CN115739013A - Three-dimensional multifunctional graphene film and preparation method thereof - Google Patents
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Abstract
The invention discloses a three-dimensional multifunctional graphene film and a preparation method thereof, wherein the method comprises the following steps: the first step is as follows: mixing metal powder, trimesic acid, hydrofluoric acid, nitric acid and deionized water to obtain a precursor solution; the second step is that: transferring the precursor solution into the inner liner of a polytetrafluoroethylene reaction kettle, and heating to obtain an unpurified MOF material; the third step: purifying the unpurified MOF material to obtain a MOF powder; the fourth step: taking the MOF powder, allowing the MOF layer to be converted into a three-dimensional multifunctional graphene film. Different from the direct heat treatment of the MOF synthetic material, the three-dimensional multifunctional graphene film and the preparation method thereof have the advantages that the material prepared by the method cannot agglomerate, and the distribution density of metal on the carrier is higher. The green precise manufacturing technology adopting the laser scribing technology provides a feasible technology for manufacturing the high-efficiency and firm 3D-GCM, and can be applied to wastewater purification and sustainable clean energy production.
Description
Technical Field
The invention relates to the technical field of water treatment purification and energy production, in particular to a three-dimensional multifunctional graphene membrane and a preparation method thereof.
Background
The growing demand for energy and water is a problem that is currently plaguing many countries, and in order to solve this problem, extensive research has been carried out on the purification of sewage and the production of hydrogen by hydrolysis. Among many advanced functional nanomaterials, graphene Oxide (GO) nanoplates have given great attention by material scientists because of their high structural stability, excellent water permeability and sieving properties. Thus, GO nanosheets can be stacked into a three-dimensional porous membrane for rapid and efficient production of clean water from wastewater and brackish water. Different from the traditional polymer film, the three-dimensional graphene-based film (3D-GMs) can realize ultra-fast transmission of water through defects or nanochannels among single GO nano sheets; meanwhile, the narrow interlayer spacing and the large specific surface area thereof contribute to high removal performance of various organic substances and soluble metal ions through repulsion or adsorption. 3D-GMs may have a better tradeoff between breakthrough permeability and rejection than conventional membranes.
However, conventional 3D-GMs is made from GO dispersions with mass fractions less than 1.0wt% by self-assembly, which usually takes a significant amount of time. In addition, the stability of this kind of GO membrane in water is relatively poor, when the membrane soaks in water and bears certain pressure, water very easily gets into in the membrane for GO nano sheet mutual separation leads to GO membrane to decompose in several hours. In a practical separation process, the transverse shear forces generated by the tangential flow can severely damage the structure of the GO membrane in a short time. Although there are many strategies that can be used to improve the stability of GO membranes, such as reduction by chemical crosslinkers or polyvalent metal cations, hydriodic acid or hydrazine, intercalation into polyelectrolytes or epoxy resins, etc., these modification approaches still require large amounts of solvent to disperse the modifier into the narrow interlayer spacing of the GO nanosheets for the crosslinking reaction. In summary, both the structural engineering of 3D-GMs and the cross-linking modification of 3D-GMs pose additional environmental risks due to the large amount of chemicals or waste solvents involved and there is no better choice in self-assembly manufacturing of 3D-GMs.
Currently, many studies have constructed three-dimensional graphene-based catalytic membranes (3D-GCMs) using a method of incorporating active Metal Nanoparticles (MNPs) into the pores of the membrane and have exhibited various characteristics, such as production of clean hydrogen gas. In order to improve the production efficiency of H2, plasma photocatalytic techniques are widely used to induce the generation of thermal electrons, thereby accelerating the catalytic dissociation of water on the surfaces of MNPs. Meanwhile, electron transfer on the surfaces of MNPs can also activate various peroxides to generate Reactive Oxygen Species (ROS), which can degrade intractable organic pollutants (organic dyes and antibiotics) in water. However, electron-hole pairs photo-induced in the metal nanoparticles can undergo ultra-fast recombination due to the large diameter of the nanoparticles, which hinders the transfer of thermal electrons to the outside and reduces the efficiency of plasma photocatalysis.
To maximize the separation of electron-hole pairs, MNPs must be prevented from clustering and coupled with efficient electron acceptors with high electron mobility. In order to obtain 3D-GCMs with excellent photocatalytic performance, precursors of MNPs are generally mixed with GO dispersion liquid and uniformly fixed on the surface of a functional group of a GO nano-sheet, and then crystal growth, reduction and solution self-assembly are orderly carried out, so that the preparation of three-dimensional GCM is finally realized. The preparation process needs to consume a large amount of time, solvents, chemical agents and metal catalysts, and therefore the three-dimensional multifunctional graphene film and the preparation method thereof are provided.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a three-dimensional multifunctional graphene film and a preparation method thereof, so as to solve the problems.
