CN116876006A - Method for preparing ultrathin high-entropy metal hydroxide nanosheet catalyst by low-temperature cold quenching - Google Patents
Method for preparing ultrathin high-entropy metal hydroxide nanosheet catalyst by low-temperature cold quenching Download PDFInfo
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- 229910000000 metal hydroxide Inorganic materials 0.000 title claims abstract description 60
- 150000004692 metal hydroxides Chemical class 0.000 title claims abstract description 59
- 239000002135 nanosheet Substances 0.000 title claims abstract description 58
- 239000003054 catalyst Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000010791 quenching Methods 0.000 title claims abstract description 6
- 230000000171 quenching effect Effects 0.000 title claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 75
- 238000006243 chemical reaction Methods 0.000 claims abstract description 56
- 238000005303 weighing Methods 0.000 claims abstract description 8
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 3
- 150000002739 metals Chemical class 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 72
- 239000000203 mixture Substances 0.000 claims description 69
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 46
- 238000007789 sealing Methods 0.000 claims description 45
- 238000001816 cooling Methods 0.000 claims description 26
- 239000010453 quartz Substances 0.000 claims description 23
- 230000000630 rising effect Effects 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 23
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 23
- 239000012498 ultrapure water Substances 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 22
- 238000000967 suction filtration Methods 0.000 claims description 22
- 238000004321 preservation Methods 0.000 claims description 19
- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 claims description 18
- IYWJIYWFPADQAN-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;ruthenium Chemical group [Ru].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O IYWJIYWFPADQAN-LNTINUHCSA-N 0.000 claims description 17
- BMGNSKKZFQMGDH-FDGPNNRMSA-L nickel(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ni+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BMGNSKKZFQMGDH-FDGPNNRMSA-L 0.000 claims description 17
- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 claims description 17
- HYZQBNDRDQEWAN-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;manganese(3+) Chemical compound [Mn+3].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O HYZQBNDRDQEWAN-LNTINUHCSA-N 0.000 claims description 16
- FJDJVBXSSLDNJB-LNTINUHCSA-N cobalt;(z)-4-hydroxypent-3-en-2-one Chemical compound [Co].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FJDJVBXSSLDNJB-LNTINUHCSA-N 0.000 claims description 16
- 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 16
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical class CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000007605 air drying Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 23
- 239000011572 manganese Substances 0.000 abstract description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 17
- 239000010949 copper Substances 0.000 abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 15
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract description 2
- 229910052748 manganese Inorganic materials 0.000 abstract description 2
- 229910052707 ruthenium Inorganic materials 0.000 abstract description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 abstract 1
- 229910017052 cobalt Inorganic materials 0.000 abstract 1
- 239000010941 cobalt Substances 0.000 abstract 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract 1
- 229910052802 copper Inorganic materials 0.000 abstract 1
- 230000008014 freezing Effects 0.000 abstract 1
- 238000007710 freezing Methods 0.000 abstract 1
- 239000011812 mixed powder Substances 0.000 abstract 1
- 229910052759 nickel Inorganic materials 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 86
- 239000011701 zinc Substances 0.000 description 14
- 239000000047 product Substances 0.000 description 12
- 239000012467 final product Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 150000003839 salts Chemical group 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000010411 electrocatalyst Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229920008651 Crystalline Polyethylene terephthalate Polymers 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000002564 cardiac stress test Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention relates to a method for preparing an ultrathin high-entropy metal hydroxide nano-sheet catalyst by low-temperature cold quenching, belonging to the fields of material science and engineering technology and chemistry. The metal elements of the ultrathin high-entropy metal hydroxide nano-sheet catalyst prepared by the method are five of ruthenium (Ru), zinc (Zn), manganese (Mn), copper (Cu), iron (Fe), cobalt (Co) and nickel (Ni), and the hydroxide solution for synthesizing the catalyst is sodium hydroxide. Firstly, weighing a certain amount of mixed powder A of acetylacetonate of five metals according to the proportion of various metal elements in a finished product, preparing sodium hydroxide solution B with a certain concentration, then placing the A into a preheated muffle furnace, preserving heat to a molten state, placing the B into a low-temperature freezing tank with a certain temperature for a certain time, then rapidly pouring the A in the molten state into the cooled B, directly suction-filtering, collecting and drying the obtained product after a period of reaction, and finally obtaining the ultrathin high-entropy metal hydroxide nanosheet catalyst. The method has the characteristics of simplicity in operation, controllable yield, strong applicability and the like, and has remarkable advantages compared with the traditional method for preparing the high-entropy catalyst.
