CN112495380A - Cu-Fe bimetallic nanosheet and preparation method thereof - Google Patents
Cu-Fe bimetallic nanosheet and preparation method thereof Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 229910017827 Cu—Fe Inorganic materials 0.000 title claims abstract description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 210
- 239000000243 solution Substances 0.000 claims abstract description 190
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 96
- 150000003839 salts Chemical class 0.000 claims abstract description 56
- 238000010438 heat treatment Methods 0.000 claims abstract description 47
- 238000005406 washing Methods 0.000 claims abstract description 47
- 239000008367 deionised water Substances 0.000 claims abstract description 45
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 45
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 26
- 239000000047 product Substances 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000012266 salt solution Substances 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- 239000008139 complexing agent Substances 0.000 claims abstract description 7
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 24
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 16
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 15
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 12
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 12
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 11
- 229910021592 Copper(II) chloride Inorganic materials 0.000 claims description 9
- 229960005070 ascorbic acid Drugs 0.000 claims description 8
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 6
- 239000008103 glucose Substances 0.000 claims description 6
- 238000006722 reduction reaction Methods 0.000 claims description 5
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- 239000011668 ascorbic acid Substances 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 abstract description 34
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 abstract description 34
- 238000006731 degradation reaction Methods 0.000 abstract description 34
- 230000003197 catalytic effect Effects 0.000 abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 129
- 239000010949 copper Substances 0.000 description 127
- 239000002994 raw material Substances 0.000 description 57
- 239000002086 nanomaterial Substances 0.000 description 25
- 238000001291 vacuum drying Methods 0.000 description 15
- 239000000463 material Substances 0.000 description 7
- 229910000510 noble metal Inorganic materials 0.000 description 7
- 239000002211 L-ascorbic acid Substances 0.000 description 6
- 235000000069 L-ascorbic acid Nutrition 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010970 precious metal Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XYBSIYMGXVUVGY-UHFFFAOYSA-N 2,2',4,4'-Tetrabromodiphenyl ether Chemical compound BrC1=CC(Br)=CC=C1OC1=CC=C(Br)C=C1Br XYBSIYMGXVUVGY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 150000001879 copper Chemical class 0.000 description 2
- IYRDVAUFQZOLSB-UHFFFAOYSA-N copper iron Chemical compound [Fe].[Cu] IYRDVAUFQZOLSB-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
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- 229910002549 Fe–Cu Inorganic materials 0.000 description 1
- 229930003779 Vitamin B12 Natural products 0.000 description 1
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- AGVAZMGAQJOSFJ-WZHZPDAFSA-M cobalt(2+);[(2r,3s,4r,5s)-5-(5,6-dimethylbenzimidazol-1-yl)-4-hydroxy-2-(hydroxymethyl)oxolan-3-yl] [(2r)-1-[3-[(1r,2r,3r,4z,7s,9z,12s,13s,14z,17s,18s,19r)-2,13,18-tris(2-amino-2-oxoethyl)-7,12,17-tris(3-amino-3-oxopropyl)-3,5,8,8,13,15,18,19-octamethyl-2 Chemical compound [Co+2].N#[C-].[N-]([C@@H]1[C@H](CC(N)=O)[C@@]2(C)CCC(=O)NC[C@@H](C)OP(O)(=O)O[C@H]3[C@H]([C@H](O[C@@H]3CO)N3C4=CC(C)=C(C)C=C4N=C3)O)\C2=C(C)/C([C@H](C\2(C)C)CCC(N)=O)=N/C/2=C\C([C@H]([C@@]/2(CC(N)=O)C)CCC(N)=O)=N\C\2=C(C)/C2=N[C@]1(C)[C@@](C)(CC(N)=O)[C@@H]2CCC(N)=O AGVAZMGAQJOSFJ-WZHZPDAFSA-M 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
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- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000003586 protic polar solvent Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 235000019163 vitamin B12 Nutrition 0.000 description 1
- 239000011715 vitamin B12 Substances 0.000 description 1
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- 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
- B01J23/74—Iron group metals
- B01J23/745—Iron
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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Abstract
The invention discloses a Cu-Fe bimetallic nanosheet and a preparation method thereof, and the preparation method comprises the following steps: 1) preparing NaOH solution: using deionized water to NaOHDissolving in a beaker, transferring to a volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use; 2) preparing a Cu salt solution and an Fe salt solution: dissolving Cu salt and Fe salt in different beakers respectively by using deionized water, transferring the dissolved Cu salt and Fe salt to different volumetric flasks respectively after the Cu salt and Fe salt are completely dissolved, and washing, fixing the volume and shaking up for later use; 3) putting the NaOH solution prepared in the step 1) into a flask, adding the Cu salt solution and the Fe salt solution prepared in the step 2) into the single-neck flask, then adding a complexing agent and a reducing agent, uniformly mixing, and heating in a water bath; 4) after the water bath heating in the step 3) is finished, centrifugally separating a reaction product, and drying to obtain a product, namely the Cu-Fe bimetallic nanosheet, wherein the prepared Cu-Fe bimetallic nanosheet has excellent catalytic performance in catalyzing degradation of Congo red, and the prepared Cu0.6Fe0.4The degradation rate of the Congo red catalyzed by the nanosheets reaches 97%.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a Cu-Fe bimetallic nanosheet and a preparation method thereof.