(II) technical scheme
In order to achieve the above purpose, the invention provides the following technical scheme:
a method for preparing a three-dimensional multifunctional graphene film, comprising the steps of:
the first step is as follows: mixing metal powder, trimesic acid, hydrofluoric acid, nitric acid and deionized water, placing the mixture in a constant-temperature magnetic stirrer, and fully stirring the mixture to dissolve the mixture to obtain a precursor solution;
the second step is that: transferring the precursor solution into a polytetrafluoroethylene reaction kettle lining, sealing the reaction kettle, heating at 100-200 ℃ for 6-24h, naturally cooling to room temperature, centrifuging for 10min, collecting the precipitate inside, and washing with deionized water to obtain an unpurified MOF material;
the third step: purifying unpurified MOF materials in hot water at 50-100 ℃ for 1-6h, then purifying in hot ethanol at 50-100 ℃ for 1-6h, finally transferring the materials to a vacuum drying oven, and carrying out vacuum drying at 60-100 ℃ for 6-18h to obtain MOF powder;
the fourth step: taking MOF powder, fixing and compacting two glass sheets on a metal copper sheet die to form an MOF layer, setting nanosecond pulse laser parameters, scanning the MOF layer, and converting the MOF layer into a three-dimensional multifunctional graphene film after laser scribing of the whole MOF layer is finished.
The precursor solution comprises metal powder, trimesic acid, hydrofluoric acid, nitric acid and deionized water, and is prepared from the following components in parts by weight: 0.32g to 0.64g of metal powder, 2.4g to 3.23g of trimesic acid, 0.5mL of hydrofluoric acid with the concentration of 35 percent to 50 percent, 0.5mL of nitric acid with the concentration of 50 percent to 80 percent and 50mL of deionized water.
Preferably, the metal powder is any one or more of 0.32g to 0.64g of copper powder, 0.53g of palladium powder, and 0.54g of silver powder.
Preferably, the concentration of the hydrofluoric acid is 40% and the concentration of the nitric acid is 65%.
Preferably, the mass ratio of the metal powder to the trimesic acid in the first step is 1:1-1:10 (1: 1:10- (1.
Preferably, the heating temperature in the second step is 150 ℃ and the heating time is 12h.
Preferably, the hot water temperature in the third step is 80 ℃, the purification time is 3 hours, the hot ethanol temperature is 60 ℃, the purification time is 3 hours, the temperature in the vacuum drying oven is 80 ℃, and the vacuum drying time is 8 hours.
Preferably, in the fourth step, the nanosecond pulse laser parameters are set as: the wavelength range is one of 1064, 532, 355 and 266nm, the pulse time of the generated laser is 60-100ns, and the spot size of the laser is 50-150 μm.
Preferably, the area and the thickness of the three-dimensional multifunctional graphene film are 3.14cm2 and 0.5mm defined by the copper die.
(III) advantageous effects
Compared with the prior art, the three-dimensional multifunctional graphene film and the preparation method thereof provided by the invention have the following beneficial effects:
1. according to the three-dimensional multifunctional graphene-based catalytic membrane and the preparation method thereof, a novel multifunctional three-dimensional graphene-based catalytic membrane (3D-GCM) is successfully prepared by a green one-step laser scribing technology, and Active Metal Nanoparticles (AMNs) are loaded for simultaneously obtaining water and clean energy. The prepared 3D-GCM shows high porosity and uniformly distributed AMNs, shows high flux and super-strong adsorption capacity under the driving of ultra-low pressure (0.1 bar), and can remove organic pollutants in wastewater. After adsorption saturation, AMNs in the 3D-GCM start an advanced oxidation process through catalysis, and the film which is seriously polluted is self-cleaned, so that the adsorption capacity is finally well recovered. Most importantly, the 3D-GCM welded by laser scribing overcomes the problem of damage of transverse shearing force to a membrane structure in a long-term separation process. In addition, 3D-GCM can emit a large number of thermal electrons from AMNs under illumination, so that the membrane catalytic hydrolysis reaction is realized and hydrogen energy is generated.
