CN111330520A - Preparation method and application of graphene and UIO-66 composite aerogel - Google Patents

Preparation method and application of graphene and UIO-66 composite aerogel Download PDF

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CN111330520A
CN111330520A CN202010159069.4A CN202010159069A CN111330520A CN 111330520 A CN111330520 A CN 111330520A CN 202010159069 A CN202010159069 A CN 202010159069A CN 111330520 A CN111330520 A CN 111330520A
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uio
graphene
graphene oxide
composite
composite aerogel
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袭锴
张旭
许波连
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Nanjing University Shenzhen Research Institute
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Nanjing University Shenzhen Research Institute
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    • 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
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0091—Preparation of aerogels, e.g. xerogels
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
    • B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28047—Gels
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/184—Preparation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents

Abstract

The invention discloses a preparation method and application of graphene and UIO-66 composite aerogel, and belongs to the technical field of functional material preparation. The preparation method comprises the steps of sequentially adding the graphene oxide dispersion liquid and the UIO-66 powder, sealing the container, then vibrating or stirring, heating, promoting the formation of the self-assembled three-dimensional frame structure of the graphene oxide and the uniform compounding of the UIO-66 powder and graphene oxide sheets to obtain the graphene porous composite hydrogel, and finally drying to obtain the composite aerogel. The composite aerogel prepared by the method has a self-supporting porous structure, and the preparation method is mild in condition and simple to operate, and can effectively prevent the graphene oxide sheets and crystals from agglomerating. The composite aerogel has a large specific surface area, and has good adsorption performance on methylene blue dye under 1atm and 298K under visible light. The prepared aerogel material has a three-dimensional structure, has good mechanical properties, and is convenient to recover and recycle.