Description
(2) Technical field
The invention relates to a method for preparing an ultrathin high-entropy metal hydroxide nano-sheet catalyst by low-temperature cold quenching, belonging to the fields of material science and engineering technology and chemistry.
(3) Background art
Green hydrogen is ideal hydrogen energy meeting the aims of energy conservation, emission reduction and double carbon, and particularly relates to the preparation of hydrogen by using renewable energy sources and often relates to electrolysis of water. For the water electrolysis process, the Oxygen Evolution Reaction (OER) at the anode occurs more slowly than the Hydrogen Evolution Reaction (HER) at the cathode—the OER reaction involves a synergistic proton-electron transfer (CPET) reaction of four electrons, the kinetics and slow diffusion of which severely limit the electrocatalytic efficiency and thus reduce the overall "electro-hydrogen" conversion energy efficiency. Therefore, the development and utilization of high-performance electrocatalysts is of great importance for the smooth progress of OER reactions and the further development of electrocatalytic cleavage water pathways for the production of green hydrogen energy.
The traditional noble metal catalyst has the problems of high cost and low reserves, and is one of the key objects of the current research because of the highly adjustable charge, spin and combination freedom of the five-membered and above-component high-entropy material in order to reduce the loading of noble metal and research and develop materials with good electrocatalytic activity and stability for OER reaction. The high-entropy material has thermodynamic high-entropy effect (stable single-phase solid solution is easy to form between elements), structural lattice distortion effect (larger lattice distortion and defects than those of the traditional alloy are arranged in a lattice), kinetic slow diffusion effect (diffusion and phase change in the material are slow, structural changes such as coarsening and recrystallization are not easy to generate at high temperature), and performance cocktail effect (the basic characteristics of different components and interaction among the components enable the high-entropy material to show more complex characteristics, and the performance of the high-entropy material can be adjusted by adjusting the relative content of the components). These properties allow the high entropy material to have not only excellent electrocatalytic activity but also stability when used in OER reactions. Meanwhile, the two-dimensional sheet material has remarkable advantages in the field of catalysis, and is mainly characterized by huge specific surface area, excellent mechanical property, higher conductivity and the like, and the characteristics can enable the two-dimensional sheet material to have electrochemical reaction surface active sites with higher density, higher activity and higher stability. Therefore, the preparation of the ultrathin high-entropy metal hydroxide nano-sheet catalyst is expected to develop an OER catalyst system with more excellent performance and durability.
To further optimize the surface properties of the catalyst, conventional methods generally include chemical methods, phase transitions, surface etching, electrodeposition, and the like. However, these processes are relatively complex to operate and yield-unstable, and the rapid cooling of the molten salt forms defect-rich oxyhydroxide on the surface of the metal oxide or hydroxide catalyst during the reaction, thereby serving as a true "working" surface to enhance catalytic activity (molten salts have properties different from aqueous solutions, such as stability at high temperatures, low vapor pressure over a wide range, low viscosity, good conductivity, high ion migration and diffusion rates, high heat capacity, ability to dissolve various materials, etc.). The method has the characteristics of low cost, simple operation, controllable yield, strong applicability and the like, and has remarkable advantages compared with the traditional method for preparing the high-entropy catalyst. Therefore, the invention provides a method for preparing the ultrathin high-entropy metal hydroxide nano-sheet catalyst by using the rapid cooling method of molten salt for the first time.