2. Different from the direct heat treatment of the MOF synthetic material, the three-dimensional multifunctional graphene film and the preparation method thereof have the advantages that the material prepared by the method cannot agglomerate, and the distribution density of metal on the carrier is higher. The green precise manufacturing technology adopting the laser scribing technology provides a feasible technology for manufacturing the high-efficiency and firm 3D-GCM, and can be applied to wastewater purification and sustainable clean energy production.
Drawings
FIG. 1 is a schematic diagram of the preparation method of an embodiment of the present invention;
FIG. 2 is a Transmission Electron Microscope (TEM) photograph of a three-dimensional multifunctional graphene film prepared according to an embodiment of the present invention;
FIG. 3 is an X-ray photoelectron spectrum (XPS, a) and a high resolution XPS (b) of a three-dimensional multifunctional graphene film prepared according to example 1 (Cu @ 3D-GCM) of the present invention;
FIG. 4 is an XPS plot (plot a) and a high resolution XPS plot (plot b) of a three-dimensional multifunctional graphene film prepared according to example 2 (Cu/Ag @ 3D-GCM) of the present invention;
FIG. 5 is an XPS plot (plot a) and a high resolution XPS plot (plot b) of a three-dimensional multifunctional graphene film prepared according to example 3 (Cu/Pd @ 3D-GCM) of the present invention;
FIG. 6 shows the results of 5 cycles of rhodamine B (RhB) removal efficiency and adsorption capacity within 3 hours for a three-dimensional multifunctional graphene film prepared according to example 3 (Cu/Pd @ 3D-GCM) of the present invention;
FIG. 7 is a comparison of the removal performance and hydrogen generation performance of three-dimensional multifunctional graphene films obtained in example 1 (Cu @ 3D-GCM), example 2 (Cu/Ag @ 3D-GCM), and example 3 (Cu/Pd @ 3D-GCM) of the present invention with respect to RhB.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
The preparation method of the three-dimensional multifunctional graphene film provided by the embodiment of the invention comprises the following steps:
(1) 0.64g of copper powder, 2.4g of trimesic acid, hydrofluoric acid (40%, 0.5 mL), nitric acid (65%, 0.5 mL) and 50mL of deionized water are mixed, placed in a constant-temperature magnetic stirrer, and fully stirred at 60 ℃ for a certain time to dissolve the copper powder, so as to obtain a precursor solution.
(2) And (2) transferring the precursor solution obtained in the step (1) into a lining of a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, heating the reaction kettle at 150 ℃ for 12h, naturally cooling to room temperature, centrifuging for 10min, collecting the precipitate inside, and washing with deionized water to obtain the unpurified MOF material.
(3) Purifying the unpurified MOF material obtained in the step (2) in hot water at 80 ℃ for 3h, then in hot ethanol at 60 ℃ for 3h to remove residual metal ions on the material, and finally transferring the material to a vacuum drying oven to be dried in vacuum at 80 ℃ for 8h to obtain MOF powder.
(4) Taking a certain amount of MOF powder obtained in the step (3), and fixing and compacting two glass sheets on a metal copper sheet die to form an MOF layer. The parameters of the nanosecond pulse laser are set to be 80ns, the wavelength of the nanosecond pulse laser is 1064nm, and the size of a light spot is 100mm, so that the MOF layer can be scanned by using an accurate energy source. After laser scribing, the MOF layer was converted into a copper-modified three-dimensional multifunctional graphene film (Cu 3D-GCM) with an area and thickness of 3.14cm defined by the copper mold itself 2 、0.5mm。
The three-dimensional multifunctional graphene film is prepared by the method.
Example 2
The preparation method of the three-dimensional multifunctional graphene film provided by the embodiment comprises the following steps:
(1) 0.32g of copper powder, 0.54g of silver powder, 3.23g of trimesic acid, hydrofluoric acid (40%, 0.5 mL), nitric acid (65%, 0.5 mL) and 50mL of deionized water were mixed, placed in a constant-temperature magnetic stirrer, and fully stirred at 60 ℃ for a certain time to dissolve the copper powder, thereby obtaining a precursor solution.
(2) And (2) transferring the precursor solution obtained in the step (1) into a lining of a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, heating the reaction kettle at 150 ℃ for 12h, naturally cooling to room temperature, centrifuging for 10min, collecting the precipitate inside, and washing with deionized water to obtain the unpurified MOF material.
(3) Purifying the unpurified MOF material obtained in the step (2) in hot water at 80 ℃ for 3h, then in hot ethanol at 60 ℃ for 3h to remove residual metal ions on the material, and finally transferring the material to a vacuum drying oven to be dried in vacuum at 80 ℃ for 8h to obtain MOF powder.
