CN110473712B - MOF derived nanosheet intercalation material, and preparation method and application thereof - Google Patents
MOF derived nanosheet intercalation material, and preparation method and application thereof Download PDFInfo
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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Abstract
The invention discloses an MOF derived nanosheet intercalation material, a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) heating, mixing and stirring the cobalt acetate, the benzimidazole, the methanol and the toluene solution, adding ammonia water to obtain two-dimensional MOF nanosheet Co2bim4Washing with ultrapure water and ethanol, and drying at 80 deg.C for 24 hr; (2) heating the obtained purple powder to 350 ℃ at the heating rate of 1 ℃/min, calcining for 3 h in the air atmosphere, and obtaining porous cobaltosic oxide nanosheets; (3) dispersing porous cobaltosic oxide nanosheets and polyethyleneimine in water, stirring for one hour at room temperature, freeze-drying for 24 hours, then heating to 600-900 ℃ at a heating rate of 2 ℃/min in an argon or nitrogen atmosphere, and calcining for 4 hours to obtain an MOF derived nanosheet intercalation material, namely porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel; the prepared electrode plate is applied to a super capacitor, shows specific capacitance as high as 2251F/g and good rate characteristic, and is a very potential super capacitor material.
Description
Technical Field
The invention relates to a synthesis method of a covalent organic framework film, in particular to an MOF derived nanosheet intercalation material, a preparation method and application thereof.
Background
With the rapid development of global economy, the rapid consumption of petroleum and coal, and the continuously worsening environmental pollution problem, people are forced to make an urgent need for developing new technologies for more efficient, clean and sustainable energy and energy conversion and storage. In recent years, development and utilization of various green energy technologies and clean and renewable new energy technologies, such as electric energy, wind energy, solar energy, tidal energy and the like, have attracted extensive attention.
The super capacitor is a novel energy storage element between a common capacitor and a battery, and has the advantages of wide use temperature range (-20 ℃ to 60 ℃), short charging time, high output power, no pollution, long service life and the like. Electrode materials are one of the key factors determining the performance of the super capacitor, and at present, the super capacitor can be divided into an electric double layer capacitor and a pseudo capacitor according to different mechanisms of stored electric energy. The electrode materials used for electric double layer capacitors are often porous carbon materials (such as activated carbon, carbon aerogel, carbon nanotubes, graphene, etc.); the pseudo capacitor is also called a faraday quasi-capacitor, and the generation mechanism is different from that of an electric double layer capacitor, and the electrode material of the pseudo capacitor is mainly metal oxide and conductive polymer. The effective combination of the materials can possibly obtain the electrode material of the super capacitor with excellent electrochemical performance.
Metal Organic Frameworks (MOFs) are a class of multidimensional periodic network framework materials formed by connecting Organic ligands containing oxygen or nitrogen elements with transition Metal ions. The MOFs crystal has the characteristics of three-dimensional open pore channel, higher specific surface area, regular and adjustable pore structure, pore surface and the like. The MOFs also have a pore channel structure and special properties which are regularly arranged like microporous and mesoporous molecular sieves. In addition, the porous carbon material and the porous metal oxide material prepared by sintering the MOFs material reserve rich pore channel structures of the MOFs material to a certain extent, so that the material can be widely applied to various fields such as catalysis, adsorption, energy storage and the like. However, the MOFs are easy to aggregate, and the metal-organic framework compound is difficult to be uniformly dispersed in a solvent, so that the effective compounding of the metal-organic framework compound and the conductive polymer material is limited.
The aerogel material is in a solid matter form, is one of the solids with the minimum density in the world, and has the characteristics of a porous network structure, a huge specific surface area, controllability of mesoscopic dimensions and the like. Typically, the aerogel material is a silicon aerogel or a carbon aerogel; wherein the carbon aerogel is the only aerogel with conductivity and can be used as an electrode material of an electric double layer super capacitor. However, the electric double layer super capacitor has much lower capacitance than the pseudocapacitance super capacitor, thereby limiting the popularization and application of the material.
