CN115636954A - Super-elastic double-layer photo-thermal hydrogel with high mechanical strength and preparation method and application thereof - Google Patents
Super-elastic double-layer photo-thermal hydrogel with high mechanical strength and preparation method and application thereof Download PDFInfo
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- Y02A20/124—Water desalination
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/138—Water desalination using renewable energy
- Y02A20/142—Solar thermal; Photovoltaics
Abstract
The invention relates to the technical field of functional material preparation, and discloses a super-elastic double-layer photo-thermal hydrogel with high mechanical strength, a preparation method and application thereof, wherein the preparation method comprises the following steps: soaking delignified wood blocks into a sodium hydroxide solution, stirring to obtain a suspension, filtering, washing to be neutral, freeze-drying to obtain cellulose fibers, adding the cellulose fibers into a polyvinyl alcohol aqueous solution, dispersing, adding a cross-linking agent and a catalyst, and stirring to obtain a mixed solution; equally dividing the mixed solution into a part A and a part B, pouring the part A into a mold, placing the mold in liquid nitrogen for directional freezing, adding a light absorbent into the part B, and pouring the part B into the mold for directional freezing; and taking out the gel together with the frozen mould, thawing, and soaking to be neutral to obtain the super-elastic double-layer photo-thermal hydrogel. The super-elastic double-layer photo-thermal hydrogel can keep structural stability and high-efficiency, long-term and stable evaporation in a complex and severe environment.
Description
Technical Field
The invention belongs to the technical field of functional material preparation, and particularly relates to a super-elastic double-layer photo-thermal hydrogel with high mechanical strength, and a preparation method and application thereof.
Background
The shortage of fresh water resources is an important problem for restricting the sustainable development of human beings. The use of interfacial solar steam generation for desalination of sea water and purification of water quality to produce clean water is considered to be an important solution to the problems presented at present. The development of highly efficient solar photothermal materials for photothermal conversion is the core of its technology. Among them, the hydrogel-based material is considered as one of the most important materials in the water evaporation process.
The hydrogel is a polymer network formed by crosslinking hydrophilic polymers and composed of a large number of water molecules, and the unique three-dimensional pore channel structure of the hydrogel can ensure the transmission of the water molecules, improve the water evaporation rate and enhance the reflection and scattering of internal light, so that more light energy can be captured. However, conventional hydrogel evaporators typically have only a single network. Due to the lack of structural complexity, the polymer is soft in property and limited in mechanical strength, and when the polymer is applied to severe environments such as acid-base, heavy metal industrial wastewater and soil, a polymer network structure of the polymer is easily damaged, so that a pore channel is shrunk, collapsed or blocked. In addition, most chemically crosslinked hydrogels have low elasticity due to the irreversibility of covalent bonds, and are damaged upon loading, which seriously affects evaporation performance.
Therefore, a photo-thermal hydrogel material with high mechanical strength, which can maintain structural stability and efficient, long-term and stable evaporation in a complex and severe environment and can be prepared by a simple and convenient method, is needed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the super-elastic double-layer photo-thermal hydrogel which has high mechanical strength and mechanical stability and is applied to solar-driven interfacial evaporation, photo-thermal seawater desalination and sewage treatment, and the preparation method and the application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of super-elastic double-layer photo-thermal hydrogel with high mechanical strength comprises the following steps:
1) Immersing the delignified wood block into a sodium hydroxide solution with the concentration of 4-6%; stirring for 4-6 h at 75-80 ℃ to obtain suspension, cooling the suspension to room temperature, filtering, washing with deionized water to neutrality to obtain log fibers; freezing at-15 to-30 ℃ for 4 to 8 hours, and then carrying out vacuum freeze drying at-40 to-65 ℃ for 36 to 72 hours to obtain cellulose fibers;
2) Mixing polyvinyl alcohol with deionized water to obtain a polyvinyl alcohol aqueous solution with the mass percentage concentration of 2-4%; then adding the cellulose fibers obtained in the step 1), dispersing, adding a cross-linking agent and a catalyst, and stirring at room temperature to obtain a mixed solution; wherein the mass ratio of the polyvinyl alcohol to the cellulose fiber is 1-3; the volume ratio of the crosslinking agent to the catalyst to the polyvinyl alcohol aqueous solution is 1: 80 to 100 portions; equally dividing the mixed solution into a part A and a part B, wherein a light absorbent is added into the part B;
3) Pouring the part A into a mold, placing the part A into liquid nitrogen for directional freezing, pouring the part B into the same mold, and performing directional freezing in the liquid nitrogen until the gel is completely frozen; then freezing the gel and the mould for 8h at-15 to-30 ℃, taking out the gel, unfreezing the gel at room temperature, and soaking the gel in deionized water to be neutral to obtain the super-elastic double-layer photo-thermal hydrogel.