Background
Metals have unique physicochemical properties and are widely used in many fields, particularly in the field of catalysis. When the size of the metal particles is reduced to the nanometer level, the metal material is affected by the size effect, and the physical and chemical properties of the material are enhanced. Compared with bulk materials, the nano material has higher catalytic activity, better electrical, optical and magnetic properties and the like. With the intensive research on the nano material, the researchers find that the bimetallic nano material has better application prospect compared with a single metal nano material. The bimetallic nano-material does not simply combine or enhance the properties of two metals, but shows excellent optical, thermal, electrochemical, catalytic and mechanical properties through the synergistic effect of the two metals. The bimetallic nano-material has potential application value in the fields of catalysis, magnetic recording, sensing, medical diagnosis and the like.
Among many metal materials, noble metals are favored by researchers because of their unique physicochemical properties, such as high stability, unique electrical, optical, and catalytic properties. At present, bimetallic nanomaterials are mainly researched on noble metals, and researchers try to combine noble metals with noble metals, noble metals with non-noble metals, or load bimetallic nanoparticles on a special carrier to prepare high-efficiency bimetallic catalysts. At present, a large number of high-activity bimetallic nanomaterials are developed, but most of the bimetallic nanomaterials are precious metal materials, the cost is high, the comprehensive economic benefit is low, and researchers reduce the cost by compounding precious metals and non-precious metals or loading metals on special supporting materials so as to reduce the consumption of the precious metals, but the development of the bimetallic nanomaterials is limited by the problems that the space structure is complex, the stability is low, active components are easy to lose, and the like. In addition, catalyst recovery is also a problem. Therefore, it is necessary to develop a low-cost, easily recyclable and highly efficient bimetallic nanomaterial.
Copper has abundant reserves, low cost and better catalytic performance, and has infinite possibility of replacing noble metals such as silver and the like in industrial application. Fe has two outermost 4s electron and unsaturated 3d electron shells, which exhibit rich physicochemical properties, such as specific magnetic and catalytic properties. Combining Cu with Fe, it is possible to produce nanomaterials with high catalytic activity, stability and ease of recovery.
The preparation of bimetallic nano-materials of Cu and Fe combination usually adopts the following methods: (1) a co-reduction method: preparation of nano Fe/Cu bimetal by using sodium borohydride to reduce mixed solution of Fe salt and Cu salt (Zhang hong, Liu Dan, Zhang Wen Bo, and removal of methylene blue in water [ J]Journal of national university, Nature version, 2018, 039(004):5-8, Nakseedee P, Tanboonchuy V, Khemthong P, et aL.Role of Cu on Zero Va LentBimeta Cu-Fe in aromatic Removal with Gas Bubbling [ J]. EnvironmentaL Progress &Sustainablele Energy, 2017, 36(5): 1449-; (2) displacement deposition method: reducing Fe salt, and depositing Cu on the surface of Fe (baiting, Sunliping, Linying Jie, etc.. influence and mechanism of copper load rate on reduction rate of dichloromethane in nano Fe/Cu bimetal + vitamin B12 system [ J]Application chemical industry, 2018, 047(010): 2124-; li H F, Wang J, Wang R, et aL. Debromination of 2,2 ',4, 4' -tetrabromodiphenyL ether (BDE-47) by synthetic Pd/Fe0 and Cu/Fe0 in different protic soLvents [J]Chemosphere, 2018, 212: 946-953.); (3) cu nanowires and Fe nanowires are treated by electric melting explosion technology to prepare nano materials (Lerner M I, Psakhie S G, Lozhkomoev A S, et aL. Fe-Cu Nanocomposites by High Pressure conductivity of Powders by electric melting explosion of metals [ J]Adv Eng Mater, 2018, 20(8): 1701024 · 1701029.). Although there are many methods for preparing Cu-Fe bimetallic nanomaterials, these methods have many disadvantages. For example, nanomaterials prepared by co-reduction methods have poor stability; the nano material prepared by the displacement deposition method has the problem of uneven dispersion of Cu nano particles, the problems have great influence on the activity of the nano material as a catalyst, a special device is needed by an electric melting and explosion method, the production cost is greatly increased, the nano material mostly takes nano zero-valent iron as a main body, and reports about the bimetallic nano material with Cu as the main body part and Fe doped in the nano material are less.