Disclosure of Invention
The invention aims to provide an MOF derived nanosheet intercalation material, a preparation method and application thereof aiming at the defects in the prior art, and the material is a two-dimensional MOF nanosheet material Co2(bim)4As a precursor, roasting to obtain a porous cobaltosic oxide nanosheet; the electrostatic binding force of Polyethyleneimine (PEI) on the porous cobaltosic oxide nano sheet material is utilized to realize effective intercalation compounding, and then the porous cobaltosic oxide nano sheet-nitrogen-doped carbon composite aerogel is obtained by roasting; the obtained porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel can show excellent electrochemical performance and cycling stability, and the related preparation method is simple and easy to control, and is suitable for popularization and application.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of an MOF derived nanosheet intercalation material comprises the steps of firstly, preparing a two-dimensional MOF nanosheet material Co2(bim)4As a precursor, roasting to obtain a porous cobaltosic oxide nanosheet; the electrostatic binding force of Polyethyleneimine (PEI) on the porous cobaltosic oxide nano sheet material is utilized to realize effective intercalation compounding, and then the porous cobaltosic oxide nano sheet-nitrogen-doped carbon composite aerogel is obtained by roasting; the method comprises the following steps:
step 1: synthesis of two-dimensional MOF nanosheet material Co2(bim)4
Adding cobalt acetate and benzimidazole (bim) into a mixed solvent of toluene and methanol, and then adding ammonia water as an auxiliary agent; carrying out ultrasonic treatment on the prepared solution for 5 minutes, heating and stirring the solution at the temperature of 60 ℃, and reacting the solution for 12 hours, wherein the mass ratio of cobalt acetate, benzimidazole, methylbenzene, methanol and ammonia water is 0.25: 1-1.2: 47-50: 17-20: 4-10;
step 2: preparation of porous cobaltosic oxide nanosheet
Mixing Co2(bim)4Placing the mixture in a covered crucible, heating the mixture to 350-400 ℃ in a muffle furnace at a heating rate of 2.3 ℃/min, keeping the temperature for 4-6 h, and naturally cooling to obtain black powder, namely the porous cobaltosic oxide nanosheet;
and step 3: preparation of porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel
Dispersing porous cobaltosic oxide nanosheets and Polyethyleneimine (PEI), wherein the molecular weight of PEI is 600, ultrasonically treating for 1h, freeze-drying for one day in a freeze dryer, heating to 600-900 ℃ at the heating rate of 2 ℃/min in the argon or nitrogen atmosphere, and calcining for 4h to obtain porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel, namely the MOF-derived nanosheet intercalation material; wherein the amount ratio of the substances is 2.5: 0.1-0.15: 500-520.
An MOF derived nanosheet intercalation material prepared by the method.
An application of the MOF derived nanosheet intercalation material as a supercapacitor electrode material.
The application comprises the following specific steps:
step 1: preparation of composite aerogel-foam nickel electrode slice
Pretreatment of foamed nickel: the foam nickel cut into a rectangle is firstly soaked in 6M HCL for 15min by ultrasonic wave, then is cleaned for 15min by deionized water and ethanol respectively by ultrasonic wave, and is dried in an oven at 60 ℃ for overnight. Putting a powder sample of porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel, acetylene black and polyvinylidene fluoride (PVDF) into a mortar together according to the mass ratio of 8:1, dropwise adding analytically pure N-methyl pyrrolidone (NMP) into the mortar, grinding into slurry, dropwise coating the slurry into the area of treated foamed nickel 2/3, standing at 60 ℃ for 12 hours for drying, and finally pressurizing to 10MPa on a tablet press to obtain the composite aerogel-foamed nickel electrode plate;
step 2: and (3) applying the composite aerogel-foam nickel electrode plate obtained in the step (1) to a supercapacitor electrode.
The composite aerogel-foamed nickel electrode plate has the specific capacitance of 2251F/g, has the characteristics of high specific capacity, good cycle performance, stable structure and the like, and is an excellent energy storage material.
The invention has the beneficial effects that:
MOF derived nanosheet intercalation materials.
The MOF derived nanosheet intercalation material prepared by the invention, namely the porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel, effectively realizes the full compounding of the porous cobaltosic oxide nanosheet and the polyethyleneimine macromolecule by utilizing the electrostatic acting force between the polyethyleneimine and the porous cobaltosic oxide nanosheet.
The MOF derivative nanosheet intercalation material prepared by the invention, namely the porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel, is applied as an electrode material of a super capacitor, and combines the advantages of a double electric layer super capacitor and a pseudocapacitance super capacitor; in addition, the composite material obtained by the invention is suitable for the fields of supercapacitors and the like.
Drawings
Fig. 1 is SEM and TEM photographs of the porous cobaltosic oxide nanosheet-nitrogen doped carbon composite aerogel material prepared in example 1.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
Example 1
(1) 0.115g of cobalt acetate and 4.4g of benzimidazole (bim) were added to a mixed solvent of 85ml of analytically pure toluene and 75ml of analytically pure methanol, and 15ml of analytically pure ammonia water was added as an auxiliary. Carrying out ultrasonic treatment on the prepared solution for 5 minutes, heating and stirring the solution at 60 ℃ for reaction for 12 hours, cooling the solution to room temperature after the reaction is finished, and washing the solution with distilled water and ethanol respectively;
(2) 100mg of Co2(bim)4Placing the mixture in a covered crucible, heating the mixture in a muffle furnace at the heating rate of 2.3 ℃/min to 350 ℃, keeping the temperature for 4 hours, and naturally cooling to obtain black powder, namely the porous cobaltosic oxide nanosheet;
(3) dispersing 50mg of porous cobaltosic oxide nanosheet and 50mg of polyethyleneimine (PEI, the molecular weight is 600) in 1g of deionized water, performing ultrasonic treatment for 1h, freeze-drying the mixture in a freeze dryer for one day, heating the freeze-dried mixture to 800 ℃ at the heating rate of 2 ℃/min in the argon or nitrogen atmosphere, and calcining the freeze-dried mixture for 4h to obtain the porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel. SEM and TEM photographs are shown in FIG. 1, in which a is an SEM image; b is a TEM image; the obtained porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel can be seen to have fluffy structural pores, and the cobaltosic oxide nanosheets are uniformly distributed on the surface of the porous nitrogen-doped carbon aerogel.
