Preparation method of a slice-stacked CuCoO2 and application thereof

By preparing stacked CuCoO2 nanomaterials, the problem of low treatment efficiency of organic pollutants in industrial wastewater is solved, providing an efficient, stable and low-cost material solution suitable for the industrialization of optoelectronic functional materials.

CN119612604BActive Publication Date: 2025-11-21INST OF PHYSICS HENAN ACAD OF SCI +1
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Patent Information

Application Number
CN202411819018.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-11
Publication Date
2025-11-21
Estimated Expiration
2044-12-11

AI Technical Summary

Technical Problem

Existing technologies are insufficient for efficiently treating organic pollutants in industrial wastewater, and the morphological differences in copper-based metal oxide materials lead to unstable performance.

Method used

A method for preparing CuCoO2 nanomaterials by stacking sheets was adopted. By combining hydrothermal reaction and surfactant, the morphology and composition of the material were controlled, and CuCoO2 nanosheets with large specific surface area and multiple active sites were prepared.

Benefits of technology

It achieves efficient adsorption and degradation of organic pollutants, has good material stability, is simple to operate, and has low cost, making it suitable for the industrialization of optoelectronic functional materials.

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Abstract

The application discloses a preparation method of CuCoO2 nanosheet stacking material and application thereof, and the preparation comprises the following steps: dissolving copper nitrate, cobalt nitrate, a surfactant and a mineralizer in a solvent, and forming a suspension A after strong stirring, then transferring the suspension A into an autoclave to perform a hydrothermal reaction by heating, cooling to room temperature after the hydrothermal reaction is completed, and then cleaning and drying by using deionized water and anhydrous ethanol to obtain the product. The method can prepare the CuCoO2 electrode with a sheet stacking morphology in one step, and can be widely applied to related fields as an adsorption and degradation material.
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Description

Technical Field

[0001] This invention relates to the field of metal oxides, specifically to a method for preparing CuCoO2 nanosheet stacked materials and their applications. Background Technology

[0002] Organic pollutants in industrial wastewater pose a serious threat to human life and health. How to efficiently treat organic pollutants in water bodies has become a crucial issue in current scientific research and engineering technology. In recent years, copper-based metal oxides have attracted considerable attention for their advantages of low cost, high stability, and good activity in the catalytic degradation of organic pollutants. Furthermore, 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 efficiency of organic pollutants.

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

[0004] The purpose of this invention is to design a method for preparing stacked CuCoO2 with advantages such as low cost, simple operation, and high sample adsorption and degradation performance.

[0005] To achieve the above-mentioned technical effects, the present invention is implemented through the following technical solution: a method for preparing stacked CuCoO2 sheets, characterized by comprising the following steps:

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

[0007] S2. Weigh out the mineralizer and surfactant in a mass ratio of 4:1 to 2. Then add the mineralizer and surfactant to the solution A obtained in S2. Stir vigorously for 0.5 to 3 hours under strong stirring conditions to obtain suspension B.

[0008] S3. Transfer the suspension B from step S2 to the lining of the autoclave, seal the autoclave, place it in an oven and heat it to 130-150°C, and carry out a hydrothermal reaction for 23-26 hours until the hydrothermal reaction is completed. After the autoclave has cooled to room temperature naturally, open the autoclave and take out the suspension C.

[0009] S4. After the reactor body cools naturally to room temperature, open the reactor body and remove the precipitate. The reaction product is washed alternately with deionized water and anhydrous ethanol, centrifuged 6 times, and then dried to obtain 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 mineralizing agent is one of sodium hydroxide and potassium hydroxide, or a mixture of the two.

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

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

[0014] Preferably, in S3, the filling ratio of the suspension B transferred into the liner 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 this invention are:

[0017] The method of stacked CuCoO2 used in this invention has a relatively mature and inexpensive technical route. At the same time, CuCoO2 has a stacked morphology, which has a large specific surface area, many active sites, and the material is resistant to acid and alkali, thus overcoming the defects of few active sites and poor stability of materials in current degradation processes.

[0018] The preparation process provided by this invention has the advantages of simple operation, easy parameter control, green and environmentally friendly, high yield, low temperature and rapid preparation, and low cost. It can be widely used in the preparation of novel optoelectronic functional materials based on copper-iron ore CuCoO2, which is conducive to the development and industrialization of novel optoelectronic functional materials. Attached Figure Description

[0019] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0020] Figure 1 The field emission scanning electron image of the sample prepared in Example 1 of this invention;

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

[0022] Figure 3 The field emission scanning electron image of the sample prepared in Example 2 of the present invention is shown. Detailed Implementation

[0023] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0024] Example 1

[0025] A hydrothermal preparation method for stacked CuCoO2 sheets, 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 of deionized water and stir continuously for 1 hour to obtain mixed solution A;

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

[0028] 1.3 Transfer the mixed solution B from step 2.2 to a 100mL 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 complete, allow the vessel to cool naturally to room temperature, then open the vessel and pour out the suspension C;

[0030] 1.5. Pour the suspension into a 50mL centrifuge tube and centrifuge with deionized water and alcohol six times in sequence until the supernatant is clear and colorless. Then discard the supernatant.

[0031] 1.6. Place the centrifuge tubes from 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 plate-like CuCoO2, including 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 again for 2 hours to form suspension A;

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

[0036] 1.3 After the reaction is complete, allow the vessel to cool naturally to room temperature before opening the vessel and removing 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] The morphology of the sample obtained in Implementation 1 differs from that of the sample obtained in Implementation 2. The stacked CuCoO2 material obtained in Implementation 1 has a larger specific surface area than the blocky CuCoO2 material, and can more effectively adsorb and degrade organic pollutants.

Claims

1. A method for preparing stacked CuCoO2 sheets, characterized in that, It consists of the following steps: S1. Weigh out copper salt and cobalt salt in a molar ratio of 1:0.8-2, then dissolve them simultaneously in 70 mL of deionized water and stir evenly for 0.5-3 h to obtain solution A; S2. Weigh out the mineralizer and surfactant in a mass ratio of 4:1 to 2. Then add the mineralizer and surfactant to the solution A obtained in S2. Stir vigorously for 0.5 to 3 hours under strong stirring conditions to obtain suspension B. S3. Transfer the suspension B from step S2 to the lining of the autoclave, seal the autoclave, place it in an oven and heat it to 130-150°C, and carry out a hydrothermal reaction for 23-26 hours until the hydrothermal reaction is completed. After the autoclave has cooled to room temperature naturally, open the autoclave and take out the suspension C. S4. After the reactor body cools naturally to room temperature, open the reactor body and remove the precipitate. The reaction product is washed alternately with deionized water and anhydrous ethanol, centrifuged 6 times, and then dried to obtain powdered stacked CuCoO2 material. In S2, the surfactant is sodium dodecyl sulfate.

2. The method for preparing 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 stacked CuCoO2 according to claim 1, characterized in that, In S2, the mineralizing agent is one of sodium hydroxide and potassium hydroxide, or a mixture of the two.

4. The method for preparing stacked CuCoO2 according to claim 1, characterized in that, In S3, the autoclave is a stainless steel autoclave with a polytetrafluoroethylene lining.

5. The method for preparing stacked CuCoO2 according to claim 1, characterized in that, In S3, the filling ratio of the suspension B transferred to the liner of the autoclave is 70%.

6. The application of a stacked CuCoO2 according to any one of claims 1-5, characterized in that, The application of stacked CuCoO2 sheets in the adsorption and degradation of organic pollutants.

Citation Information

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