Further, the delignified wood block in the step 1) is prepared by the following method: adding 8-12 g of sodium chlorite and 2-3 mL of acetic acid into 400-600 mL of deionized water, mixing and stirring; and then immersing the cut wood blocks into the solution, stirring for 6-8 h at the constant temperature of 90-100 ℃ to obtain a mixed solution, cooling the mixed solution to room temperature, filtering, washing with deionized water to be neutral, and thus obtaining the delignified wood blocks.
Furthermore, the volume of the cut wood block is 10 multiplied by 5 multiplied by 1mm, and the mass is 8-12 g.
Further, the wood block is a xylem part of any woody plant.
Further, the cross-linking agent in the step 2) is glutaraldehyde.
Further, the catalyst in the step 2) is 1.2mol/L hydrochloric acid.
Further, the light absorbent in the step 2) is one or more of MXene material, conjugated polymer material, carbon-based material and biomass charcoal;
the MXene material is one or more of any novel transition metal carbon/nitride two-dimensional nano layered materials;
the conjugated polymer material is one or more of polypyrrole and polydopamine;
the carbon-based material is one or more of graphene, carbon nano tubes, carbon fibers, fullerene and porous carbon materials;
the biomass charcoal is one or more of natural black materials of roots, stems, leaves and outer skins of plants after high-temperature carbonization and cuttlefish meal.
A super-elastic double-layer photo-thermal hydrogel with high mechanical strength is prepared by the preparation method.
The application of the super-elastic double-layer photo-thermal hydrogel with high mechanical strength in solar-driven interfacial evaporation, photo-thermal seawater desalination and sewage treatment.
Compared with the prior art, the invention has the following technical effects:
1. the invention provides a preparation method and application of a super-elastic double-layer photo-thermal hydrogel with high mechanical strength.
2. The super-elastic double-layer photo-thermal hydrogel with high mechanical strength has excellent mechanical stability and underwater super-elasticity, 80.6 percent of maximum compression stress is kept after 1000 compression cycles when 80 percent of compression deformation amount is applied, and almost no plastic deformation exists after 1000 underwater cycles.
3. The super-elastic double-layer photo-thermal hydrogel with high mechanical strength has excellent steam generation, seawater desalination and sewage treatment performances; the salinity of the purified seawater is greatly reduced, the requirement of the world health organization on safe application water is met, the fish tank detection test paper shows that the purified sewage can be used for normal survival of aquatic organisms, and the hydrogel water purification effect is excellent.
4. The preparation method and the application of the super-elastic double-layer photo-thermal hydrogel with high mechanical strength have the advantages of wide raw material source, low manufacturing cost, simple process and large-scale production, and the obtained product can keep structural stability and high-efficiency, long-term and stable evaporation in a complicated and severe environment, can be used for sewage treatment and seawater desalination, and has wide application prospect.
In conclusion, the preparation method of the super-elastic double-layer photothermal hydrogel with high mechanical strength, disclosed by the invention, has the advantages that the cellulose fibers are added and are inserted in the hydrate network of the polyvinyl alcohol hydrogel, the stability of the polyvinyl alcohol hydrogel is reinforced, and meanwhile, the disorderly pore structure in the hydrogel is changed into the parallel-arranged bundle-shaped tissue by adopting an ice template induced directional freezing method for water transmission, so that the photothermal hydrogel with high mechanical strength and mechanical stability and applied to solar-driven interface evaporation, photothermal seawater desalination and sewage treatment is obtained.