Chinese patent publication No. CN105414558A discloses a method for preparing monodisperse spherical nano-copper-iron, which comprises dissolving copper salt, iron salt and stabilizer in organic solvent, and controlling the total metal ion concentration of copper and iron, the volume ratio of organic solvent to stabilizer and the molar ratio of copper salt to iron salt; then purging with nitrogen at the temperature of 110-; and after the reaction is finished, cooling to room temperature, precipitating the nano material by using ethanol, centrifugally washing by using normal hexane, and drying in vacuum to obtain a product. The preparation temperature of the nano copper-iron material obtained by the method is high, the obtained product is spherical, the surface appearance is single, and the development of the nano copper-iron material is limited.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a Cu-Fe bimetallic nanosheet and a preparation method thereof, the prepared Cu-Fe bimetallic nanosheet has excellent catalytic performance in catalyzing degradation of Congo red, the preparation method is simple, and the reaction conditions are mild.
The Cu-Fe bimetallic nanosheet is characterized in that the Cu-Fe bimetallic nanosheet is in a shape controlled by changing the molar ratio of Cu salt to Fe salt.
The preparation method of the Cu-Fe bimetallic nanosheet is characterized in that the Cu-Fe bimetallic nanosheet is prepared by a chemical reduction method, and specifically comprises the following steps:
1) preparing NaOH solution: dissolving NaOH in a beaker by using deionized water, transferring the solution to a medium-volume flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing a Cu salt solution and an Fe salt solution: dissolving Cu salt and Fe salt in different beakers respectively by using deionized water, transferring the dissolved Cu salt and Fe salt to different volumetric flasks respectively after the Cu salt and Fe salt are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting the NaOH solution prepared in the step 1) into a flask, adding the Cu salt solution and the Fe salt solution prepared in the step 2) into the flask, then adding a complexing agent and a reducing agent, uniformly mixing, and heating in a water bath;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and drying to obtain the product, namely the Cu-Fe bimetallic nanosheet.
The preparation method of the Cu-Fe bimetallic nanosheet is characterized in that the concentration of NaOH solution in the step 1) is 10-30 mol/L, preferably 15-25 mol/L.
The preparation method of the Cu-Fe bimetallic nanosheet is characterized in that the Cu salt in the step 2) is Cu (NO)3)2、CuSO4Or CuCl2The Fe salt is Fe (NO)3)3、Fe2(SO4)3Or FeCl3。
The preparation method of the Cu-Fe bimetallic nanosheet is characterized in that the molar ratio of the Cu salt to the Fe salt in the step 3) is 1:0.11-4, the molar ratio of the total mole number of the Cu salt and the Fe salt to the complexing agent is 1:20-50, and the molar ratio of the total mole number of the Cu salt and the Fe salt to the reducing agent is 1: 1-5.
The preparation method of the Cu-Fe bimetallic nanosheet is characterized in that in the step 3), the complexing agent is anhydrous ethylenediamine, and the reducing agent is ascorbic acid, glucose or hydrazine hydrate.
The preparation method of the Cu-Fe bimetallic nanosheet is characterized in that in the step 3), the water bath temperature is 60-80 ℃, and the water bath heating time is 0.5-1.5 h.
The preparation method of the Cu-Fe bimetallic nanosheet is characterized in that in the step 4), the drying temperature is 45-60 ℃, and the drying time is 20-24 h.
Compared with the prior art, the invention has the beneficial effects that:
1) by adopting the technical scheme of the invention, the flaky Cu-Fe bimetallic nano-material which takes Cu as a main body and has uniform appearance can be prepared, the prepared Cu-Fe bimetallic nano-sheet has excellent catalytic performance in catalyzing degradation of Congo red, and the prepared Cu-Fe bimetallic nano-sheet has excellent catalytic performance0.6Fe0.4The degradation rate of the congo red catalyzed by the nanosheets reaches 97%, and the material has good reusability when being used as a catalyst;
2) the preparation method is simple, has mild reaction conditions, and has the characteristics of environmental protection.
Drawings
FIG. 1 shows Cu prepared in example 40.6Fe0.4Scanning electron microscope images of the bimetallic nanosheets;
FIG. 2 shows Cu prepared in example 40.6Fe0.4A high-resolution transmission electron microscope image of the bimetallic nanosheets;
FIG. 3 shows Cu prepared in example 40.6Fe0.4An absorbance change diagram of degradation of Congo red catalyzed by the bimetallic nanosheets;
FIG. 4 shows Cu prepared in example 40.6Fe0.4A graph of degradation rate of Congo red catalyzed by bimetallic nanosheets.
