Preparation method of MXene doped cobalt oxide MOF material

Abstract

The invention discloses a preparation method of an MXene doped cobalt oxide MOF material, and the preparation method comprises the following steps: (1) carrying out stirring I, centrifugation I and drying I on a mixture containing cobalt salt, an alcoholic solution and an MOF ligand to obtain MOF powder; and (2) dispersing the MOF powder and MXene powder into water, stirring II, centrifuging II, drying II, and calcining to obtain the MXene doped cobalt oxide MOF material. According to the method, the cobalt oxide MOF is grown on an MXene lamellar structure through in-situ growth, so that the MXene doped cobalt oxide MOF can be obtained. The MXene has excellent heat and electricity conduction, performance and stability. The invention provides a simple and rapid composite material preparation method which has important practice and research values in the technical field.

Description

Technical Field

[0001] The present application relates to a method for preparing a MXene-doped cobalt oxide MOF material, which belongs to the field of preparation of nanomaterials. Background Art

[0002] With the continuous development of productivity and the improvement of quality of life, people's demands for production and life are getting higher and higher, which has promoted the demand for nanomaterials. Nanomaterials have important applications in energy storage, sensing, catalysis and other fields. After long-term exploration, scientific researchers have developed more and more efficient methods for preparing nanomaterials. MXene itself has excellent thermal conductivity, electrical conductivity, performance and stability, and is extremely suitable for the preparation of composite nanomaterials. This patent explores this and proposes a simple and efficient preparation method. Summary of the invention

[0003] According to one aspect of the present application, a method for preparing a MXene-doped cobalt oxide MOF material is provided, the preparation method comprising the following steps:

[0004] (1) stirring a mixture containing a cobalt salt, an alcohol solution, and a MOF ligand for I, centrifuging for I, and drying for I to obtain a MOF powder;

[0005] (2) dispersing MOF powder and MXene powder into water, stirring II, centrifuging II, drying II, and calcining to obtain the MXene-doped cobalt oxide MOF material;

[0006] The MOF ligand is selected from at least one of 2-methylimidazole and porphyrin.

[0007] Optionally, the MXene powder is selected from at least one of accordion-shaped, multi-layered, and single-layered.

[0008] Optionally, the usage of the cobalt salt, alcohol solution and MOF ligand is: 0.01-10 g: 20-100 mL: 0.5-10 g.

[0009] Optionally, in step (1), the cobalt salt is selected from at least one of cobalt chloride, cobalt nitrate and cobalt acetate.

[0010] Optionally, in step (1), the alcohol solution is selected from at least one of methanol, ethanol and propanol.

[0011] Optionally, the usage ratio of the MOF powder, MXene powder and water is: 0.01-1 g: 0.01-1 g: 1-50 mL.

[0012] Optionally, the time of stirring I and stirring II is independently selected from 1 to 48 hours.

[0013] Optionally, the time of stirring I and stirring II is independently selected from any value among 1h, 5h, 12h, 24h, 36h, 48h or a range value between any two of the above points.

[0014] Optionally, the speeds of centrifugation I and centrifugation II are independently selected from 6000 to 10000 rpm.

[0015] Optionally, the speeds of centrifugation I and centrifugation II are independently selected from any value among 6000 rpm, 7000 rpm, 8000 rpm, 9000 rpm, 10000 rpm or a range between any two of the above points.

[0016] Optionally, the temperatures of drying I and drying II are independently selected from 60 to 100°C.

[0017] Optionally, in step (2), the calcination temperature is 300 to 600° C., and the calcination time is 1 to 12 hours.

[0018] Optionally, the calcination temperature is selected from any value of 300°C, 400°C, 450°C, 500°C, 550°C, 600°C or a range between any two of the above values.

[0019] Optionally, the calcination time is selected from any value of 1 h, 2 h, 4 h, 6 h, 8 h, 10 h, 12 h or a range between any two of the above.

[0020] According to another aspect of the present application, a MXene-doped cobalt oxide MOF material prepared by the preparation method described above is provided.

[0021] This application is implemented using the following technical solutions:

[0022] A method for preparing a MXene-doped cobalt oxide MOF, the preparation method comprising:

[0023] (1) MOF coordination: a certain amount of cobalt salt is dispersed into an alcohol solution, a certain amount of MOF ligand is added, stirred evenly, left to stand for a certain period of time, centrifuged, washed, and dried;

[0024] (2) MXene doping: a certain amount of MXene powder and a certain amount of MOF powder prepared in step (1) are dispersed in water, stirred evenly, and then the two are mixed. After stirring for a period of time at room temperature, the mixture is centrifuged, washed, and dried;

[0025] (3) High temperature calcination: The powder obtained in step (2) is heated and calcined at a high temperature for a certain period of time.

[0026] Optionally, the washing conditions in step (1) and step (2) are: the washing liquid is methanol and water.

[0027] The beneficial effects of this application include:

[0028] 1) The MXene-doped cobalt oxide MOF process provided in this application is simple.

[0029] 2) In the present application, MXene-doped cobalt oxide MOF can be obtained by in-situ growing cobalt oxide MOF on a MXene sheet structure; the MXene itself has excellent thermal and electrical conductivity, performance and stability; the present invention provides a simple and fast method for preparing a composite material, which has important practical and research value in this technical field. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 This is a characterization diagram of the XRD spectrum of the MXene-doped cobalt oxide MOF prepared in Example 1 of the present application. DETAILED DESCRIPTION

[0031] The present application is described in detail below with reference to embodiments, but the present application is not limited to these embodiments.