Drawings
FIG. 1 is a diagram of a super-elastic double-layered photo-thermal hydrogel having high mechanical strength according to example 1 of the present invention;
FIG. 2 is an enlarged view of a hyperelastic double-layered photothermal hydrogel of example 1 having high mechanical strength according to the present invention;
FIG. 3 is a cross-sectional electron microscope of a hyperelastic double-layered photothermal hydrogel having high mechanical strength according to example 1 of the present invention;
FIG. 4 is an electron microscope view of a longitudinal section of a superelastic double-layered photothermal hydrogel having high mechanical strength according to example 1 of the present invention;
FIG. 5 is a graph showing the results of underwater superelastic compression cycle testing of a high mechanical strength superelastic double layer photothermal hydrogel in example 2 of this invention;
FIG. 6 is a graph showing the evaporation rate of a hyperelastic double-layered photothermal hydrogel having high mechanical strength in example 3 of the present invention in the treatment of simulated seawater, wastewater containing sulfuric acid, and wastewater containing sodium hydroxide;
FIG. 7 is a graph showing the evaporation rate of the super-elastic double-layered photothermal hydrogel having high mechanical strength in treating wastewater and heavy metal wastewater in soil according to example 3 of the present invention;
FIG. 8 is a graph showing a comparison between the simulated seawater treatment and the high mechanical strength super-elastic double-layered photothermal hydrogel in example 3 of the present invention;
FIG. 9 is a comparison of the high mechanical strength super-elastic double-layered photo-thermal hydrogel simulated heavy metal wastewater before and after treatment in example 3 of the present invention;
FIG. 10 is a graph showing a load comparison between the super-elastic double-layered photothermal hydrogel having high mechanical strength according to example 3 of the present invention and that of comparative example 1.
Detailed Description
The present invention will be explained in further detail with reference to examples.
Examples
Example 1
A preparation method of super-elastic double-layer photo-thermal hydrogel with high mechanical strength comprises the following steps:
1) Adding 10g of sodium chlorite and 2.5mL of acetic acid into 500mL of deionized water, and stirring and mixing uniformly; and then 10g of cut peach wood blocks are immersed in the solution, the solution is stirred for 7 hours at the constant temperature of 95 ℃ to obtain a mixed solution after full reaction, the mixed solution is cooled to room temperature and then filtered, and the mixed solution is washed to be neutral by deionized water to obtain delignified wood blocks.
2) Immersing the delignified wood block obtained in the step 1) into a 5% sodium hydroxide solution; then stirring at the constant temperature of 75 ℃ for 5 hours to fully react, cooling to room temperature after obtaining suspension, filtering, washing to be neutral by deionized water, and obtaining log fibers; freezing at-25 deg.C for 8 hr, and vacuum freeze-drying at-65 deg.C for 48 hr to obtain cellulose fiber.
3) Adding 0.6g of polyvinyl alcohol into 18mL of deionized water, stirring at 90 ℃ for 30min, then adding 0.3g of cellulose fiber obtained in the step 2), uniformly dispersing, adding 200 mu L of glutaraldehyde and 1mL of 1.2mol/L hydrochloric acid, and stirring at room temperature for 10min to obtain a mixed solution. The mixed solution is divided into a part A and a part B, wherein cuttlefish powder is added into the part B as a light absorbent.
4) Pouring the part A solution obtained in the step 3) into a mould, placing the mould in a liquid nitrogen bath for ice template-induced directional freezing, and immediately pouring the part B with the cuttlefish powder into the same mould after the bottom is solidified until the gel is completely frozen. And then putting the mould and the mould into a refrigerator at the temperature of 25 ℃ below zero for freezing for 8 hours to ensure that the mould is fully crosslinked, taking out the gel, unfreezing the gel at room temperature, and soaking the gel in deionized water until the gel is neutral to obtain the super-elastic double-layer photo-thermal hydrogel.