Detailed Description
The invention is further illustrated by the following examples, without restricting its scope to these.
The Cu-Fe bimetallic nanosheets, preferably Cu, of the present invention0.9Fe0.1And also Cu0.8Fe0.2，Cu0.7Fe0.3，Cu0.6Fe0.4，Cu0.5Fe0.5，Cu0.4Fe0.6，Cu0.3Fe0.7，Cu0.2Fe0.8And Cu0.9Fe0.1Hereinafter referred to as Cu0.9Fe0.1Bimetallic nanosheets, e.g., Cu0.8Fe0.2Bimetallic nanoplates and the like, wherein the subscripts indicate the molar ratio of Cu salt to Fe salt.
Example 1
Preparation of Cu0.9Fe0.1Bimetallic nanosheet
1) Preparing 10mol/L NaOH solution: dissolving 100g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.5 mol/L CuSO4Solution, 0.5 mol/L FeCl3Solution: 7.98g of CuSO48.11g of FeCl3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting the CuSO prepared in the step 2)4Solution and FeCl3Adding 9mL and 1mL of the solution into a flask respectively, then adding 16.7 mL of anhydrous ethylenediamine and 5mL of 1mol/L ascorbic acid solution, uniformly mixing, and heating in a water bath at 60 ℃ for 0.5 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 45 ℃ for 20h to obtain a product, namely Cu0.9Fe0.1A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 90%.
Example 2
Preparation of Cu0.8Fe0.2Bimetallic nanosheet
1) Preparing NaOH solution with the amount concentration of 15 mol/L: dissolving 150g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) CuCl with the amount concentration of the prepared substance being 0.2mol/L2Solution, 0.2mol/L Fe (NO)3)3Solution: 2.69g of CuCl24.84g of Fe (NO)3)3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and taking CuCl prepared in the step 2)2Solution, Fe (NO)3)3Adding 8mL and 2mL of the solution into a flask respectively, then adding 3.8 mL of anhydrous ethylenediamine and 6mL of 1mol/L glucose solution, fully shaking up the solution, and heating the solution in a 70 ℃ water bath for 1 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 55 ℃ for 22h to obtain a product, namely Cu0.8Fe0.2A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 92%.
Example 3
Preparation of Cu0.7Fe0.3Bimetallic nanosheet
1) Preparing a 20mol/L NaOH solution: dissolving 200g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.2mol/L CuCl2Solution, 0.2mol/L Fe (NO)3)3Solution: 2.69g of CuCl24.84 Fe (NO)3)3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting the CuCl prepared in the step 2)2Solution and Fe (NO)3)3Adding 7mL and 3mL of the solution into a flask respectively, then adding 2.7mL of anhydrous ethylenediamine and 0.61 mL of hydrazine hydrate solution with the mass fraction of 80%, uniformly mixing the solution and heating the mixture in a water bath at 80 ℃ for 1.5 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 60 ℃ for 24 hours to obtain a product, namely Cu0.7Fe0.3A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 93%.
Example 4
Preparation of Cu0.6Fe0.4Bimetallic nanosheet
1) Preparing 15mol/L NaOH solution: dissolving 150g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.1mol/L Cu (NO)3)2Solution, 0.1mol/L Fe2(SO4)3Solution: 1.88g of Cu (NO)3)23.99g of Fe2(SO4)3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting Cu (NO) prepared in the step 2)3)2Solution and Fe2(SO4)3Adding 6mL and 4mL of the solution into a flask respectively, then adding 2.5mL of anhydrous ethylenediamine and 0.1mL of 80% hydrazine hydrate solution by mass fraction, uniformly mixing, and heating in a 70 ℃ water bath for 1 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 55 ℃ for 22h to obtain a product, namely Cu0.6Fe0.4A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 97%.