(4) Summary of the invention
1. Object of the invention
The invention aims to provide a method for preparing an ultrathin high-entropy metal hydroxide nano-sheet catalyst by low-temperature cold quenching, which utilizes molten salt to rapidly cool to prepare high-entropy metal hydroxide and adjust the surface property of the high-entropy metal hydroxide nano-sheet catalyst, and simply, safely and massively prepares the ultrathin high-entropy metal hydroxide nano-sheet catalyst for OER reaction of electrolyzed water, so that the application of the electrocatalyst in energy conservation and emission reduction is enriched and the double carbon target is realized.
2. The invention is characterized in that
The key points of the invention are as follows:
(1) Weighing a certain amount of acetylacetone salt powder of five metals according to the proportion of various metal elements in the finished product, and mixing to obtain powder A. The acetylacetonate powder is ruthenium acetylacetonate (C) 15 H 21 O 6 Ru), zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Manganese acetylacetonateC 10 H 14 MnO 4 ) Copper acetylacetonate (C) 10 H 14 CuO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Any five of the following;
(2) Weighing 4g of sodium hydroxide powder, dissolving in a solution of 50ml of ultrapure water and 50ml of absolute ethyl alcohol, and uniformly stirring to obtain 1M KOH, namely a solution B;
(3) And (3) placing the powder A prepared in the step (1) into a muffle furnace preheated in advance, and preserving heat for 30min. The reaction atmosphere is air during preheating, the temperature rising rate of a muffle furnace is 5 ℃/min, the optional heat preservation temperature range is 250 ℃ to 300 ℃, and the temperature after preheating and during heat preservation is determined according to the melting point of the selected acetylacetonate;
(4) Sealing the solution B prepared in the step (2) by using a quartz beaker and a sealing film, and then placing the sealed solution B into a cooling tank at the temperature of minus 20 ℃ for 30min;
(5) And (3) rapidly pouring the molten state A obtained in the step (3) into the cooled B obtained in the step (4), carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst.
The method for preparing the ultrathin high-entropy metal hydroxide nano-sheet catalyst by rapidly cooling the molten salt has the advantages of being capable of utilizing the characteristics of the molten salt, the high-entropy material and the ultrathin two-dimensional material, and having the characteristics of simplicity in operation, stable yield and low cost. The loading of noble metals in OER catalysts can be reduced, thereby facilitating further applications of the novel energy conversion and storage.
(5) The accompanying drawings of the invention
FIG. 1 shows an ultrathin high-entropy metal hydroxide nanosheet catalyst material CuMnFeCoNi (OH) prepared by the method of the invention 10 And RuMnFeCoNi (OH) 10 Oxygen evolution catalytic Activity in 1M KOH electrolyte and commercial catalyst RuO 2 FIG. 2 is a graph showing the electrocatalytic performance comparison of the ultra-thin RuMn prepared by the method of the present inventionFeCoNi(OH) 10 Scanning electron microscopy of two-dimensional nanomaterials.