Referring to the drawings shown in fig. 1 and 2 and the enlarged drawings, it is illustrated that the hyperelastic double-layer photothermal hydrogel with high mechanical strength prepared in this example has good shape controllability, and the shape and size can be adjusted as required.
Referring to the scanning electron microscope results of fig. 3 and 4, it is demonstrated that the super-elastic double-layer photothermal hydrogel with high mechanical strength prepared in this example has a grid-like porous structure, uniform pore size, orderly arranged channels in bundles, and good water transport performance.
Example 2
A preparation method of super-elastic double-layer photothermal hydrogel with high mechanical strength comprises the following steps:
1) Adding 8g of sodium chlorite and 2mL of acetic acid into 400mL of deionized water, and stirring and mixing uniformly; and then 8g of cut balsa blocks are immersed into the solution, stirred for 6 hours at the constant temperature of 90 ℃ to obtain a mixed solution after full reaction, the mixed solution is cooled to the room temperature and then filtered, and the mixed solution is washed to be neutral by deionized water to obtain delignified blocks.
2) Immersing the delignified wood block obtained in the step 1) into a 4% sodium hydroxide solution; stirring at the constant temperature of 75 ℃ for 4 hours to fully react, cooling to room temperature after obtaining suspension, filtering, washing to be neutral by deionized water to obtain log fibers; freezing at-25 deg.C for 8 hr, and vacuum freeze-drying at-65 deg.C for 48 hr to obtain cellulose fiber.
3) Adding 0.6g of polyvinyl alcohol into 18mL of deionized water, stirring at 90 ℃ for 30min, then adding 0.3g of cellulose fibers obtained in the step 2), uniformly dispersing, then adding 200 mu L of glutaraldehyde and 1mL of 1.2mol/L hydrochloric acid, and stirring at room temperature for 10min to obtain a mixed solution. The mixed solution is divided into part A and part B, wherein polypyrrole is added into part B as a light absorbent.
4) Pouring the part A solution obtained in the step 3) into a mould, placing the mould in a liquid nitrogen bath for ice template-induced directional freezing, and immediately pouring the part B with polypyrrole into the same mould after the bottom is solidified until the gel is completely frozen. And then putting the mould and the mould into a refrigerator at the temperature of 25 ℃ below zero for freezing for 8 hours to ensure that the mould is fully crosslinked, taking out the gel, unfreezing the gel at room temperature, and soaking the gel in deionized water until the gel is neutral to obtain the super-elastic double-layer photo-thermal hydrogel.
Referring to fig. 5, the underwater superelasticity and compression stability test of the superelasticity double-layer photothermal hydrogel of this example was carried out, and 80.6% of the maximum compressive stress was maintained after 1000 compression cycles with an 80% compressive deformation amount, and almost no plastic deformation was observed after 1000 underwater cycles.
Example 3
A preparation method of super-elastic double-layer photo-thermal hydrogel with high mechanical strength comprises the following steps:
1) Adding 12g of sodium chlorite and 3mL of acetic acid into 600mL of deionized water, and stirring and mixing uniformly; and then 12g of cut poplar wood is immersed in the solution, the mixture is stirred for 8 hours at the constant temperature of 100 ℃ to obtain a mixed solution after full reaction, the mixed solution is cooled to the room temperature and then filtered, and the mixed solution is washed to be neutral by deionized water to obtain delignified wood blocks.
2) Immersing the delignified wood block obtained in the step 1) into a 6% sodium hydroxide solution; then stirring at the constant temperature of 80 ℃ for 6 hours to fully react to obtain a suspension, cooling to room temperature, filtering, washing with deionized water to be neutral to obtain log fibers; freezing at-25 deg.C for 8 hr, and vacuum freeze drying at-65 deg.C for 48 hr to obtain cellulose fiber.
3) Adding 1.2g of polyvinyl alcohol into 36mL of deionized water, stirring at 90 ℃ for 30min, then adding 0.6g of cellulose fiber obtained in the step 2), uniformly dispersing, adding 400 mu L of glutaraldehyde and 2mL of 1.2mol/L hydrochloric acid, and stirring at room temperature for 10min to obtain a mixed solution. And (3) dividing the mixed solution into an A part and a B part, wherein carbon nano tubes are added into the B part as a light absorbent.
