Preparation method and application of sheet-stacked CuCoO2

Abstract

The invention discloses a preparation method and application of a CuCoO2 nanosheet stacked material, and the preparation method comprises the following steps: dissolving copper nitrate, cobalt nitrate, a surfactant and a mineralizing agent in a solvent, intensely stirring to form a suspension A, transferring the suspension A into a high-pressure kettle, heating, and carrying out a hydrothermal reaction to obtain the CuCoO2 nanosheet stacked material. After the hydrothermal reaction is finished, cooling to room temperature, washing with deionized water and absolute ethyl alcohol, and drying to obtain a product. The method provided by the invention can be used for preparing the CuCoO2 electrode with the sheet stacking morphology in one step, and the CuCoO2 electrode can be widely applied to related fields as an adsorption and degradation material.

Description

Technical Field

[0001] The present invention relates to the field of metal oxides, and in particular to a preparation method and application of a CuCoO2 nanosheet stacking material. Background Art

[0002] Organic pollutants in industrial wastewater seriously threaten human life and health safety. How to efficiently treat organic pollutants in water has become an important issue in current scientific research and engineering technology. In recent years, copper-based metal oxides have the advantages of low cost, high stability and good activity, and have received great attention in the catalytic degradation of organic pollutants. In addition, multi-component composite transition metal oxides can accelerate interfacial electron transfer through the synergistic effect between different metals, thereby promoting the generation of active free radicals and improving the removal effect of organic pollutants.

[0003] Due to the morphology and size effect, different morphologies of materials will lead to changes in their properties. Therefore, large-scale synthesis of copper-based metal oxides with controllable composition, morphology, and size is of great significance for the preparation of functional materials. Summary of the invention

[0004] The purpose of the present invention is to design a preparation method of sheet-stacked CuCoO2 with the advantages of low cost, simple operation, high sample adsorption and degradation performance, etc.

[0005] In order to achieve the above technical effects, the present invention is implemented by the following technical scheme: A method for preparing sheet stacked CuCoO2, characterized in that it consists of the following steps:

[0006] S1. Weigh copper salt and cobalt salt in a molar ratio of 1:0.8-2, then dissolve them in 70 mL of deionized water and stir evenly for 0.5-3 h to obtain solution A.

[0007] S2, weighing a mineralizer and a surfactant in a mass ratio of mineralizer: surfactant = 4:1-2, and then adding the mineralizer and the surfactant to the solution A obtained in S2, and stirring vigorously for 0.5-3h under strong stirring conditions to obtain a suspension B;

[0008] S3, transferring the suspension B in step S2 to the inner lining of the autoclave, sealing the autoclave body, placing it in an oven and heating it to 130-150° C., and performing a hydrothermal reaction for 23-26 hours. After the hydrothermal reaction is completed, the autoclave body is naturally cooled to room temperature, and the autoclave body is opened to take out the suspension C;

[0009] S4. Wait for the kettle to cool naturally and stand to room temperature, open the kettle and take out the kettle precipitate, wash the reaction product with deionized water and anhydrous ethanol alternately, centrifuge 6 times and then dry to obtain a powdered stacked CuCoO2 material.

[0010] Preferably, in S1, the copper ions in the copper salt are divalent, and the cobalt ions in the cobalt salt are divalent.

[0011] Preferably, in S2, the mineralizer is sodium hydroxide, potassium hydroxide or a mixture of the two.

[0012] Preferably, in S2, the surfactant is one of sodium dodecyl sulfonate, sodium dodecyl sulfate or polyvinyl pyrrolidone.

[0013] Preferably, in S3, the autoclave is a stainless steel autoclave lined with polytetrafluoroethylene.

[0014] Preferably, in S3, the filling ratio of the suspension B transferred to the lining of the autoclave is 70%.

[0015] Another object of the present invention is to provide an application of sheet-stacked CuCoO2, characterized in that the sheet-stacked CuCoO2 is used in the field of adsorption and degradation of organic pollutants.

[0016] The beneficial effects of the present invention are:

[0017] The method of stacking CuCoO2 sheets adopted in the present invention has a relatively mature technical route and is inexpensive. At the same time, CuCoO2 has a sheet stacking morphology, a large specific surface area, many active sites, and acid and alkali resistance, which overcomes the defects of the current degradation material with few active sites and poor stability.

[0018] The preparation process provided by the present invention has the advantages of simple operation, easy control of parameters, green environmental protection, high yield, low temperature and fast, low cost, etc. It can be widely used in the preparation of new optoelectronic functional materials based on delafossilite CuCoO2, which is beneficial to the development and industrialization of new optoelectronic functional materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings required for describing the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other accompanying drawings can be obtained based on these accompanying drawings without paying creative work.