[0032] Unless otherwise specified, the raw materials in the examples of this application were purchased through commercial channels.

[0033] In the examples of the present application, an X-ray diffractometer is used to perform XRD characterization on the MXene-doped cobalt oxide MOF material.

[0034] Example 1

[0035] Weigh 1.5g of cobalt nitrate hexahydrate, disperse it in 70mL of methanol, add 2g of 2-methylimidazole, stir at room temperature for 1h, and let stand for 24h. Centrifuge at 8000rpm for 10min, wash three times with methanol, and dry at 60℃ to obtain MOF powder. Weigh 0.1g of the above MOF powder and disperse it in 5mL of water; weigh 0.05g of accordion-shaped MXene powder and disperse it in 5mL of water, mix the above two aqueous solutions, stir at room temperature for 12h, centrifuge at 8000rpm for 10min, wash three times with methanol, and dry at 60℃ to obtain MXene-doped MOF powder. The above powder is calcined at 400℃ in air for 2h to obtain MXene-doped cobalt oxide MOF material.

[0036] Example 2

[0037] Weigh 2g of cobalt nitrate hexahydrate, disperse it in 100mL of methanol, add 1.5g of 2-methylimidazole, stir at room temperature for 2h, and let stand for 25h. Centrifuge at 10000rpm for 12min, wash three times with methanol, and dry at 70℃ to obtain MOF powder. Weigh 0.2g of the above MOF powder and disperse it in 10mL of water; weigh 0.1g of multilayer MXene powder and disperse it in 10mL of water, mix the above two aqueous solutions, stir at room temperature for 15h, centrifuge at 10000rpm for 12min, wash three times with methanol, and dry at 70℃ to obtain MXene-doped MOF powder. The above powder is calcined at 500℃ in air for 1h to obtain MXene-doped cobalt oxide MOF material.

[0038] Example 3

[0039] Weigh 1.8g of cobalt nitrate hexahydrate, disperse it in 120mL of methanol, add 1.8g of 2-methylimidazole, stir at room temperature for 2.5h, and let stand for 18h. Centrifuge at 7000rpm for 15min, wash three times with methanol, and dry at 80℃ to obtain MOF powder. Weigh 0.3g of the above MOF powder and disperse it in 20mL of water; weigh 0.3g of accordion-shaped MXene powder and disperse it in 20mL of water, mix the above two aqueous solutions, stir at room temperature for 18h, centrifuge at 7000rpm for 15min, wash three times with methanol, and dry at 80℃ to obtain MXene-doped MOF powder. The above powder is calcined at 600℃ in air for 1.5h to obtain MXene-doped cobalt oxide MOF material. From Figure 1 As can be seen in the figure, MXene-doped cobalt oxide was successfully synthesized.

[0040] The above are only a few embodiments of the present application and do not constitute any form of limitation to the present application. Although the present application is disclosed as above with preferred embodiments, it is not intended to limit the present application. Any technician familiar with the profession, without departing from the scope of the technical solution of the present application, using the technical content disclosed above to make slight changes or modifications are equivalent to equivalent implementation cases and fall within the scope of the technical solution.

Claims

1. A method for preparing a MXene-doped cobalt oxide MOF material, characterized in that: The preparation method comprises the following steps: (1) stirring a mixture containing a cobalt salt, an alcohol solution, and a MOF ligand for I, centrifuging for I, and drying for I to obtain a MOF powder; (2) dispersing MOF powder and MXene powder into water, stirring II, centrifuging II, drying II, and calcining to obtain the MXene-doped cobalt oxide MOF material; The MOF ligand is selected from at least one of 2-methylimidazole and porphyrin.

2. The preparation method according to claim 1, characterized in that: The MXene powder is selected from at least one of an accordion shape, a multi-layer shape, and a single-layer shape.

3. The preparation method according to claim 1, characterized in that: The dosage of the cobalt salt, alcohol solution and MOF ligand is: 0.01-10 g: 20-100 mL: 0.5-10 g.

4. The preparation method according to claim 1, characterized in that: In the step (1), the cobalt salt is selected from at least one of cobalt chloride, cobalt nitrate and cobalt acetate.

5. The preparation method according to claim 1, characterized in that: In the step (1), the alcohol solution is selected from at least one of methanol, ethanol and propanol.

6. The preparation method according to claim 1, characterized in that: The usage ratio of the MOF powder, MXene powder and water is: 0.01-1 g: 0.01-1 g: 1-50 mL.

7. The preparation method according to claim 1, characterized in that: The time of stirring I and stirring II is independently selected from 1 to 48 hours.

8. The preparation method according to claim 1, characterized in that: The speeds of the centrifugation I and the centrifugation II are independently selected from 6000 to 10000 rpm.

9. The preparation method according to claim 1, characterized in that: The temperatures of the drying I and the drying II are independently selected from 60 to 100° C.; Preferably, in the step (2), the calcination temperature is 300 to 600° C., and the calcination time is 1 to 12 hours.

10. The MXene-doped cobalt oxide MOF material prepared by the preparation method according to any one of claims 1 to 9.

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