(4) And (4) taking a certain amount of MOF powder obtained in the step (3), and fixing and compacting two glass sheets on a metal copper sheet die to form an MOF layer. The parameters of the nanosecond pulse laser are set to be 80ns, the wavelength of the nanosecond pulse laser is 1064nm, and the size of a light spot is 100mm, so that the MOF layer can be scanned by using an accurate energy source. After laser scribing, the MOF layer is converted into a copper-silver modified three-dimensional multifunctional graphene film (Cu/Ag 3D-GCM), and the area and the thickness of the film are 3.14cm2 and 0.5mm limited by the copper mold.
Example 3
The embodiment is an embodiment of a method for preparing a three-dimensional multifunctional graphene film according to the present invention. The preparation method of the three-dimensional multifunctional graphene film in the embodiment includes the following steps:
(1) 0.32g of copper powder, 0.53g of palladium powder, 3.19g of trimesic acid, 40% hydrofluoric acid (0.5 mL), 65% nitric acid (0.5 mL) and 50mL of deionized water are mixed, placed in a constant-temperature magnetic stirrer, and fully stirred at 60 ℃ for a certain time to dissolve the copper powder, so that a precursor solution is obtained.
(2) And (2) transferring the precursor solution obtained in the step (1) into a lining of a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, heating the reaction kettle at 150 ℃ for 12h, naturally cooling to room temperature, centrifuging for 10min, collecting the precipitate inside, and washing with deionized water to obtain the unpurified MOF material.
(3) Purifying the unpurified MOF material obtained in the step (2) in hot water at 80 ℃ for 3h, then in hot ethanol at 60 ℃ for 3h to remove residual metal ions on the material, and finally transferring the material to a vacuum drying oven to be dried in vacuum at 80 ℃ for 8h to obtain MOF powder.
(4) And (4) taking a certain amount of MOF powder obtained in the step (3), and fixing and compacting two glass sheets on a metal copper sheet die to form an MOF layer. The parameters of the nanosecond pulse laser are set to be 80ns, the wavelength of the nanosecond pulse laser is 1064nm, and the size of a light spot is 100mm, so that the MOF layer can be scanned by using an accurate energy source. After laser scribing, the MOF layer is converted into a copper palladium modified three-dimensional multifunctional graphene film (Cu/Pd @ 3D-GCM), and the area and the thickness of the film are 3.14cm2 and 0.5mm limited by the copper mold.
As can be seen from fig. 2, TEM images of the three-dimensional multifunctional graphene films in examples 1, 2 and 3 clearly show that the films have a coral-like morphology with a porous structure and regularly arranged dark spherical spots, and the nanoparticles are uniformly dispersed without significant aggregation. In addition, lattice edges corresponding to Cu (111), ag (111), and Pd (111) structures were observed by high resolution TEM, indicating that independent crystal structures were formed. In addition, observation of the high resolution TEM images also revealed that the interlayer spacing of the material was 0.34nm, confirming the formation and efficient reduction of 3D graphene. The MNPs generated by laser scribing are uniformly distributed on the whole frame, and the layered pores are clear and visible and are abundant in quantity.
As can be seen from fig. 3, the XPS image of the three-dimensional multifunctional graphene film in example 1 confirmed that it produced Cu.
As can be seen from fig. 4, the XPS image of the three-dimensional multifunctional graphene film in example 2 confirmed that it produced Cu and Ag.
As can be seen from fig. 5, the XPS image of the three-dimensional multifunctional graphene film in example 3 confirmed that it produced Cu and Pd.
As can be seen from fig. 6, when the performance of the three-dimensional multifunctional graphene film prepared in example 3 was tested under 0.1MPa with 1L of 20ppm rhodamine B solution, it was found that the removal efficiency was almost recovered to 100% of the initial value after 5 cycles of testing, and the adsorption capacity was also slightly improved. The three-dimensional multifunctional graphene membrane prepared by the embodiment has stable interception performance, and the membrane has good capability of treating dye micromolecules.
