CN111924890B - Preparation method of CoO (OH) nanoflower - Google Patents
Preparation method of CoO (OH) nanoflower Download PDFInfo
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- CN111924890B CN111924890B CN202010628798.XA CN202010628798A CN111924890B CN 111924890 B CN111924890 B CN 111924890B CN 202010628798 A CN202010628798 A CN 202010628798A CN 111924890 B CN111924890 B CN 111924890B
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- 239000002057 nanoflower Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 12
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims abstract description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 12
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 11
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
- 230000000536 complexating effect Effects 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 abstract description 10
- 239000010941 cobalt Substances 0.000 abstract description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 abstract description 8
- 239000001301 oxygen Substances 0.000 abstract description 8
- 238000001556 precipitation Methods 0.000 abstract description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000008139 complexing agent Substances 0.000 abstract description 4
- 239000007800 oxidant agent Substances 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 13
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 8
- 238000010668 complexation reaction Methods 0.000 description 5
- 229910021397 glassy carbon Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 150000003623 transition metal compounds Chemical class 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 229910001315 Tool steel Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000004502 linear sweep voltammetry Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of CoO (OH) nanoflower, which uses cobalt chloride as a cobalt source and disodium ethylenediamine tetraacetate (EDTA-2 Na) as a complexing agent, and adopts the complexing agent to complex the cobalt source to prepare Co 2+ EDTA complex, hydrogen peroxide as oxidant and complex homogeneous precipitation to prepare nanometer level ultrathin laminated CoO (OH) nanoflower. The preparation method provided by the invention is simple, mild in condition, safe, nontoxic and low in cost, and the obtained CoO (OH) nanoflower has a unique structure and good stability, has good catalytic activity and stability of Oxygen Evolution Reaction (OER) in alkaline potassium hydroxide solution, and has a good application prospect in electrochemical aspects.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a method for preparing CoO (OH) nanoflowers by a complexation homogeneous precipitation method, wherein the CoO (OH) nanoflowers are used as a catalyst to show higher catalytic activity and stability for oxygen precipitation reaction under an alkaline condition.
Background
Noble metal oxide (RuO) 2 And IrO 2 ) Is considered as the most advanced Oxygen Evolution Reaction (OER) catalyst, having high activity in acidic and basic media. However, their large-scale application is greatly limited due to their high cost, scarcity and low stability. Research into the replacement of conventional noble metal catalysts with inexpensive, high-reserves, high-catalytic-activity electrolyzed water catalysts has been continued and tremendous progress has been made.
Currently, cobalt has been widely used in various fields, mainly in battery materials, cemented carbide, tool steel, magnetic materials, and the like; while cobalt in the form of a compound is mainly used as a catalyst, reagent, desiccant, dye, etc. The cobalt-based transition metal compound has the advantages of low price, simple preparation process, strong corrosion resistance in alkaline solution and the like, and shows good catalytic activity of oxygen precipitation and hydrogen precipitation, so the cobalt-based transition metal compound is considered as one of catalyst materials with potential application value. The cobalt nano-sheet has large specific surface area and high stability, has good oxygen evolution electrocatalytic performance under alkaline conditions, can save energy sources, and has important application prospect in the electrolysis industry. At present, most of cobalt-containing nano materials are obtained by an electrochemical deposition method, and the method is relatively complex.
Disclosure of Invention
The invention aims to provide a method for preparing CoO (OH) nanoflower, which is simple and mild in condition.
Aiming at the purposes, the technical scheme adopted by the invention comprises the following steps: 1. according to the mole ratio of cobalt chloride to disodium ethylenediamine tetraacetate of 1:0.5-1:2, respectively dissolving cobalt chloride solid and disodium ethylenediamine tetraacetate solid in deionized water, then mixing the two solutions, uniformly stirring the obtained mixed solution at room temperature and fully reacting to obtain Co 2+ EDTA complexing solution.
2. Adding sodium hydroxide aqueous solution into the Co prepared in the step 1 2+ In EDTA complex solution, stirring uniformly to make pH of the solution be 12-14, adding hydrogen peroxide, and making reaction for 3-24 hr at 50-95 deg.C, in which H 2 O 2 The mol ratio of the cobalt ions to the cobalt ions is 1:1-1:10; and after the reaction is finished, centrifuging, washing and drying to obtain the CoO (OH) nanoflower.
In the step 1, the molar ratio of the cobalt chloride to the disodium edetate is preferably 1:1 to 1:1.5.
In the step 1, the concentration of cobalt ions in the obtained mixed solution is 0.001-0.05 mol/L, preferably 0.005-0.01 mol/L.
