple low-molecular organic carbonate, has the interesting properties of stable chemical properties, no toxicity to organisms and the like, so that the dimethyl carbonate has wide application as a green reagent in the chemical industry. There are many industrial methods for synthesizing dimethyl carbonate, for example, a methanol phosgenation method, a methanol oxidative carbonylation method, an ester exchange method of ethylene carbonate with methanol, and the like. Due to serious pollution of raw materials, low product conversion rate, poor principle and the like, the methods are greatly limited in practical application. The direct use of methanol and carbon dioxide for the synthesis of dimethyl carbonate greatly increases the synthesis cost and the equipment maintenance cost due to the high-temperature and high-pressure catalysis conditions required by the traditional copper-based catalyst. Therefore, it is urgent to find a catalyst which can be applied to the direct synthesis of dimethyl carbonate from methanol and carbon dioxide under low temperature and low pressure conditions.
As a class of emerging nanomaterials, two-dimensional crystals exhibit unique physical properties and promising electronic properties due to their ultra-thin thickness and two-dimensional morphology characteristics. This provides a number of opportunities for their widespread use across biological, medical, physical and chemical domains. Two-dimensional materials not only have a large increase in specific surface area compared to bulk materials, but also exhibit properties that are completely different from bulk materials due to the confinement effect of two-dimensional materials. Compared with a bulk material, the two-dimensional material is easier to expose heterojunction, and the existence of the heterojunction can cause electric charge aggregation, enhance the adsorption of reactants, reduce the activation energy of reaction and effectively improve the yield.
The copper/cuprous oxide catalyst with a two-dimensional structure and containing the heterojunction is synthesized by a hydrothermal method, and the special structure can effectively reduce the temperature and pressure required by the reaction and greatly improve the yield. The method has the advantages of simple process, low energy consumption, high atom utilization rate and environmental friendliness, and is suitable for large-scale popularization and application.
Disclosure of Invention
The invention aims to provide a preparation method of a novel copper/cuprous oxide heterojunction nanosheet catalyst aiming at the defects of the prior art.
In order to achieve the purpose, the invention provides a preparation method of a copper/cuprous oxide heterojunction nanosheet catalyst, which comprises the following steps of:
step 1, adding an organic solvent into an alcohol solvent, and uniformly stirring to obtain a mixed solution;
step 2, adding copper acetylacetonate and a surfactant into the mixed solution, and violently stirring to obtain a reaction solution;
step 3, transferring the reaction liquid to a polytetrafluoroethylene reaction kettle, sealing, and heating to 100-200 ℃ to obtain a product;
and 4, washing, drying and grinding the product to obtain the copper/cuprous oxide heterojunction nanosheet catalyst.
In some embodiments, in step 1, the organic solvent is selected from N, N-dimethylformamide, N-methylpyrrolidone, derivatives thereof, or any combination thereof.
In some embodiments, in step 1, the alcoholic solvent is selected from C 1-6 Alcohols, preferably methanol, ethanol and their derivatives or any combination thereof.
In some embodiments, in step 1, the volume ratio of alcoholic solvent to organic solvent is 1:1 to 6:1.
In some embodiments, in step 1, stirring is performed using a magnetic stirrer at a speed of 1000 to 4000r/min for a period of 10 minutes to 1 hour.
In some embodiments, in step 2, the surfactant is cetyl trimethylammonium bromide, dodecyl trimethylammonium bromide, polyvinylpyrrolidone, sodium oleate, or any combination thereof.
In some embodiments, in step 2, the molar ratio of copper acetylacetonate to surfactant is 6:1-8:1.
In some embodiments, in step 2, stirring is performed using a magnetic stirrer at a speed of 1000 to 4000r/min for a period of 10 minutes to 1 hour.
In some embodiments, in step 3, the volume ratio of the volume of the reaction solution to the volume of the polytetrafluoroethylene reaction vessel is 1:2-1:4.
In some embodiments, in step 3, the warming is a temperature programmed to the reaction temperature; preferably, the heating rate is 5-10 ℃/min; preferably, the reaction time is 6 to 12 hours.
In some embodiments, in step 4, the washing is performed by washing with deionized water until the pH of the supernatant is 7, and then washing with absolute ethanol twice.
In some embodiments, in step 4, the drying is treatment at 60-80 ℃ for 8-24 hours.
The invention also provides a copper/cuprous oxide heterojunction nanosheet catalyst prepared by the method.
The invention provides the following beneficial effects:
the method provided by the invention can synthesize the copper/cuprous oxide heterojunction nanosheet catalyst with the nanoscale thickness under the condition of low energy consumption. The prepared sample has good dispersibility and higher catalytic performance than the existing catalyst. Furthermore, by introducing the heterojunction, the photoresponse capability of the sample can be effectively improved, the practical value of the material is improved, and the method has great economic benefit.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 shows a high resolution transmission electron micrograph of the product of example 1;
FIG. 2 shows a transmission electron micrograph of the product of example 2;
FIG. 3 shows a transmission electron micrograph of the product of example 3.