4) Pouring the part A solution obtained in the step 3) into a mould, placing the mould in a liquid nitrogen bath for ice template-induced directional freezing, and immediately pouring the part B with the carbon nano tubes into the same mould after the bottom is solidified until the gel is completely frozen. And then putting the mould and the mould into a refrigerator at the temperature of 25 ℃ below zero for freezing for 8 hours to ensure that the mould is fully crosslinked, taking out the gel, unfreezing the gel at room temperature, and soaking the gel in deionized water until the gel is neutral to obtain the super-elastic double-layer photo-thermal hydrogel.
Referring to FIGS. 6 and 7, the water evaporation rate test of the superelastic bi-layer photothermal hydrogel of this example was performed by simulating a solar radiation power (1 kw m) with a xenon lamp 2 ) Under the irradiation of (2), the evaporation rate of the water in the water reaches 2.37 kg.m -2 ·h -1 The energy conversion efficiency is as high as 95 percent, and the high evaporation rate (2-2.23 kg. M) can be kept under severe and complex environments (heavy metal wastewater, acid, alkali and soil) -2 ·h- 1 )。
Referring to fig. 8, the salinity of the simulated seawater treated by the embodiment is obviously reduced, and the simulated seawater meets the quality standard of WHO drinking water.
Referring to FIG. 9, the heavy metal wastewater (including Ni) treated in this example + 、Co2 + 、Cu 2+ And Cr2O7 2+ ) The concentration of medium heavy metal ions is obviously reduced, and the heavy metal in the treated water can be discharged or recycled when the concentration is lower than the discharge standard.
Example 4
A method for preparing a super-elastic double-layered photo-thermal hydrogel having high mechanical strength, which is performed according to the method of example 1, except that:
step 2), firstly freezing the log fibers at the temperature of minus 15 ℃ for 6 hours, and then carrying out vacuum freeze drying at the temperature of minus 40 ℃ for 72 hours to obtain cellulose fibers;
adding 0.35g of polyvinyl alcohol into 16mL of deionized water in the step 3), stirring at 90 ℃ for 30min, and then adding 0.35g of the cellulose fiber obtained in the step 2);
and 4) putting the mould and the mould into a refrigerator with the temperature of-15 ℃ for freezing for 8h.
Example 5
A method for preparing a super-elastic double-layered photo-thermal hydrogel having high mechanical strength, which is performed according to the method of example 1, except that:
step 2), firstly freezing the log fibers at-30 ℃ for 4 hours, and then carrying out vacuum freeze drying at-55 ℃ for 36 hours to obtain cellulose fibers;
in the step 3), 0.81g of polyvinyl alcohol is added into 20mL of deionized water, stirred at 90 ℃ for 30min, and then 0.27g of cellulose fiber obtained in the step 2) is added;
and 4) putting the mould and the mould into a refrigerator with the temperature of-30 ℃ for freezing for 8 hours.
Comparative example
Comparative example 1
A method for preparing a super-elastic double-layered photo-thermal hydrogel having high mechanical strength was performed as in example 2, except that cellulose fibers were not added to the raw materials.
Referring to fig. 10, it can be seen that the superelastic hydrogel with cellulose fibers in example 2 can be restored after being subjected to a heavy load of 1500g, whereas the hydrogel without cellulose fibers in comparative example 1 has a structure severely damaged after being subjected to a heavy load of 1500 g.