For Cu prepared in example 40.6Fe0.4The analysis of the bimetallic nanosheets is specifically shown in fig. 1-4:
as can be seen from the scanning electron micrograph of FIG. 1, the prepared Cu0.6Fe0.4The bimetallic nano material presents a disordered sheet structure, the sheet structure is uneven in size and low in compactness, the length of the sheet structure is about 4 mu m, the thickness of the sheet structure is about 100 nm, and a plurality of pores are formed; from the high-resolution TEM image of FIG. 2, two species with different light and dark contrast can be observed, while the (111) crystal plane of Cu and the (110) crystal plane of Fe can be observed, which indicates that there is indeed a small amount of Fe3+Is reduced to Fe and is in the form of CuForming Cu-Fe bimetallic nanosheets; FIG. 3 is Cu0.6Fe0.4The absorbance change curve of the degradation of the catalytic Congo red gradually becomes smaller along with the reaction, and the absorbance value of the characteristic absorption peak of the Congo red at 498nm is shown to be smaller, so that the Cu0.6Fe0.4The bimetal nanosheets can rapidly catalyze Congo red degradation; FIG. 4 is Cu0.6Fe0.4The degradation rate curve of catalytic Congo red degradation can be seen from FIGS. 3 and 4 that the Congo red basically degrades after about 3.5min of reaction, and the degradation rate can reach 97%.
Example 5
Preparation of Cu0.5Fe0.5Bimetallic nanosheet
1) Preparing 15mol/L NaOH solution: dissolving 150g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.1mol/L Cu (NO)3)2Solution, 0.1mol/L Fe2(NO3)3Solution: 1.88g of Cu (NO)3)22.42g of Fe2(NO3)3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting Cu (NO) prepared in the step 2)3)2Solution and Fe2(NO3)3Adding 5mL and 5mL of the solution into a flask respectively, then adding 1.5 mL of anhydrous ethylenediamine and 0.1mL of 80% hydrazine hydrate solution by mass fraction, uniformly mixing, and heating in a 70 ℃ water bath for 1.0 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 45 ℃ for 24 hours to obtain a product, namely Cu0.5Fe0.5A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 93%.
Example 6
Preparation of Cu0.4Fe0.6Bimetallic nanosheet
1) Preparing a 20mol/L NaOH solution: dissolving 200g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.2mol/L Cu (NO)3)2Solution, 0.2mol/L FeCl3Solution: 3.75g of Cu (NO)3)23.24g of Fe2Cl3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting Cu (NO) prepared in the step 2)3)2Solution and FeCl3Adding 4mL and 6mL of the solution into a flask respectively, then adding 3.0mL of anhydrous ethylenediamine and 6mL of 1mol/L glucose solution, uniformly mixing, and heating in a water bath at 80 ℃ for 1.5 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 50 ℃ for 22h to obtain a product, namely Cu0.4Fe0.6A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 86%.
Example 7
Preparation of Cu0.3Fe0.7Bimetallic nanosheet
1) Preparing 10mol/L NaOH solution: dissolving 100g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.3mol/L CuSO4Solution, 0.3mol/L Fe2(NO3)3Solution: 4.79g of CuSO47.26g of Fe2(NO3)3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 100mL of NaOH solution prepared in the step 1) into a flask, and putting CuSO prepared in the step 2)4Solution and Fe2(NO3)3Adding 3mL and 7mL of the solution into a flask respectively, adding 5mL of anhydrous ethylenediamine and 6mL of 1mol/L ascorbic acid solution, uniformly mixing, and adding the mixture to 8Heating in water bath at 0 deg.C for 1 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and drying the reaction product at 55 ℃ for 24 hours in vacuum to obtain a product, namely Cu0.3Fe0.7A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 80%.
Example 8
Preparation of Cu0.2Fe0.8Bimetallic nanosheet
1) Preparing 15mol/L NaOH solution: dissolving 150g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.4mol/L CuCl2Solution, 0.4mol/L Fe2(SO4)3Solution: 5.38g of CuCl216.0g of Fe2(SO4)3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 100mL of NaOH solution prepared in the step 1) into a flask, and putting CuSO prepared in the step 2)4Solution and Fe2(NO3)3Adding 2mL and 8mL of the solution into a flask respectively, then adding 8mL of anhydrous ethylenediamine and 0.73 mL of hydrazine hydrate with the mass fraction of 80%, uniformly mixing, and heating in a water bath at 75 ℃ for 1.5 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and drying the reaction product at the temperature of 60 ℃ for 22h in vacuum to obtain a product, namely Cu0.2Fe0.8A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 88%.
Example 9
Preparation of Cu0.9Fe0.1Bimetallic nanosheet
1) Preparing 10mol/L NaOH solution: dissolving 100g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.3mol/L Cu (NO)3)2Solution, 0.3mol/L Fe2(SO4)3Solution: 5.63g of Cu (NO)3)212.0g of Fe2(SO4)3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting Cu (NO) prepared in the step 2)3)2Solution and Fe2(NO3)3Adding 9mL and 1mL of the solution into a flask respectively, then adding 7mL of anhydrous ethylenediamine and 6mL of 1mol/L ascorbic acid solution, uniformly mixing, and heating in a 70 ℃ water bath for 1.0 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 50 ℃ for 22h to obtain a product, namely Cu0.1Fe0.9A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 90%.