Description

Preparation method and application of graphene and UIO-66 composite aerogel
Technical Field
The invention belongs to the technical field of functional material preparation, and particularly relates to a preparation method and application of graphene and UIO-66 composite aerogel.
Background
Graphene oxide is an intermediate product of graphene prepared by a redox method from graphite, and the surface of the graphene has abundant oxygen-containing groups (hydroxyl and epoxy groups on the plane of a carbon atom layer, carbonyl and carboxyl groups at the edge of the layer). The two-dimensional graphene oxide can be reduced and assembled into the porous and ultra-light three-dimensional graphene aerogel by a certain method. The porous network structure endows the graphene with larger specific surface area and porosity, and can be further used for loading various functional bodies. Metal organic framework compounds (MOFs) are porous crystalline materials formed by coordination of metal ions with multifunctional organic ligands. It has large porosity, specific surface area and structural diversity, and thus is widely used in the fields of gas adsorption and separation. Wherein UIO-66 is the most stable and studied class of materials in MOFs. UIO-66 having a pore size and greater than 1500m2The specific surface area per gram is constructed by different organic ligands and metal ions Zr, is generally a regular dodecahedral secondary structural unit, and has the advantages of good chemical stability, regular and adjustable appearance, high thermal stability, large specific surface area and the like. These properties make the UIO-66 material have potential application value in gas storage and separation, dye adsorption and other aspects.
Considering the practical limitations of processability of the UIO-66 powder material, it is a preferred method to load it into a porous material for use. Generally, the graphene aerogel has a mesoporous structure formed by building a three-dimensional network, the mesoporous structure provides a channel for dye molecules to enter the interior of the pore material, and the dye molecules can strongly interact with UIO-66 with a microporous structure. The microporous/mesoporous hierarchical pore structure constructed by the synergistic effect of the graphene aerogel and the UIO-66 and the photocatalytic performance of the UIO-66 are utilized, so that the graphene and UIO-66 composite aerogel material has high adsorption performance and catalytic degradation effect on dye molecules. At present, the preparation of the graphene and UIO-66 composite material is mainly to obtain a two-dimensional composite structure by an in-situ method, and no report is found on a three-dimensional composite structure of graphene loaded with UIO-66.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of graphene and UIO-66 composite aerogel, so as to solve the problems that the preparation of the graphene and UIO-66 composite material in the prior art is mainly to obtain a two-dimensional composite structure through an in-situ method, break through the existing two-dimensional composite structure, and realize the ordered nucleation and growth of UIO-66 in a gel system by using graphene hydrogel obtained by a chemical reduction method as a template. Drying to obtain the composite aerogel material with a multi-layer porous structure; the invention also aims to provide application of the graphene and UIO-66 composite aerogel in adsorbing methylene dye.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that:
a preparation method of graphene and UIO-66 composite aerogel comprises the following steps:
1) adding graphene oxide dispersion liquid into a reaction kettle, carrying out chemical reduction self-assembly to prepare graphene hydrogel, and then adding UIO-66 powder, wherein the feeding mass ratio of the UIO-66 powder to the graphene oxide is 1:100 and 100: 1;
2) sealing the container, vibrating or stirring, and heating at the temperature of 100-300 ℃ for 0.5-10h to promote the formation of the graphene oxide self-assembly three-dimensional frame structure and the uniform composition of the UIO-66 and the graphene oxide sheets to prepare the graphene and UIO-66 composite hydrogel;
3) and drying to obtain the graphene and UIO-66 composite aerogel.
Further, in the step 1), the feeding mass ratio of the UIO-66 powder to the graphene oxide is 1:10-10: 1.
Further, in the step 2), the heating temperature is 180 ℃, and the heating time is 6 hours.
Further, the lateral dimension of the graphene oxide is 0.1-100 μm.
Preferably, the lateral dimension of the graphene oxide is 1-10 μm.
Furthermore, the concentration of the graphene oxide is 0.1-10 mg/mL.
Further, the combination of UIO-66 and the surface of graphene oxide in a composite manner includes: uniform attachment of UIO-66 to the surface of graphene oxide sheets; the UIO-66 was coated with graphene oxide sheets.
Further, the drying method comprises freeze drying, vacuum drying and supercritical drying.
The graphene and UIO-66 composite aerogel prepared by the method.
Application of graphene and UIO-66 composite aerogel in adsorbing methylene blue dye.
Has the advantages that: compared with the prior art, the invention has the following beneficial effects:
1) the graphene composite material aerogel prepared on the basis of the sol-gel principle has a self-supporting porous structure, retains the integrity of the structures of graphene oxide and UIO-66, and has the excellent performances of the graphene oxide and the UIO-66;