FIG. 4 shows a transmission electron micrograph of the product of example 4; and is
Figure 5 shows an X-ray electron diffraction (XRD) analysis of the product of example 4.
Detailed Description
The following describes embodiments of the present invention in detail. The embodiments described by referring to the drawings are exemplary only for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Example 1
A preparation method of a copper/cuprous oxide heterojunction nanosheet catalyst comprises the following steps:
(1) Adding 5mL of N, N-dimethylformamide into 30mL of ethanol, and magnetically stirring at the rotation speed of 4000r/min to obtain a mixed solution of the ethanol and the N, N-dimethylformamide;
(2) Adding 8mmol of copper acetylacetonate and 1mmol of hexadecyl trimethyl ammonium bromide into the mixed solution obtained in the step (1), and magnetically stirring for 0.5 hour at the rotating speed of 4000r/min to obtain a reaction solution;
(3) Transferring the reaction solution in the step 2 to a 140mL polytetrafluoroethylene reaction kettle, sealing, and then carrying out programmed heating to 200 ℃, wherein the heating rate is 10 ℃/min, and reacting for 8 hours to obtain a product;
(4) And (3) washing with water and ethanol for 3 times, drying in an oven at 60 ℃ for 24 hours, and putting the dried product into a mortar for grinding and dispersing to obtain the copper/cuprous oxide heterojunction nanosheet catalyst.
FIG. 1 shows a high-resolution transmission electron micrograph of the obtained powder. The obtained copper/cuprous oxide heterojunction nanosheet catalyst shows two different lattice spacings, which shows that the obtained sample is high in purity and accurate in synthesis.
Example 2
A preparation method of a copper/cuprous oxide heterojunction nanosheet catalyst comprises the following steps:
(1) Adding 15mL of N, N-dimethylformamide into 15mL of ethanol, and magnetically stirring at the rotating speed of 1000r/min to obtain a mixed solution of the ethanol and the N, N-dimethylformamide;
(2) Adding 6mmol of copper acetylacetonate and 1mmol of hexadecyl trimethyl ammonium bromide into the mixed solution obtained in the step (1), and magnetically stirring for 1 hour at the rotating speed of 1000r/min to obtain a reaction solution;
(3) Transferring the reaction solution in the step 2 into a 60mL polytetrafluoroethylene reaction kettle, sealing, and then carrying out programmed heating to 100 ℃, wherein the heating rate is 5 ℃/min, and reacting for 8 hours to obtain a product;
(4) And (3) washing with water and ethanol for 3 times, drying in an oven at 60 ℃ for 24 hours, and putting the dried product into a mortar for grinding and dispersing to obtain the copper/cuprous oxide heterojunction nanosheet catalyst.
The morphology (transmission electron micrograph) of the obtained powder is shown in FIG. 2. The obtained copper/cuprous oxide heterojunction nanosheet catalyst has only one shape and is in a nanosheet shape.
Example 3
A preparation method of a copper/cuprous oxide heterojunction nanosheet catalyst comprises the following steps:
(1) Adding 10mL of N, N-dimethylformamide into 30mL of ethanol, and magnetically stirring at a rotating speed of 3000r/min to obtain a mixed solution of ethanol and N, N-dimethylformamide;
(2) Adding 6mmol of copper acetylacetonate and 1mmol of sodium oleate into the mixed solution in the step 1, and magnetically stirring for 1 hour at the rotating speed of 4000r/min to obtain a reaction solution;
(3) Transferring the reaction solution in the step 2 to a polytetrafluoroethylene reaction kettle of 80mL, sealing, and then carrying out programmed heating to 150 ℃, wherein the heating rate is 8 ℃/min, and reacting for 8 hours to obtain a product;
(4) And (3) washing with water and ethanol for 3 times, drying in an oven at 60 ℃ for 24 hours, and putting the dried product into a mortar for grinding and dispersing to obtain the copper/cuprous oxide heterojunction nanosheet catalyst.
The morphology (transmission electron micrograph) of the obtained powder is shown in FIG. 3. The obtained copper/cuprous oxide heterojunction catalyst is of a nanosheet shape.