[0020] Figure 1 This is a field emission scanning electron image of the sample prepared in Example 1 of the present invention;

[0021] Figure 2 The X-ray crystal diffraction pattern of the sample prepared in Example 1 of the present invention;

[0022] Figure 3 Field emission scanning electron image of the sample prepared for Example 2 of the present invention. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] Example 1

[0025] A hydrothermal preparation method of sheet stacked CuCoO2, the method is as follows:

[0026] 1.1. Dissolve 15 mmol Cu(NO3)2·3H2O and 15 mmol Co(NO3)3·6H2O in 70 mL deionized water and stir for 1 hour to obtain a mixed solution A.

[0027] 1.2. Add 4 g of sodium hydroxide to the suspension under vigorous stirring, then add 2 g of sodium dodecyl sulfate, and continue to vigorously stir for 1 hour at a stirring rate of 300 rpm to obtain suspension B;

[0028] 1.3. Transfer the mixed solution B in step 2.2 into a 100 mL stainless steel autoclave lined with polytetrafluoroethylene with a filling ratio of 70%. After sealing the autoclave, heat it in an oven at 140°C for 24 hours.

[0029] 1.4. After the reaction is completed, wait for the kettle to cool naturally to room temperature, open the kettle and pour out the suspension C;

[0030] 1.5. Pour the suspension into a 50 mL centrifuge tube and centrifuge it 6 times with deionized water and alcohol respectively until the supernatant is transparent and colorless, then discard the supernatant;

[0031] 1.6. Bake the centrifuge tube precipitate in 1.5 in an oven at 60°C for 12 hours to obtain the desired stacked CuCoO2 powder.

[0032] Example 2

[0033] This embodiment provides a conventional method for preparing hexagonal flake CuCoO2, comprising the following steps:

[0034] 1.1. Dissolve copper nitrate and cobalt nitrate in 70 mL of deionized water, stir for 1 hour, then add 0.1 mol NaOH and stir for another 2 hours to form suspension A;

[0035] 1.2. Add suspension A into a 100 mL polytetrafluoroethylene reactor and heat in an oven at 160°C for 24 hours.

[0036] 1.3. After the reaction is completed, wait for the kettle to cool naturally to room temperature, open the kettle and take out the reaction solution.

[0037] 1.4. The reaction product was washed alternately with deionized water and anhydrous ethanol and then dried at 60° C. for 12 hours to obtain CuCoO2 powder. The CuCoO2 was a hexagonal block sample.

[0038] There are differences in the morphology of the samples obtained in Implementation 1 and Implementation 2. The sheet-stacked CuCoO2 material obtained in Implementation 1 has a larger specific surface area than the bulk CuCoO2 material, and can more effectively adsorb and degrade organic pollutants.

Claims

1. A method for preparing a sheet stacked CuCoO2, characterized in that: It consists of the following steps: S1. Weigh copper salt and cobalt salt in a molar ratio of 1:0.8-2, then dissolve them in 70 mL of deionized water and stir evenly for 0.5-3 h to obtain solution A. S2, weighing a mineralizer and a surfactant in a mass ratio of mineralizer: surfactant = 4:1-2, and then adding the mineralizer and the surfactant to the solution A obtained in S2, and stirring vigorously for 0.5-3h under strong stirring conditions to obtain a suspension B; S3, transferring the suspension B in step S2 to the inner lining of the autoclave, sealing the autoclave body, placing it in an oven and heating it to 130-150° C., and performing a hydrothermal reaction for 23-26 hours. After the hydrothermal reaction is completed, the autoclave body is naturally cooled to room temperature, and the autoclave body is opened to take out the suspension C; S4. Wait for the kettle to cool naturally and stand to room temperature, open the kettle and take out the kettle precipitate, wash the reaction product with deionized water and anhydrous ethanol alternately, centrifuge 6 times and then dry to obtain a powdered stacked CuCoO2 material.

2. The method for preparing a sheet stacked CuCoO2 according to claim 1, characterized in that: In S1, the copper ions in the copper salt are divalent, and the cobalt ions in the cobalt salt are divalent.

3. The method for preparing a sheet stacked CuCoO2 according to claim 1, characterized in that: In S2, the mineralizer is sodium hydroxide, potassium hydroxide or a mixture of the two.

4. The method for preparing a sheet stacked CuCoO2 according to claim 1, characterized in that: In S2, the surfactant is one of sodium dodecyl sulfonate, sodium dodecyl sulfate or polyvinyl pyrrolidone.

5. The method for preparing a sheet stack of CuCoO2 according to claim 1, characterized in that: In S3, the autoclave is a stainless steel autoclave lined with polytetrafluoroethylene.

6. The method for preparing a sheet stack of CuCoO2 according to claim 1, characterized in that: In S3, the suspension B is transferred to the inner lining of the autoclave at a filling ratio of 70%.

7. An application of CuCoO2 stacked sheets, characterized in that: The application of the sheet stacked CuCoO2 in the field of adsorption and degradation of organic pollutants.

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