Example 10
Preparation of Cu0.7Fe0.3Bimetallic nanosheet
1) Preparing 10mol/L NaOH solution: dissolving 100g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.2mol/L Cu (NO)3)2Solution, 0.2mol/L Fe2(SO4)3Solution: 3.75g of Cu (NO)3)28.0g of Fe2(SO4)3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting Cu (NO) prepared in the step 2)3)2Solution and Fe2(NO3)3Adding 7mL and 3mL of the solution into a flask respectively, then adding 4mL of anhydrous ethylenediamine and 0.3 mL of hydrazine hydrate with the mass fraction of 80%, uniformly mixing, and heating in a water bath at 75 ℃ for 0.5 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction productVacuum drying at 55 ℃ for 24h to obtain a product, namely Cu0.7Fe0.3A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 94%.
Example 11
Preparation of Cu0.5Fe0.5Bimetallic nanosheet
1) Preparing 15mol/L NaOH solution: dissolving 150g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.3mol/L Cu (NO)3)2Solution, 0.3mol/L FeCl3Solution: 5.63g of Cu (NO)3)24.86g of FeCl3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting Cu (NO) prepared in the step 2)3)2Solution and Fe2(NO3)3Adding 5mL and 5mL of solution into a flask respectively, then adding 5mL of anhydrous ethylenediamine and 0.4 mL of hydrazine hydrate with the mass fraction of 80%, uniformly mixing, and heating in a water bath at 70 ℃ for 1.5 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 55 ℃ for 24 hours to obtain a product, namely Cu0.5Fe0.5A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 93%.
Example 12
Preparation of Cu0.6Fe0.4Bimetallic nanosheet
1) Preparing 10mol/L NaOH solution: dissolving 100g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.4mol/L CuSO4Solution, 0.4mol/L Fe2(SO4)3Solution: 7.50g of Cu (NO)3)216.00g of Fe2(SO4)3Dissolving in different beakers with deionized waterAfter completely dissolving, respectively transferring the solution into different 100mL volumetric flasks, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting Cu (NO) prepared in the step 2)3)2Solution and Fe2(NO3)3Adding 6mL and 4mL of the solution into a flask respectively, then adding 9.3mL of anhydrous ethylenediamine and 0.5mL of hydrazine hydrate with the mass fraction of 80%, uniformly mixing, and heating in a water bath at 75 ℃ for 1.0 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 60 ℃ for 22h to obtain a product, namely Cu0.6Fe0.4A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 93%.
Example 13
Preparation of Cu0.4Fe0.6Bimetallic nanosheet
1) Preparing 15mol/L NaOH solution: dissolving 150g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.1mol/L CuCl2Solution, 0.3mol/L FeCl3Solution: 1.34g of CuCl21.62g of FeCl3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting Cu (NO) prepared in the step 2)3)2Solution and Fe2(NO3)3Adding 4mL and 6mL of the solution into a flask respectively, then adding 2.5mL of anhydrous ethylenediamine and 3mL of 1mol/L ascorbic acid solution, uniformly mixing, and heating in a 70 ℃ water bath for 1.0 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 50 ℃ for 22h to obtain a product, namely Cu0.4Fe0.6A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 92%.
Example 14
Preparation of Cu0.8Fe0.2Bimetallic nanosheet
1) Preparing a 20mol/L NaOH solution: dissolving 200g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.3mol/L Cu (NO)3)2Solution, 0.3mol/L Fe (NO)3)3Solution: 5.63g of Cu (NO)3)27.26g of Fe (NO)3)3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting Cu (NO) prepared in the step 2)3)2Solution and Fe2(NO3)3Adding 8mL and 2mL of the solution into a flask respectively, then adding 6mL of anhydrous ethylenediamine and 9mL of 1mol/L glucose solution, uniformly mixing, and heating in a water bath at 60 ℃ for 1.0 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 50 ℃ for 22h to obtain a product, namely Cu0.8Fe0.2A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 94%.
Example 15
Preparation of Cu0.6Fe0.4Bimetallic nanosheet
1) Preparing 15mol/L NaOH solution: dissolving 150g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.1mol/L Cu (NO)3)2Solution, 0.1mol/L Fe (NO)3)3Solution: 1.88g of Cu (NO)3)22.42g of Fe (NO)3)3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting Cu (NO) prepared in the step 2)3)2Solution and Fe2(NO3)3Adding 6mL and 4mL of the solution into a flask respectively, then adding 2.5mL of anhydrous ethylenediamine and 0.1mL of hydrazine hydrate with the mass fraction of 80%, uniformly mixing, and heating in a 70 ℃ water bath for 1.0 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 50 ℃ for 22h to obtain a product, namely Cu0.6Fe0.4A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 92%.