2) the invention has universality and is almost suitable for all crystals. In addition, the present invention does not have any special requirement for graphene and graphene oxide, and any graphene oxide dispersion liquid that is stably dispersed is suitable for the present invention. The graphene porous composite aerogel with various functional characteristics can be prepared based on the method, so that the method is suitable for different application fields;
3) the invention is convenient for batch or industrial production. The method adopts a one-step method, can be realized only by stirring and mixing two materials of UIO-66 and graphene oxide, has wide source of used solvent, low price, simple test equipment and instrument and convenient operation, keeps the integrity of the structures of the graphene oxide and the UIO-66 in the synthesis process, and can effectively prevent the agglomeration of graphene oxide sheets and crystals;
4) compared with CN109589933A magnetic nanocomposite, the three-dimensional graphene aerogel material prepared by the method is strong in mechanical property and convenient to recover, and reduces the preparation cost and operation difficulty of recovering by using magnetic substances.
Drawings
FIG. 1 is a schematic diagram of the preparation of UIO-66/graphene composite hydrogel;
FIG. 2 is an SEM scan of an aerogel;
FIG. 3 is a BET pore size distribution plot of a hydrogel;
FIG. 4 is a graph of dye adsorption capacity of pure graphene-based aerogel at 298K, 1 atm;
FIG. 5 is a graph of dye adsorption capacity of graphene and UIO-66 composite aerogel at 298K, 1 atm.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to be limiting.
The graphene oxide is prepared by a modified Hummers method, and the specific method is as follows: under the condition of ice-water bath, adding graphite powder and nitrate into concentrated sulfuric acid with the mass concentration of 95-98% according to the mass ratio of 1 (0.01-100) to be uniformly mixed, adding potassium permanganate into the mixed solution, wherein the feeding mass ratio of the potassium permanganate to the graphite powder is (0.1-10):1, and keeping the temperature at 10 ℃ or below for 0.5-2h (preferably 2 h); then removing ice water bath, heating to 10-100 deg.C (preferably 35 deg.C) and maintaining for 10-120 min (preferably 30 min), adding water, stirring, and adding hydrogen peroxide to reduce residual potassium permanganate and MnO2(ii) a Centrifuging, washing the residue with hot water until the pH of the suspension is 7, dispersing the obtained powder in water again, performing ultrasonic treatment, and filtering to obtain suspension, namely graphene oxide dispersion. The nitrate is preferably one of chemically pure and analytically pure: potassium nitrate, sodium nitrate (preferably sodium nitrate).
The crystals can be synthesized by solvothermal methods. Specifically, the method can be carried out as follows: mixing metal salt or metal salt hydrate, organic ligand and solvent in proportion, then carrying out solvothermal reaction on the mixture to obtain crystal precipitate, and further carrying out centrifugation or standing treatment and vacuum drying to obtain crystal powder. The choice of metal centers in the metal salts or metal salt hydrates covers almost all metals, including main group elements, transition elements, copper-based metals, etc. The organic ligand may be selected from the group consisting of carboxylic acids, imidazoles, pyridines, porphyrins, and the like, which are chemically pure or analytically pure drugs. The solvent is selected from one of the following chemically pure or analytically pure reagents: methanol, ethanol, N-dimethylformamide, deionized water and the like.
Example 1
Preparing a 250mL reaction bottle in an ice bath, adding 96mL concentrated sulfuric acid, adding a solid mixture of 2g of graphite powder and 1g of sodium nitrate under magnetic stirring, slowly adding 6g of potassium permanganate, controlling the reaction temperature to be not more than 10 ℃, reacting for 2h under the ice bath condition, taking out, and stirring at 35 ℃ in a water bath. As the reaction proceeded, the reaction finally became brown slurry, to which was then slowly added a 5% by mass sulfuric acid solution for dilution. After 240mL of sulfuric acid solution was added, 5mL of 5% hydrogen peroxide was added thereto, and the solution became bright yellow with bubbling. And (3) filtering after continuously stirring, and then washing with a hydrochloric acid solution with the mass fraction of 10% and deionized water for multiple times until the solution is neutral. The product obtained is finally stored in the form of an aqueous dispersion of concentration for later use.
Example 2
The preparation of the sample was carried out as follows: adding N, N-dimethylformamide into a prepared reaction bottle at room temperature, adding 0.053g of anhydrous zirconium chloride and 0.037g of terephthalic acid under magnetic stirring, completely dissolving, and reacting for 24 hours at 120 ℃ in an oil bath. After the reaction is finished, centrifuging at a low speed, removing supernatant at room temperature, and then repeatedly washing and centrifuging for 3 times by using an N, N-dimethylformamide solvent. The obtained product is dried in vacuum at 120 ℃ to finally obtain UIO-66 crystal powder.
Example 3
Sequentially adding a graphene oxide aqueous phase dispersion liquid and UIO-66 crystal powder into a polytetrafluoroethylene lining reaction kettle with the size of 50mL, and controlling the initial feeding ratio of the raw materials as follows: 6mL of graphene oxide solution with the concentration of 4 mg/mL; UIO-66 crystalline powder 20 mg. And continuously mixing and reacting the obtained mixture for 6h at 180 ℃ in a hydrothermal kettle to obtain the UIO-66 graphene composite hydrogel. Further carrying out freeze drying on the composite material to finally obtain the UIO-66 graphene composite material aerogel.