Claims (9)
1. A preparation method of super-elastic double-layer photo-thermal hydrogel with high mechanical strength is characterized by comprising the following steps:
1) Immersing the delignified wood block into a sodium hydroxide solution with the concentration of 4-6%; stirring for 4-6 h at 75-80 ℃ to obtain suspension, cooling the suspension to room temperature, filtering, washing with deionized water to neutrality to obtain log fibers; freezing for 4-8 h at-15 to-30 ℃, and then carrying out vacuum freeze drying for 36-72 h at-40 to-65 ℃ to obtain cellulose fibers;
2) Mixing polyvinyl alcohol with deionized water to obtain a polyvinyl alcohol aqueous solution with the mass percentage concentration of 2-4%; then adding the cellulose fiber obtained in the step 1), dispersing, adding a cross-linking agent and a catalyst, and stirring at room temperature to obtain a mixed solution; wherein the mass ratio of the polyvinyl alcohol to the cellulose fiber is 1-3; the volume ratio of the cross-linking agent to the catalyst to the polyvinyl alcohol aqueous solution is 1: 80 to 100 portions; equally dividing the mixed solution into an A part and a B part, wherein a light absorbent is added into the B part;
3) Pouring the part A into a mold, placing the part A into liquid nitrogen for directional freezing, then pouring the part B into the same mold, and performing directional freezing in the liquid nitrogen until the gel is completely frozen; then freezing the gel together with the mould for 8h at the temperature of-15 ℃ to-30 ℃, taking out the gel, unfreezing the gel at room temperature, and soaking the gel in deionized water until the gel is neutral to obtain the super-elastic double-layer photo-thermal hydrogel.
2. The method for preparing the super-elastic double-layer photothermal hydrogel with high mechanical strength according to claim 1, wherein the delignified wood block in the step 1) is prepared by the following method: adding 8-12 g of sodium chlorite and 2-3 mL of acetic acid into 400-600 mL of deionized water, mixing and stirring; and then immersing the cut wood blocks into the solution, stirring for 6-8 h at the constant temperature of 90-100 ℃ to obtain a mixed solution, cooling the mixed solution to room temperature, filtering, washing with deionized water to be neutral, and thus obtaining the delignified wood blocks.
3. The method for preparing the super-elastic double-layered photothermal hydrogel having high mechanical strength according to claim 2, wherein the cut wood block has a volume of 10 x 5 x 1mm and a mass of 8 to 12g.
4. The method for preparing the super-elastic double-layered photothermal hydrogel with high mechanical strength according to claim 2, wherein said wood block is xylem part of any woody plant.
5. The method for preparing a superelastic double layer photothermal hydrogel according to claim 1, wherein said crosslinking agent in step 2) is glutaraldehyde.
6. The method for preparing a superelastic double layer photothermal hydrogel according to claim 1, wherein said catalyst in step 2) is 1.2mol/L hydrochloric acid.
7. The method for preparing the superelastic double layer photo-thermal hydrogel having high mechanical strength according to claim 1, wherein the light absorbent in step 2) is one or more of MXene material, conjugated polymer material, carbon-based material and biomass charcoal;
the MXene material is one or more of any novel transition metal carbon/nitride two-dimensional nano layered materials;
the conjugated polymer material is one or more of polypyrrole and polydopamine;
the carbon-based material is one or more of graphene, carbon nano tubes, carbon fibers, fullerene and porous carbon materials;
the biomass charcoal is one or more of natural black materials of roots, stems, leaves and outer skins of plants after high-temperature carbonization and cuttlefish meal.
8. A super-elastic double-layered photothermal hydrogel having high mechanical strength, which is prepared by the method for preparing a super-elastic double-layered photothermal hydrogel having high mechanical strength according to any one of claims 1 to 7.
9. Use of the high mechanical strength superelastic bi-layer photothermal hydrogel of claim 8 in solar driven interfacial evaporation, photothermal desalination, sewage treatment.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116515146A (en) * | 2023-05-06 | 2023-08-01 | 陕西科技大学 | Multifunctional film material with cellulose/graphene-Mxene hybrid interweaving structure and preparation method thereof |
| CN116925421A (en) * | 2023-07-17 | 2023-10-24 | 陕西科技大学 | Thermal insulation foam material based on cellulose-muscovite-zinc oxide and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116515146A (en) * | 2023-05-06 | 2023-08-01 | 陕西科技大学 | Multifunctional film material with cellulose/graphene-Mxene hybrid interweaving structure and preparation method thereof |
| CN116925421A (en) * | 2023-07-17 | 2023-10-24 | 陕西科技大学 | Thermal insulation foam material based on cellulose-muscovite-zinc oxide and preparation method thereof |
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