In the above step 2, the concentration of the aqueous sodium hydroxide solution is preferably 1.0 to 5.0mol/L.
In the above step 2, the H is preferably 2 O 2 The molar ratio of the cobalt ions is 1:2-1:6.
In the step 2, it is more preferable to stir the mixture at 60 to 90℃for 3 to 12 hours.
The beneficial effects of the invention are as follows:
the invention adopts a complexation homogeneous precipitation method, firstly uses complexing agent EDTA-2Na to complex cobalt source, when in operation, the complexing agent is slightly excessive to ensure complete complexation of cobalt source, then NaOH is added to ensure that the pH value of the solution is 12-14, and meanwhile OH is provided - Then use H 2 O 2 CoO (OH) nanoflower formed of nanoscale ultrathin lamellar structures is simply and efficiently prepared as an oxidizing agent by controlling the amount of the oxidizing agent so that the complex bonds are slowly broken and new bonds are formed. The preparation method is simple, safe and nontoxic, has low cost, and the obtained CoO (OH) nanoflower has unique structure and good stability, has good OER catalytic activity and stability in alkaline potassium hydroxide solution, and has good application prospect in electrochemical aspect.
Drawings
FIG. 1 is an XRD pattern of CoO (OH) nanoflower obtained in example 1.
FIG. 2 is a scanning electron micrograph of CoO (OH) nanoflower obtained in example 1.
Fig. 3 is a partial enlarged view of fig. 2.
FIG. 4 is a field emission transmission electron micrograph of CoO (OH) nanoflower obtained in example 1.
FIG. 5 is a scanning electron micrograph of CoO (OH) nanoflower obtained in example 2.
FIG. 6 is a scanning electron micrograph of CoO (OH) nanoflower obtained in example 3.
FIG. 7 is a CoO (OH) nanoflower catalyst prepared in example 1 with a commercial RuO 2 Test chart of catalyst oxygen evolution reaction performance.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, but the scope of the present invention is not limited to these examples.
Example 1
1. 0.24g (1 mmol) of cobalt chloride solid with purity of 99% or more and 0.38g (1 mmol) of EDTA-2Na solid with purity of 99% or more are respectively dissolved in 80mL of deionized water, and the solution is fully dissolved and then fixed in a 100mL volumetric flask. The resulting aqueous cobalt chloride solution is thenMixing with EDTA-2Na water solution to make cobalt ion concentration in the mixed solution be 0.005mol/L, stirring and making them react for 3 hr at room temperature to make them implement full complexation so as to obtain Co 2+ EDTA complexing solution.
2. Under stirring, 20mL of Co prepared in step 1 was added 2+ Dropwise adding 5mol/L NaOH aqueous solution into EDTA complexing solution, regulating pH value of the solution to 13, then adding 20 mu L9.79 mol/L H 2 O 2 The aqueous solution was stirred slowly for 3 hours in a water bath at 90 ℃. And after the reaction is finished, centrifugal separation is carried out, washing is carried out for 3 times by using water and 1 time by using ethanol, and finally vacuum drying is carried out at 60 ℃ to obtain the CoO (OH) nanoflower. The XRD pattern of fig. 1 shows that the resulting sample is CoO (OH), consistent with its standard card. As can be seen from fig. 2 to 4, the obtained CoO (OH) is a nanoflower composed of an ultrathin two-dimensional lamellar structure, and has regular morphology and uniform size.
Example 2
In step 2 of this example, the mixture was slowly stirred in a water bath at 80℃for 5 hours, and the same procedure as in example 1 was followed to obtain CoO (OH) nanoflower (see FIG. 5).
Example 3
1. 0.48g (2 mmol) of cobalt chloride solid with purity of more than 99% and 0.76g (2 mmol) of EDTA-2Na solid with purity of more than 99% are respectively dissolved in 80mL of deionized water, and the solution is fully dissolved and then fixed in a 100mL volumetric flask. Mixing the obtained cobalt chloride aqueous solution and EDTA-2Na aqueous solution to make cobalt ion concentration in the mixed solution be 0.01mol/L, stirring at room temperature for 3 hr to make them implement full complexation so as to obtain Co 2+ EDTA complexing solution.
2. Under stirring, 20mL of Co prepared in step 1 was added 2+ Adding 5mol/L NaOH aqueous solution into EDTA complex solution, regulating pH value of the solution to 12, then adding 120 mu L9.79 mol/L H 2 O 2 The aqueous solution was stirred uniformly and then allowed to stand at 60℃for 24 hours. Otherwise, the same procedure as in example 1 was conducted to obtain CoO (OH) nanoflower (see fig. 6).