(4) Foam nickel pretreatment: cutting the foam nickel into rectangles, firstly ultrasonically soaking the foam nickel in 6M HCL for 15min, then ultrasonically cleaning the foam nickel for 15min by using deionized water and ethanol respectively, and drying the foam nickel in an oven at 60 ℃ overnight. Putting the powder sample prepared in the step (3), acetylene black and polyvinylidene fluoride (PVDF) into a mortar together according to the mass ratio of 8:1:1, dropwise adding analytically pure N-methyl pyrrolidone (NMP), grinding into slurry, dropwise coating the slurry on foamed nickel in an area of 2/3, placing the foamed nickel at 60 ℃ for 12 hours for drying, and finally pressurizing the dried porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel/foamed nickel sheet on a tablet press to 10MPa to obtain the required electrode slice.
Examples 2 to 6
The examples are the same as example 1 except that the differences are shown in table 1:
TABLE 1
Comparative example 1
The step (3) in example 1 was removed, and the same procedure as in example 1 was repeated to obtain a final product.
Performance detection
The porous cobaltosic oxide nanosheet material prepared in comparative example 1 and the porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel material prepared in example 1 were used as supercapacitor electrode materials, respectively, and the measured specific capacitance values are shown in table 2.
Through the comparison of the data, the improved preparation method of the porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel material effectively improves the specific capacitance of the capacitor of the product, so that the porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel material has a wide application prospect when being used as an electrode material of a super capacitor.
Although the above embodiments do not address the full scope of the disclosure with respect to the selection of parameters, in alternate embodiments, the invention can be practiced within the full scope of the disclosed parameters. The present invention is not limited to the above examples, and variations, additions, deletions, and substitutions which may be made by those skilled in the art within the spirit and scope of the present invention should also be considered as falling within the scope of the present invention.
Claims (5)
1. A preparation method of an MOF derived nanosheet intercalation material is characterized by comprising the following specific steps:
step 1: synthesis of two-dimensional MOF nanosheet material Co2(bim)4
Adding cobalt acetate and benzimidazole into a mixed solvent of toluene and methanol, and then adding ammonia water as an auxiliary agent; carrying out ultrasonic treatment on the prepared solution for 5 minutes, heating and stirring the solution at the temperature of 60 ℃ for reaction for 12 hours, wherein the mass ratio of the cobalt acetate to the benzimidazole to the toluene to the methanol to the ammonia water is = 0.25: 1-1.2: 47-50: 17-20: 4-10;
step 2: preparation of porous cobaltosic oxide nanosheet
Mixing Co2（bim）4Placing the crucible in a covered crucible, heating the crucible to 350-400 ℃ in a muffle furnace at a heating rate of 2.3 ℃/min, keeping the temperature for 4-6 h,naturally cooling to obtain black powder, namely the porous cobaltosic oxide nanosheet;
and step 3: preparation of porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel
Dispersing a porous cobaltosic oxide nanosheet and polyethyleneimine, wherein the molecular weight of the polyethyleneimine is 600 in water, performing ultrasonic treatment for 1h, freeze-drying the mixture in a freeze dryer for one day, heating the mixture to 600-900 ℃ at a heating rate of 2 ℃/min in an argon or nitrogen atmosphere, and calcining the mixture for 4h to obtain the porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel, namely the MOF derived nanosheet intercalation material; wherein the amount ratio of the substances is porous cobaltosic oxide nano-sheet, polyethyleneimine and water = 2.5: 0.1-0.15: 500-520.
2. An MOF derived nanosheet intercalation material made by the method of claim 1.
3. Use of a MOF derived nanosheet intercalation material of claim 2 as a supercapacitor electrode material.
4. The application according to claim 3, characterized by comprising the following specific steps:
step 1: preparation of composite aerogel-foam nickel electrode slice
Pretreatment of foamed nickel: ultrasonically soaking the foam nickel cut into a rectangle in 6M HCL for 15min, ultrasonically cleaning the foam nickel for 15min by using deionized water and ethanol respectively, and drying the foam nickel in an oven at 60 ℃ overnight; putting a powder sample of porous cobaltosic oxide nanosheet-nitrogen-doped carbon composite aerogel, acetylene black and polyvinylidene fluoride (PVDF) into a mortar together according to the mass ratio of 8:1, dropwise adding analytically pure N-methyl pyrrolidone (NMP) into the mortar, grinding into slurry, dropwise coating the slurry into the area of treated foam nickel 2/3, placing the slurry at 60 ℃ for 12 hours for drying, and finally pressurizing to 10MPa on a tablet press to obtain the composite aerogel-foam nickel electrode plate;
step 2: and (3) applying the composite aerogel-foam nickel electrode plate obtained in the step (1) to a supercapacitor electrode.
5. The use of claim 4, wherein the composite aerogel-nickel foam electrode sheet has a specific capacitance of 2251F/g.
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