(6) Embodiments of the invention
The following describes embodiments of the method of the present invention:
example 1
Ultrathin high-entropy metal hydroxide nanosheets CuMnFeCoNi (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) was weighed out in the molar ratio of Cu to Mn to Fe to Co to Ni=1:1:1:1:1 in the final product 10 H 14 CuO 4 ) Manganese acetylacetonate (C) 10 H 14 MnO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 250 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature keeping temperature is 250 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuMnFeCoNi (OH) 10 。
Example 2
Ultrathin high-entropy metal hydroxide nanosheets CuZnFeCoNi (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) was weighed out in the molar ratio of Cu to Zn to Fe to Co to Ni=1:1:1:1:1 in the final product 10 H 14 CuO 4 ) Zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) MixingPowder A is obtained. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 250 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature keeping temperature is 250 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuZnFeCoNi (OH) 10 。
Example 3
Ultrathin high-entropy metal hydroxide nanosheets CuMnZnCoNi (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) was weighed out in the molar ratio of Cu to Mn to Zn to Co to Ni=1:1:1:1:1 in the final product 10 H 14 CuO 4 ) Manganese acetylacetonate (C) 10 H 14 MnO 4 ) Zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 250 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature keeping temperature is 250 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuMnZnCoNi (OH) 10 。
Example 4
Ultrathin high-entropy metal hydroxide nanosheets CuMnFeZnNi (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) was weighed out in the molar ratio of Cu to Mn to Fe to Zn to Ni=1:1:1:1:1 in the final product 10 H 14 CuO 4 ) Manganese acetylacetonate (C) 10 H 14 MnO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 250 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature keeping temperature is 250 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuMnFeZnNi (OH) 10 。
Example 5
Ultrathin high-entropy metal hydroxide nanosheets CuMnFeCoZn (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) was weighed out in terms of the molar ratio of Cu to Mn to Fe to Co to Zn=1:1:1:1:1 in the finished product 10 H 14 CuO 4 ) Manganese acetylacetonate (C) 10 H 14 MnO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 250 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature keeping temperature is 250 ℃. Thereafter, solution B was filled into a quartz beakerSealing with sealing film, and placing into cooling tank at-20deg.C for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuMnFeCoZn (OH) 10 。
Example 6
Ultrathin high-entropy metal hydroxide nanosheets ZnMnFeCoNi (OH) 10 Is prepared by the following steps.
1mmol of zinc acetylacetonate (C) was weighed out in the molar ratio of Zn to Mn to Fe to Co to Ni=1:1:1:1:1 in the final product 10 H 14 ZnO 4 ) Manganese acetylacetonate (C) 10 H 14 MnO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 250 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature keeping temperature is 250 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst ZnMnFeCoNi (OH) 10 。
Example 7
Ultrathin high-entropy metal hydroxide nanosheets RuMnFeCoNi (OH) 10 Is prepared by the following steps.
1mmol of ruthenium acetylacetonate (C) is weighed out according to the mol ratio of Ru to Mn to Fe to Co to Ni=1:1:1:1:1 in the finished product 15 H 21 O 6 Ru), manganese acetylacetonate (C) 10 H 14 MnO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst RuMnFeCoNi (OH) 10 。
Example 8
Ultrathin high-entropy metal hydroxide nanosheets CuRuFeCoNi (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) was weighed out according to the molar ratio of Cu to Ru to Fe to Co to Ni=1:1:1:1:1 in the finished product 10 H 14 CuO 4 ) Ruthenium acetylacetonate (C) 15 H 21 O 6 Ru), iron acetylacetonate (C) 15 H 21 FeO 6 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuRuFeCoNi (OH) 10 。
Example 9
Ultrathin high-entropy metal hydroxide nanosheets CuMnRuCoNi (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) was weighed out in the molar ratio of Cu to Mn to Ru to Co to Ni=1:1:1:1:1 in the final product 10 H 14 CuO 4 ) Manganese acetylacetonate (C) 10 H 14 MnO 4 ) Ruthenium acetylacetonate (C) 15 H 21 O 6 Ru), cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuMnRuCoNi (OH) 10 。
Example 10
Ultrathin high-entropy metal hydroxide nanosheets CuMnFeRuNi (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) was weighed out in the molar ratio of Cu to Mn to Fe to Ru to Ni=1:1:1:1:1 in the final product 10 H 14 CuO 4 ) Manganese acetylacetonate (C) 10 H 14 MnO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Ruthenium acetylacetonate (C) 15 H 21 O 6 Ru), nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reactionThe atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuMnFeRuNi (OH) 10 。
Example 11
Ultrathin high-entropy metal hydroxide nanosheets CuMnFeCoRu (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) was weighed out in the molar ratio of Cu to Mn to Fe to Co to Ru=1:1:1:1:1 in the final product 10 H 14 CuO 4 ) Manganese acetylacetonate (C) 10 H 14 MnO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Ruthenium acetylacetonate (C) 15 H 21 O 6 Ru), and mixing to obtain powder A. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuMnFeCoRu (OH) 10 。
Example 12
Ultrathin high-entropy metal hydroxide nanosheets RuZnFeCoNi (OH) 10 Is prepared by the following steps.