Example 4
Sequentially adding a graphene oxide aqueous phase dispersion liquid and UIO-66 crystal powder into a polytetrafluoroethylene lining reaction kettle with the size of 50mL, and controlling the initial feeding ratio of the raw materials as follows: 6mL of graphene oxide solution with the concentration of 0.1 mg/mL; UIO-66 crystalline powder 60 mg. And continuously mixing and reacting the obtained mixture for 0.5h at 100 ℃ in a hydrothermal kettle to obtain the UIO-66 graphene composite hydrogel. And further carrying out vacuum drying on the composite material to finally obtain the UIO-66 graphene composite material aerogel.
Example 5
Sequentially adding a graphene oxide aqueous phase dispersion liquid and UIO-66 crystal powder into a polytetrafluoroethylene lining reaction kettle with the size of 50mL, and controlling the initial feeding ratio of the raw materials as follows: 6mL of graphene oxide solution with the concentration of 2 mg/mL; UIO-66 crystalline powder 0.12 mg. And continuously mixing and reacting the obtained mixture for 2h at 140 ℃ in a hydrothermal kettle to obtain the UIO-66 graphene composite hydrogel. Further on it carry outSupercritical fluidAnd drying to finally obtain the UIO-66 graphene composite aerogel.
Example 6
Sequentially adding a graphene oxide aqueous phase dispersion liquid and UIO-66 crystal powder into a polytetrafluoroethylene lining reaction kettle with the size of 50mL, and controlling the initial feeding ratio of the raw materials as follows: 6mL of graphene oxide solution with the concentration of 4 mg/mL; UIO-66 crystalline powder 40 mg. And continuously mixing and reacting the obtained mixture for 4 hours at 220 ℃ in a hydrothermal kettle to obtain the UIO-66 graphene composite hydrogel. Further carrying out freeze drying on the composite material to finally obtain the UIO-66 graphene composite material aerogel.
Example 7
Sequentially adding a graphene oxide aqueous phase dispersion liquid and UIO-66 crystal powder into a polytetrafluoroethylene lining reaction kettle with the size of 50mL, and controlling the initial feeding ratio of the raw materials as follows: 6mL of graphene oxide solution with the concentration of 6 mg/mL; UIO-66 crystalline powder 80 mg. And continuously mixing and reacting the obtained mixture for 7h at 240 ℃ in a hydrothermal kettle to obtain the UIO-66 graphene composite hydrogel. And further carrying out supercritical drying on the composite material to finally obtain the UIO-66 graphene composite material aerogel.
Example 8
Sequentially adding a graphene oxide aqueous phase dispersion liquid and UIO-66 crystal powder into a polytetrafluoroethylene lining reaction kettle with the size of 50mL, and controlling the initial feeding ratio of the raw materials as follows: 6mL of graphene oxide solution with the concentration of 8 mg/mL; UIO-66 crystalline powder 100 mg. And continuously mixing and reacting the obtained mixture for 8 hours at 280 ℃ in a hydrothermal kettle to obtain the UIO-66 graphene composite hydrogel. And further carrying out vacuum drying on the composite material to finally obtain the UIO-66 graphene composite material aerogel.
Example 9
Sequentially adding a graphene oxide aqueous phase dispersion liquid and UIO-66 crystal powder into a polytetrafluoroethylene lining reaction kettle with the size of 50mL, and controlling the initial feeding ratio of the raw materials as follows: 5mL of graphene oxide solution with the concentration of 10 mg/mL; UIO-66 crystalline powder 120 mg. And continuously mixing and reacting the obtained mixture for 10h at 300 ℃ in a hydrothermal kettle to obtain the UIO-66 graphene composite hydrogel. Further carrying out freeze drying on the composite material to finally obtain the UIO-66 graphene composite material aerogel.
In the above embodiment, the lateral dimension of the graphene oxide is 0.1 to 100 μm, and preferably, the lateral dimension of the graphene oxide is 1 to 10 μm.
Example 10
The internal structure state of the composite aerogel and the three-dimensional honeycomb structure of the graphene aerogel are 50-500 mu m, and the composite aerogel belongs to a large hole. The surface morphology of the graphene and UIO-66 composite aerogel obtained in example 7 is that UIO-66 is uniformly distributed on the surface of the graphene aerogel. In the graphene and UIO-66 composite aerogel obtained in the embodiments 3, 4, 5, 6, 8 and 9, the UIO-66 distribution on the surface of the graphene sheet layer is sparse, and the compounding amount of the UIO-66 is less than that in the embodiment 7. According to the pore size distribution curve of the graphene and UIO-66 composite aerogel, the pore sizes of micropores and mesopores are mainly 0.9-1.2 nm and 3-7 nm, and the porous structure of the graphene and UIO-66 composite aerogel can be obtained by combining the three-dimensional cellular structure of the graphene aerogel seen by a scanning electron microscope. Dye adsorption capacity curves of the graphene and UIO-66 composite aerogel obtained in example 7, the pure graphene-based aerogel obtained in example 3 and the pure UIO-66 sample at 298K and 1atm are shown in FIGS. 4-5. The graphene and UIO-66 composite aerogel prepared by the method has good methylene blue adsorption performance, and the adsorption capacity of the dye methylene blue of the graphene aerogel or the UIO-66 crystal is higher than that of pure graphene aerogel or pure UIO-66 crystal under the same condition.
It is to be noted that the above-mentioned list is only a few specific embodiments of the present invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.