Example 16
Preparation of Cu0.5Fe0.5Bimetallic nanosheet
1) Preparing a 25mol/L NaOH solution: dissolving 250g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.3mol/L Cu (NO)3)2Solution, 0.3mol/L Fe2(SO4)3Solution: 5.63g of Cu (NO)3)212.00g of Fe2(SO4)3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting Cu (NO) prepared in the step 2)3)2Solution and Fe2(NO3)3Adding 5mL and 5mL of the solution into a flask respectively, then adding 4.0 mL of anhydrous ethylenediamine and 0.6 mL of hydrazine hydrate with the mass fraction of 80%, uniformly mixing, and heating in a 70 ℃ water bath for 1.0 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 50 ℃ for 24 hours to obtain a product, namely Cu0.5Fe0.5A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 92%.
Example 17
Preparation of Cu0.7Fe0.3Bimetallic nanosheet
1) Preparing 15mol/L NaOH solution: dissolving 150g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.1mol/L Cu (NO)3)2Solution, 0.1mol/L FeCl3Solution: 1.88g of Cu (NO)3)21.62g of FeCl3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting Cu (NO) prepared in the step 2)3)2Solution and Fe2(NO3)3Adding 7mL and 3mL of the solution into a flask respectively, then adding 3.3mL of anhydrous ethylenediamine and 0.2mL of hydrazine hydrate with the mass fraction of 80%, uniformly mixing, and heating in a water bath at 80 ℃ for 1.0 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 60 ℃ for 22h to obtain a product, namely Cu0.7Fe0.3A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 95%.
Example 18
Preparation of Cu0.2Fe0.8Bimetallic nanosheet
1) Preparing 15mol/L NaOH solution: dissolving 150g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.2mol/L CuSO4Solution, 0.2mol/L FeCl3Solution: 3.75g of CuSO43.24g of FeCl3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 200mL of NaOH solution prepared in the step 1) into a flask, and putting Cu (NO) prepared in the step 2)3)2Solution and Fe2(NO3)3Adding 2mL and 8mL of the solution into a flask respectively, adding 3.5mL of anhydrous ethylenediamine and 10mL of 1mol/L ascorbic acid solution, mixing uniformly, and adding water at 80 DEG CBath heating for 1.0 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and vacuum drying at 60 ℃ for 24 hours to obtain a product, namely Cu0.2Fe0.8A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 93%.
Example 19
Preparation of Cu0.4Fe0.6Bimetallic nanosheet
1) Preparing 10mol/L NaOH solution: dissolving 100g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.3mol/L CuSO4Solution, 0.3mol/L Fe2(NO3)3Solution: 4.79g of CuSO47.26g of Fe2(NO3)3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 100mL of NaOH solution prepared in the step 1) into a flask, and putting CuSO prepared in the step 2)4Solution and Fe2(NO3)3Adding 4mL and 6mL of the solution into a flask respectively, then adding 5mL of anhydrous ethylenediamine and 15 mL of 1mol/L glucose solution, uniformly mixing, and heating in a water bath at 60 ℃ for 1 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and drying the reaction product at the temperature of 45 ℃ for 24 hours in vacuum to obtain a product, namely Cu0.4Fe0.6A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 90%.
Example 20
Preparation of Cu0.5Fe0.5Bimetallic nanosheet
1) Preparing 15mol/L NaOH solution: dissolving 150g of NaOH in a beaker by using deionized water, transferring the solution into a 250mL volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing 0.1mol/L CuNO3Solution, 0.1mol/L Fe2(NO3)3Solution: 1.88g of CuNO32.42g of Fe2(NO3)3Dissolving the raw materials in different beakers by using deionized water respectively, transferring the raw materials into different 100mL volumetric flasks respectively after the raw materials are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting 100mL of NaOH solution prepared in the step 1) into a flask, and putting CuSO prepared in the step 2)4Solution and Fe2(NO3)3Adding 5mL and 5mL of the solution into a flask respectively, then adding 2.5mL of anhydrous ethylenediamine and 3mL of 1mol/L ascorbic acid solution, uniformly mixing, and heating in a 70 ℃ water bath for 1 h;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and drying the reaction product at 55 ℃ for 20 hours in vacuum to obtain a product, namely Cu0.5Fe0.5A bimetallic nanosheet. The degradation rate of the Congo red catalyzed by the nanosheets is 95%.