1mmol of ruthenium acetylacetonate (C) is weighed according to the mol ratio of Ru, zn, fe, co, ni=1:1:1:1:1 in the finished product 15 H 21 O 6 Ru), zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst RuZnFeCoNi (OH) 10 。
Example 13
Ultrathin high-entropy metal hydroxide nanosheets RuMnZnCoNi (OH) 10 Is prepared by the following steps.
1mmol of ruthenium acetylacetonate (C) is weighed according to the mol ratio of Ru to Mn to Zn to Co to Ni=1:1:1:1:1 in the finished product 15 H 21 O 6 Ru), manganese acetylacetonate (C) 10 H 14 MnO 4 ) Zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, collecting and drying the mixture for 24h to obtain the ultrathin productHigh entropy metal hydroxide nanosheet catalyst RuMnZnCoNi (OH) 10 。
Example 14
Ultrathin high-entropy metal hydroxide nanosheets RuMnFeZnNi (OH) 10 Is prepared by the following steps.
1mmol of ruthenium acetylacetonate (C) is weighed according to the mol ratio of Ru to Mn to Fe to Zn to Ni=1:1:1:1:1 in the finished product 15 H 21 O 6 Ru), manganese acetylacetonate (C) 10 H 14 MnO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst RuMnFeZnNi (OH) 10 。
Example 15
Ultrathin high-entropy metal hydroxide nanosheets RuMnFeCoZn (OH) 10 Is prepared by the following steps.
1mmol of ruthenium acetylacetonate (C) is weighed according to the mol ratio of Ru to Mn to Fe to Co to Zn=1:1:1:1:1 in the finished product 15 H 21 O 6 Ru), manganese acetylacetonate (C) 10 H 14 MnO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Powder A is obtained after mixing. Weighing 4g sodium hydroxide powder, dissolving in 50ml ultrapure water and 50ml anhydrous ethanol mixed solution, stirring uniformly to obtain1M KOH, solution B. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst RuMnFeCoZn (OH) 10 。
Example 16
Ultrathin high-entropy metal hydroxide nanosheets CuRuZnCoNi (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) was weighed out according to the molar ratio of Cu to Ru to Zn to Co to Ni=1:1:1:1:1 in the finished product 10 H 14 CuO 4 ) Ruthenium acetylacetonate (C) 15 H 21 O 6 Ru), zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuRuZnCoNi (OH) 10 。
Example 17
Ultrathin high-entropy metal hydroxide nanosheets CuRuFeZnNi (OH) 10 Is prepared by the following steps.
Weighing 1mmol of each B according to the molar ratio of Cu to Ru to Fe to Zn to Ni=1:1:1:1:1 in the finished productCopper acetylacetonate (C) 10 H 14 CuO 4 ) Ruthenium acetylacetonate (C) 15 H 21 O 6 Ru), iron acetylacetonate (C) 15 H 21 FeO 6 ) Zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuRuFeZnNi (OH) 10 。
Example 18
Ultrathin high-entropy metal hydroxide nanosheets CuRuFeCoZn (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) is weighed according to the molar ratio of Cu to Ru to Fe to Co to Zn=1:1:1:1:1 in the finished product 10 H 14 CuO 4 ) Ruthenium acetylacetonate (C) 15 H 21 O 6 Ru), iron acetylacetonate (C) 15 H 21 FeO 6 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, the molten state A is rapidly poured into the cooled B to be treatedAfter reacting for 30min, filtering the obtained mixture, washing the mixture with absolute ethyl alcohol, collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuRuFeCoZn (OH) 10 。
Example 19
Ultrathin high-entropy metal hydroxide nanosheets CuMnRuZnNi (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) was weighed out in the molar ratio of Cu to Mn to Ru to Zn to Ni=1:1:1:1:1 in the final product 10 H 14 CuO 4 ) Manganese acetylacetonate (C) 10 H 14 MnO 4 ) Ruthenium acetylacetonate (C) 15 H 21 O 6 Ru), zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuMnRuZnNi (OH) 10 。
Example 20
Ultrathin high-entropy metal hydroxide nanosheets CuMnRuCoZn (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) was weighed out in terms of the molar ratio of Cu to Mn to Ru to Co to Zn=1:1:1:1:1 in the finished product 10 H 14 CuO 4 ) Manganese acetylacetonate (C) 10 H 14 MnO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Ruthenium acetylacetonate (C) 15 H 21 O 6 Ru), zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Powder A is obtained after mixing. Weighing and weighing4g of sodium hydroxide powder was dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and after stirring uniformly, 1M KOH, solution B, was obtained. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuMnRuCoZn (OH) 10 。
Example 21
Ultrathin high-entropy metal hydroxide nanosheets CuMnFeRuZn (OH) 10 Is prepared by the following steps.