To demonstrate the beneficial effects of the present invention, the inventors prepared CoO (OH) nanoflower prepared in example 1 with commercial RuO 2 The catalysts were compared for Oxygen Evolution (OER) performance. First, 2mg CoO (OH) nanoflower or commercialRuO (Ruo) melting 2 The catalyst was dispersed in a solution of 800. Mu.L of water, 10. Mu.L of 5% Nafion and 200. Mu.L of isopropanol, and sonicated uniformly to prepare a catalyst solution. And uniformly dripping 4 mu L of the catalyst solution on the polished glassy carbon electrode, and drying at 60 ℃ to obtain the pretreated glassy carbon electrode. The Linear Sweep Voltammetry (LSV) of the resulting treated glassy carbon electrode was measured with a CHI 660E electrochemical workstation in a standard three electrode system at room temperature. The results of FIG. 7 show that at N 2 In saturated 1M KOH solution, the oxygen evolution reaction performance of the CoO (OH) nanoflower of the invention is superior to that of the commercial RuO 2 A catalyst.
Claims (5)
1. The preparation method of the CoO (OH) nanoflower is characterized by comprising the following steps:
(1) According to the mole ratio of cobalt chloride to disodium ethylenediamine tetraacetate of 1:0.5-1:2, respectively dissolving cobalt chloride solid and disodium ethylenediamine tetraacetate solid in deionized water, and then mixing the two solutions, wherein the cobalt ion concentration in the obtained mixed solution is 0.001-0.05 mol/L; stirring the obtained mixed solution uniformly at room temperature and fully reacting to obtain Co 2+ -EDTA complexing solution;
(2) Adding 1.0-5.0 mol/L sodium hydroxide aqueous solution into Co prepared in the step (1) 2+ In EDTA complex solution, stirring uniformly to make pH of the solution be 12-14, adding hydrogen peroxide, and making reaction for 3-24 hr at 50-95 deg.C, in which H 2 O 2 The mol ratio of the cobalt ions to the cobalt ions is 1:1-1:10; and after the reaction is finished, centrifuging, washing and drying to obtain the CoO (OH) nanoflower.
2. The method for preparing CoO (OH) nanoflower according to claim 1, wherein: in the step (1), the molar ratio of the cobalt chloride to the disodium ethylenediamine tetraacetate is 1:1-1:1.5.
3. The method for preparing CoO (OH) nanoflower according to claim 1, wherein: in the step (1), the concentration of cobalt ions in the obtained mixed solution is 0.005-0.01 mol/L.
4. The method for preparing CoO (OH) nanoflower according to claim 1, wherein: in step (2), the H 2 O 2 The molar ratio of the cobalt ions is 1:2-1:6.
5. The method for preparing CoO (OH) nanoflower according to claim 1, wherein: in the step (2), stirring and reacting for 3-12 hours at 60-90 ℃.
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JP5017747B2 (en) * | 2001-04-23 | 2012-09-05 | 株式会社豊田中央研究所 | Cobalt oxide hydroxide plate-like particles |
JP4669214B2 (en) * | 2003-09-30 | 2011-04-13 | 株式会社田中化学研究所 | Cobalt oxyhydroxide particles and method for producing the same |
CN102344173A (en) * | 2011-10-25 | 2012-02-08 | 中信大锰矿业有限责任公司 | Method for producing lithium cobaltite by preparing hydroxyl trivalent cobalt oxide through wet chemical reaction |
CN102689933A (en) * | 2012-03-15 | 2012-09-26 | 湖南红太阳电源新材料股份有限公司 | Method for producing hydroxy cobalt oxide |
CN103232075B (en) * | 2013-04-11 | 2015-06-03 | 湖南雅城新材料发展有限公司 | Preparation method for cobalt oxyhydroxide |
CN107445213B (en) * | 2016-06-01 | 2021-11-02 | 中国科学院大连化学物理研究所 | Hollow hexahydric cyclic cobalt oxyhydroxide nano material and preparation method thereof |
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A cobalt oxyhydroxide-modified upconversion nanosystem for sensitive fluorescence sensing of ascorbic acid in human plasma;Yao Cen 等;《Nanoscale》;第7卷;13951 * |
Light-Assisted Synthesis of Metal Oxide Heirarchical Structures and Their Catalytic Applications;Cecil K. King’ondu 等;《J. Am. Chem. Soc》;第133卷;4186–4189 * |
Ultrathin CoOOH Oxides Nanosheets Realizing Efficient Photocatalytic Hydrogen Evolution;Shi He 等;《J. Phys. Chem. C》;第119卷;26362−26366 * |
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