Example 4
A preparation method of a copper/cuprous oxide heterojunction nanosheet catalyst comprises the following steps:
(1) Adding 10mL of N, N-dimethylformamide into 35mL of ethanol, and magnetically stirring at a rotation speed of 2000r/min to obtain a mixed solution of ethanol and N, N-dimethylformamide;
(2) Adding 7mmol of copper acetylacetonate and 1mmol of sodium oleate into the mixed solution in the step 1, and magnetically stirring for 1 hour at the rotating speed of 2000r/min to obtain a reaction solution;
(3) Transferring the reaction solution in the step 2 into a 90mL polytetrafluoroethylene reaction kettle, sealing, and then, carrying out temperature programming to 180 ℃, wherein the temperature rise rate is 9 ℃/min, and reacting for 8 hours to obtain a product;
(4) And (3) washing with water and ethanol for 3 times, drying in an oven at 60 ℃ for 24 hours, and putting the dried product into a mortar for grinding and dispersing to obtain the copper/cuprous oxide heterojunction nanosheet catalyst.
The morphology (transmission electron micrograph) of the obtained powder is shown in FIG. 4. The obtained copper/cuprous oxide heterojunction catalyst has a nanosheet shape.
The copper/cuprous oxide heterojunction nanosheet catalyst obtained in example 1 was subjected to X-ray diffraction (XRD) analysis, and the XRD spectrum obtained was as shown in fig. 5. By comparing the JCPDF standard card (85-1326) of copper with the JCPDF standard card (74-1230) of cuprous oxide, the obtained copper/cuprous oxide heterojunction nanosheet catalyst is obviously composed of two different substances, namely copper and cuprous oxide. The diffraction peak has high intensity and slightly widened peak shape, which shows that the sample has high purity and the shape is in nano scale.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A preparation method of a copper/cuprous oxide heterojunction nanosheet catalyst is characterized by comprising the following steps:
step 1, adding an organic solvent into an alcohol solvent, and uniformly stirring to obtain a mixed solution, wherein the organic solvent is selected from N, N-dimethylformamide, N-methylpyrrolidone and derivatives thereof or any combination of N, N-dimethylformamide, N-methylpyrrolidone and derivatives thereof, and the alcohol solvent is selected from C 1-6 Alcohol and its derivatives or any combination thereof, and the volume ratio of the alcohol solvent to the organic solvent is 1:1-6:1;
step 2, adding copper acetylacetonate and a surfactant into the mixed solution, and violently stirring to obtain a reaction solution, wherein the surfactant is cetyl trimethyl ammonium bromide, dodecyl trimethyl ammonium bromide, sodium oleate or any combination thereof, and the molar ratio of the copper acetylacetonate to the surfactant is 6:1-8:1;
step 3, transferring the reaction liquid to a polytetrafluoroethylene reaction kettle, sealing, and heating to 100-200 ℃ to obtain a product;
and 4, washing, drying and grinding the product to obtain the copper/cuprous oxide heterojunction nanosheet catalyst.
2. The method of claim 1, wherein the alcoholic solvent is selected from methanol, ethanol, derivatives thereof, and any combination thereof.
3. The method according to claim 1, wherein the stirring in step 1 or 2 is carried out using a magnetic stirrer at a rotation speed of 1000 to 4000r/min for a period of 10 minutes to 1 hour.
4. The preparation method of claim 1, wherein in step 3, the volume ratio of the reaction solution volume to the polytetrafluoroethylene reaction kettle is 1:2-1:4.
5. The production method according to claim 1, wherein in step 3, the temperature rise is a temperature programmed to the reaction temperature.
6. The production method according to claim 5, wherein the temperature rise rate is 5 to 10 ℃/min.
7. The method according to claim 1, wherein the reaction time is 6 to 12 hours.
8. The method according to claim 1, wherein in step 4, the washing is performed by washing with deionized water until the pH of the supernatant is 7, and then washing with absolute ethanol twice.
9. The method according to claim 1, wherein the drying is carried out at 60 to 80 ℃ for 8 to 24 hours in step 4.
10. A copper/cuprous oxide heterojunction nanosheet catalyst prepared by the method of any one of claims 1-9.
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| CN101905899B (en) * | 2010-08-16 | 2012-01-04 | 河北工业大学 | Method for preparing ordered nano cuprous oxide polycrystalline powder |
| CN102357659B (en) * | 2011-07-27 | 2013-10-16 | 西安交通大学 | Preparation method of Cu-Cu2O heterogenous junction |
| CN102557106B (en) * | 2012-01-12 | 2013-09-18 | 淮阴师范学院 | Preparation method of cuprous oxide hollow nanometer cubes |
| TWI494160B (en) * | 2013-03-19 | 2015-08-01 | Univ Ishou | Copper-based catalysts for apply to catalyze ammonia to nitrogen |
| CN104098121A (en) * | 2014-06-27 | 2014-10-15 | 江苏华东锂电技术研究院有限公司 | Preparation method for cuprous oxide |
| CN104071824B (en) * | 2014-07-17 | 2015-06-17 | 齐鲁工业大学 | Method for preparing cuprous oxide nanocrystalline with rough surface and controllable morphological structure |
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