Through comparison among the examples 1, 2, 3, 4 and 6, the Cu-Fe bimetallic nanosheets prepared in different examples show a tendency that the efficiency of catalyzing degradation of Congo red as a catalyst increases and then decreases with the increase of the content of Fe salt, when the molar ratio of the Cu salt to the Fe salt is 1: 0.66; the molar ratio of the total molar amount of the Cu salt and the Fe salt to the anhydrous ethylenediamine is 1: 37.4; when the molar ratio of the total molar amount of the Cu salt and the Fe salt to the reducing agent is 1:1.64, the degradation rate of the catalytic Congo red is highest, and from the viewpoint of catalytic effect, the molar ratio of the Cu salt to the Fe salt is preferably 1:0.66, and the molar ratio of the total molar amount of the Cu salt and the Fe salt to the anhydrous ethylenediamine is preferably 1: 37.4; the molar ratio of the total molar amount of the Cu salt and the Fe salt to the reducing agent is preferably 1: 1.64.
Claims (8)
1. A Cu-Fe bimetallic nanosheet is characterized in that the Cu-Fe bimetallic nanosheet is in a shape controlled by changing the molar ratio of Cu salt to Fe salt.
2. The preparation method of the Cu-Fe bimetallic nanosheet as claimed in claim 1, which is characterized in that the Cu-Fe bimetallic nanosheet is prepared by a chemical reduction method, and specifically comprises the following steps:
1) preparing NaOH solution: dissolving NaOH in a beaker by using deionized water, transferring the solution to a volumetric flask after the solution is cooled, and washing, fixing the volume and shaking up for later use;
2) preparing a Cu salt solution and an Fe salt solution: dissolving Cu salt and Fe salt in different beakers respectively by using deionized water, transferring the dissolved Cu salt and Fe salt to different volumetric flasks respectively after the Cu salt and Fe salt are completely dissolved, and washing, fixing the volume and shaking up for later use;
3) putting the NaOH solution prepared in the step 1) into a flask, adding the Cu salt solution and the Fe salt solution prepared in the step 2) into the single-neck flask, then adding a complexing agent and a reducing agent, uniformly mixing, and heating in a water bath;
4) after the water bath heating in the step 3) is finished, centrifugally separating the reaction product, and drying to obtain the product, namely the Cu-Fe bimetallic nanosheet.
3. The preparation method of Cu-Fe bimetallic nanosheets as in claim 2, wherein the concentration of NaOH solution in step 1) is 10-30 mol/L, preferably 15-25 mol/L.
4. The method for preparing Cu-Fe bimetallic nanosheets as in claim 2, wherein the Cu salt in step 2) is Cu (NO)3)2、CuSO4Or CuCl2The Fe salt is Fe (NO)3)3、Fe2(SO4)3Or FeCl3。
5. The method for preparing Cu-Fe bimetallic nanosheets as in claim 2, wherein the molar ratio of the Cu salt to the Fe salt in step 3) is 1:0.11-4, the molar ratio of the total number of moles of the Cu salt and the Fe salt to the molar ratio of the complexing agent is 1:20-50, and the molar ratio of the total number of moles of the Cu salt and the Fe salt to the molar ratio of the reducing agent is 1: 1-5.
6. The method for preparing Cu-Fe bimetallic nanosheets as in claim 2, wherein in step 3) the complexing agent is anhydrous ethylenediamine and the reducing agent is ascorbic acid, glucose or hydrazine hydrate.
7. The preparation method of the Cu-Fe bimetallic nanosheet as claimed in claim 2, wherein the water bath temperature in step 3) is 60-80 ℃, and the water bath heating time is 0.5-1.5 h.
8. The preparation method of Cu-Fe bimetallic nanosheets as in claim 2, wherein the drying temperature in step 4) is 45-60 ℃ and the drying time is 20-24 h.
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Citations (2)
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| CN105290419A (en) * | 2015-11-04 | 2016-02-03 | 郑州大学 | Fishbone-shaped core-shell structure nanometer nickel-copper alloy powder and preparation method thereof |
| CN110883339A (en) * | 2018-09-10 | 2020-03-17 | 临沂大学 | Method for preparing superfine metal powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105290419A (en) * | 2015-11-04 | 2016-02-03 | 郑州大学 | Fishbone-shaped core-shell structure nanometer nickel-copper alloy powder and preparation method thereof |
| CN110883339A (en) * | 2018-09-10 | 2020-03-17 | 临沂大学 | Method for preparing superfine metal powder |
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| Title |
|---|
| R. D. NOCE等: "Magnetic properties of Fe–Cu alloys prepared by pulsed electrodeposition", 《JOURNAL OF APPLIED PHYSICS》, vol. 106, 9 November 2009 (2009-11-09), pages 093907 - 1 * |
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