Claims (10)

1. A preparation method of graphene and UIO-66 composite aerogel is characterized by comprising the following steps:
1) adding graphene oxide dispersion liquid into a reaction kettle, carrying out chemical reduction self-assembly to prepare graphene hydrogel, and then adding UIO-66 powder, wherein the feeding mass ratio of the UIO-66 powder to the graphene oxide is 1:100 and 100: 1;
2) sealing the container, vibrating or stirring, and heating at the temperature of 100-300 ℃ for 0.5-10h to promote the formation of the graphene oxide self-assembly three-dimensional frame structure and the uniform composition of the UIO-66 and the graphene oxide sheets to prepare the graphene and UIO-66 composite hydrogel;
3) and drying to obtain the graphene and UIO-66 composite aerogel.
2. The preparation method of the graphene and UIO-66 composite aerogel according to claim 1, wherein in the step 1), the feeding mass ratio of the UIO-66 powder to the graphene oxide is 1:10-10: 1.
3. The preparation method of the graphene and UIO-66 composite aerogel according to claim 1, wherein the heating temperature in the step 2) is 180 ℃ and the heating time is 6 hours.
4. The method for preparing graphene and UIO-66 composite aerogel according to claim 1, wherein the lateral dimension of said graphene oxide is 0.1-100 μm.
5. The method for preparing graphene and UIO-66 composite aerogel according to claim 4, wherein the lateral dimension of said graphene oxide is 1-10 μm.
6. The preparation method of the graphene and UIO-66 composite aerogel according to claim 1, wherein the concentration of the graphene oxide is 0.1-10 mg/mL.
7. The method for preparing graphene and UIO-66 composite aerogel according to any one of claims 1 to 6, wherein the combination of the UIO-66 and the graphene oxide in a surface composite mode comprises: uniform attachment of UIO-66 to the surface of graphene oxide sheets; the UIO-66 was coated with graphene oxide sheets.
8. The method for preparing graphene and UIO-66 composite aerogel according to any one of claims 1 to 6, wherein the drying method comprises freeze drying, vacuum drying and supercritical drying.
9. Graphene and UIO-66 composite aerogels prepared by the method of any one of claims 1 to 6.
10. Use of the graphene of claim 9 in combination with UIO-66 aerogel for adsorbing methylene blue dye.
CN202010159069.4A 2020-03-09 2020-03-09 Preparation method and application of graphene and UIO-66 composite aerogel Pending CN111330520A (en)

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Application publication date: 20200626