As can be seen from fig. 7, in the three-dimensional multifunctional graphene films prepared in example 1, example 2, and example 3, cu/pd @3d-GCM showed the highest photocatalytic activity, and the RhB removal rate reached 98.4% under irradiation for 90 minutes (a in fig. 7). From the pseudo first order kinetic results, the surface catalytic reaction rate constant (k) of Cu/Pd @3D-GCM was calculated to be 0.0459/min (b in FIG. 7). The hydrogen production experiment of water was performed under visible light irradiation by supplying electrons using ethanol as a sacrificial agent. The hydrogen production performance of Cu/Pd @3D-GCM is 1.3474 mmol/(g.h), which is about 7 times higher than that of Cu @3D-GCM (0.1927 mmol/(g.h)) (c in FIG. 7). Therefore, the three-dimensional multifunctional graphene membrane shows high hydrogen production and photocatalytic degradation regeneration performance.
Different from the direct heat treatment of the MOF synthetic material, the three-dimensional multifunctional graphene film and the preparation method thereof provided by the embodiment of the invention have the advantages that the material prepared by the method cannot agglomerate, and the distribution density of metal on the carrier is higher. The green precision manufacturing technology adopting the laser scribing technology provides a feasible technology for manufacturing the efficient and firm 3D-GCM, and can be applied to wastewater purification and sustainable clean energy production. Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A preparation method of a three-dimensional multifunctional graphene film is characterized by comprising the following steps:
the first step is as follows: mixing metal powder, trimesic acid, hydrofluoric acid, nitric acid and deionized water, placing the mixture in a constant-temperature magnetic stirrer, and fully stirring the mixture to dissolve the mixture to obtain a precursor solution;
the second step is that: transferring the precursor solution into a polytetrafluoroethylene reaction kettle lining, sealing the reaction kettle, heating at 100-200 ℃ for 6-24h, naturally cooling to room temperature, centrifuging for 10min, collecting the precipitate inside, and washing with deionized water to obtain an unpurified MOF material;
the third step: purifying unpurified MOF materials in hot water at 50-100 ℃ for 1-6h, then purifying in hot ethanol at 50-100 ℃ for 1-6h, finally transferring the materials to a vacuum drying oven, and carrying out vacuum drying at 60-100 ℃ for 6-18h to obtain MOF powder;
the fourth step: taking MOF powder, fixing and compacting two glass sheets on a metal copper sheet die to form an MOF layer, setting nanosecond pulse laser parameters, scanning the MOF layer, and converting the MOF layer into a three-dimensional multifunctional graphene film after laser scribing of the whole MOF layer is finished.
2. The method of preparing the three-dimensional multifunctional graphene film according to claim 1, wherein: the precursor solution comprises metal powder, trimesic acid, hydrofluoric acid, nitric acid and deionized water, and is prepared from the following components in parts by weight: 0.32g to 0.64g of metal powder, 2.4g to 3.23g of trimesic acid, 0.5mL of hydrofluoric acid with the concentration of 35 percent to 50 percent, 0.5mL of nitric acid with the concentration of 50 percent to 80 percent and 50mL of deionized water.
3. The method of preparing the three-dimensional multifunctional graphene film according to claim 1, wherein: the metal powder is any one or more of 0.32g-0.64g of copper powder, 0.53g of palladium powder and 0.54g of silver powder.
4. The method of preparing the three-dimensional multifunctional graphene film according to claim 2, wherein: the concentration of the hydrofluoric acid is 40%, and the concentration of the nitric acid is 65%.
5. The method of preparing the three-dimensional multifunctional graphene film according to claim 1, wherein: the mass ratio of the metal powder to the trimesic acid in the first step is 1:1-1:10 (1: 1:10- (1.
6. The method of preparing the three-dimensional multifunctional graphene film according to claim 1, wherein: the heating temperature in the second step is 150 ℃, and the heating time is 12h.
7. The method of preparing the three-dimensional multifunctional graphene film according to claim 1, wherein: and in the third step, the temperature of hot water is 80 ℃, the purification time is 3 hours, the temperature of hot ethanol is 60 ℃, the purification time is 3 hours, the temperature in a vacuum drying box is 80 ℃, and the vacuum drying time is 8 hours.
8. The method of preparing the three-dimensional multifunctional graphene film according to claim 1, wherein: in the fourth step, nanosecond pulse laser parameters are set as follows: the wavelength range is one of 1064, 532, 355 and 266nm, the pulse time of the generated laser is 60-100ns, and the spot size of the laser is 50-150 μm.
9. The method of preparing the three-dimensional multifunctional graphene film according to claim 1, wherein: the area and the thickness of the three-dimensional multifunctional graphene film are 3.14cm limited by the copper die 2 、0.5mm。
10. A three-dimensional multifunctional graphene film prepared by the method of any one of claims 1-9.
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