1mmol of copper acetylacetonate (C) was weighed out according to the molar ratio of Cu to Mn to Fe to Ru to Zn=1:1:1:1:1 in the finished product 10 H 14 CuO 4 ) Manganese acetylacetonate (C) 10 H 14 MnO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Ruthenium acetylacetonate (C) 15 H 21 O 6 Ru), zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Powder A is obtained after mixing. 4g of sodium hydroxide powder was weighed and dissolved in a solution of 50ml of ultrapure water and 50ml of absolute ethanol, and 1M KOH, solution B, was obtained after stirring uniformly. And (3) placing the powder A into a muffle furnace preheated to 300 ℃ in advance, and preserving the heat for 30min. The reaction atmosphere is air, the temperature rising rate of the muffle furnace is 5 ℃/min, and the temperature preservation temperature is 300 ℃. And then sealing the solution B by using a quartz beaker and a sealing film, and then placing the solution B into a cooling tank at the temperature of minus 20 ℃ for 30min. Finally, rapidly pouring the molten state A into the cooled B, carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst CuMnFeRuZn (OH) 10 。
Claims (1)
1. The method for preparing the ultrathin high-entropy metal hydroxide nano-sheet catalyst by low-temperature cold quenching is characterized by comprising the following steps of:
(1) Weighing a certain amount of acetylacetone salt powder of five metals according to the proportion of various metal elements in the finished product, and mixing to obtain powder A. The acetylacetonate powder is ruthenium acetylacetonate (C) 15 H 21 O 6 Ru), zinc acetylacetonate (C) 10 H 14 ZnO 4 ) Manganese acetylacetonate (C) 10 H 14 MnO 4 ) Copper acetylacetonate (C) 10 H 14 CuO 4 ) Iron acetylacetonate (C) 15 H 21 FeO 6 ) Cobalt acetylacetonate (C) 15 H 21 CoO 6 ) Nickel acetylacetonate (C) 10 H 14 NiO 4 ) Any five of the following;
(2) Weighing 4g of sodium hydroxide powder, dissolving in a solution of 50ml of ultrapure water and 50ml of absolute ethyl alcohol, and uniformly stirring to obtain 1M KOH, namely a solution B;
(3) And (3) placing the powder A prepared in the step (1) into a muffle furnace preheated in advance, and preserving heat for 30min. The reaction atmosphere is air during preheating, the temperature rising rate of a muffle furnace is 5 ℃/min, the optional heat preservation temperature range is 250 ℃ to 300 ℃, and the temperature after preheating and during heat preservation is determined according to the melting point of the selected acetylacetonate;
(4) Sealing the solution B prepared in the step (2) by using a quartz beaker and a sealing film, and then placing the sealed solution B into a cooling tank at the temperature of minus 20 ℃ for 30min;
(5) And (3) rapidly pouring the molten state A obtained in the step (3) into the cooled B obtained in the step (4), carrying out suction filtration on the obtained mixture after the reaction is carried out for 30min, washing the mixture with absolute ethyl alcohol, and collecting and naturally air-drying the mixture for 24h to obtain the ultrathin high-entropy metal hydroxide nano-sheet catalyst.
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