CN117998830B - Preparation method of functional reduced graphene oxide/metal-polyphenol framework composite aerogel - Google Patents
Preparation method of functional reduced graphene oxide/metal-polyphenol framework composite aerogel Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 126
- 239000004964 aerogel Substances 0.000 title claims abstract description 70
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 100
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 22
- 150000008442 polyphenolic compounds Chemical class 0.000 claims abstract description 21
- 235000013824 polyphenols Nutrition 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 18
- 230000009467 reduction Effects 0.000 claims abstract description 13
- 239000012266 salt solution Substances 0.000 claims abstract description 13
- 239000011358 absorbing material Substances 0.000 claims abstract description 12
- 238000001338 self-assembly Methods 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000001263 FEMA 3042 Substances 0.000 claims description 58
- 229940033123 tannic acid Drugs 0.000 claims description 58
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- 229940074391 gallic acid Drugs 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 14
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 13
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 13
- 235000015523 tannic acid Nutrition 0.000 claims description 13
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 13
- 238000004108 freeze drying Methods 0.000 claims description 11
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- 150000003839 salts Chemical class 0.000 claims description 7
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- 238000002604 ultrasonography Methods 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 20
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- 239000010949 copper Substances 0.000 description 18
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- 239000012188 paraffin wax Substances 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 229920002079 Ellagic acid Polymers 0.000 description 8
- 229960002852 ellagic acid Drugs 0.000 description 8
- 238000009210 therapy by ultrasound Methods 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
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- 230000010287 polarization Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- AFSDNFLWKVMVRB-UHFFFAOYSA-N Ellagic acid Chemical compound OC1=C(O)C(OC2=O)=C3C4=C2C=C(O)C(O)=C4OC(=O)C3=C1 AFSDNFLWKVMVRB-UHFFFAOYSA-N 0.000 description 2
- ATJXMQHAMYVHRX-CPCISQLKSA-N Ellagic acid Natural products OC1=C(O)[C@H]2OC(=O)c3cc(O)c(O)c4OC(=O)C(=C1)[C@H]2c34 ATJXMQHAMYVHRX-CPCISQLKSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- 230000007123 defense Effects 0.000 description 2
- 230000005672 electromagnetic field Effects 0.000 description 2
- 230000005670 electromagnetic radiation Effects 0.000 description 2
- 235000004132 ellagic acid Nutrition 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- FAARLWTXUUQFSN-UHFFFAOYSA-N methylellagic acid Natural products O1C(=O)C2=CC(O)=C(O)C3=C2C2=C1C(OC)=C(O)C=C2C(=O)O3 FAARLWTXUUQFSN-UHFFFAOYSA-N 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229920001864 tannin Polymers 0.000 description 2
- 239000001648 tannin Substances 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
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- 238000002156 mixing Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a functional reduced graphene oxide/metal-polyphenol framework composite aerogel wave-absorbing material and a preparation method thereof, belonging to the technical field of wave-absorbing material preparation, wherein the preparation method comprises the following steps: (1) Preparing graphene oxide solution with concentration of 5-10mg/mL, polyphenol solution with concentration of 5-30mg/mL and metal salt solution with concentration of 5-30mg/mL respectively. (2) Under the stirring state, firstly adding a metal salt solution into a polyphenol solution to obtain a metal-polyphenol framework solution, then adding the metal-polyphenol framework solution into a graphene oxide solution, and adding ammonia water to adjust the pH value to 8-11 to obtain uniform slurry. (3) Transferring the slurry into a tetrafluoroethylene reaction kettle, and performing hydrothermal reduction self-assembly reaction at 200 ℃ for 24 hours to obtain gel. (4) And drying the obtained gel to obtain the reduced graphene oxide/metal-polyphenol framework composite aerogel. The method is simple to operate and environment-friendly, and the obtained aerogel has the functions of wave absorption, water repellency, heat insulation and the like.
Description
Technical Field
The invention relates to the technical field of wave-absorbing material preparation, in particular to a functional reduced graphene oxide/metal-polyphenol framework composite aerogel wave-absorbing material and a preparation method thereof.
Background
With the continuous progress of electronic information and communication technology, the use of electronic devices has led to wider application fields of electromagnetic waves. The electronic equipment such as a mobile phone, a computer and the like is used, so that the work and the life of people are more efficient, convenient and intelligent. The use of radar detection and satellite positioning in the field of national defense greatly enhances the security of national defense. However, with the widespread use of these electronic devices, problems are also brought about, and the electronic devices generate excessive electromagnetic radiation, which not only seriously affects the physical health of people, but also interferes with the safety problems such as the normal operation of the precision instruments and equipment and information leakage. Therefore, developing a high-performance wave-absorbing material with light weight, thin thickness, strong absorption capacity and wide absorption frequency band is important to solve the electromagnetic radiation problem.
The traditional wave-absorbing material needs higher density, higher filling rate and thicker thickness to achieve the wave-absorbing effect, thereby limiting the application field. Compared with the prior art, the reduced graphene oxide is taken as one of novel carbon materials, and has the advantages of large specific surface area, low density, good chemical stability, adjustable conductivity, strong dielectric loss capacity and the like, so that the reduced graphene oxide is widely focused in the field of wave-absorbing materials. However, pure reduced graphene oxide has high dielectric characteristics and is free from magnetism, so that the problems of poor impedance matching, single loss mechanism, poor wave absorption performance, narrow absorption bandwidth and the like are caused. Many studies improve the impedance matching and loss mechanisms of reduced graphene oxide by rationally designing the microstructure and selecting complementary components to construct a composite.
Compared with the powder-shaped composite wave-absorbing material, the aerogel has the advantages of simple preparation, light weight, high porosity, large specific surface area and the like, so that researchers are applied to the wave-absorbing field. The aerogel structure not only can retain the inherent characteristics of the reduced graphene oxide, but also can overcome the problems of stacking of the reduced graphene oxide sheets and poor impedance matching. In recent years, aerogels prepared by compositing magnetic nanoparticles with reduced graphene oxide exhibit excellent wave-absorbing properties. Cao et al prepared Ni-MOF-RGO aerogel by hydrothermal treatment and freeze drying, the minimum reflection loss reached-51.19 dB at a matching thickness of 1.9mm, and the effective absorption band reached 6.32GHz at a matching thickness of 2.3mm (ACS APPLIED MATERIALS & interfaces. 2023, 15, 9685-9696). However, such aerogels are complex to prepare, environmentally unfriendly and not suitable for complex environments.
Generally, excellent wave absorbing materials have functions of water repellency, heat insulation, and the like in addition to good electromagnetic wave absorption properties, so as to be used in complex and severe practical application environments. For example, the wave-absorbing material with heat insulation performance and hydrophobic performance is used on an aircraft, so that the invasion of water can be reduced to ensure the normal operation of electronic components. According to the invention, the graphene oxide is dispersed by using polyphenol, and the functional reduced graphene oxide/metal-polyphenol composite aerogel is obtained through hydrothermal reduction and drying, so that the aerogel has the characteristics of low density, light weight and the like, has the functions of water repellency, heat insulation and the like, and can realize efficient wave absorption under the condition of low addition. The introduction of polyphenol can prevent graphene oxide sheets from stacking, is beneficial to the formation of a three-dimensional porous structure of aerogel, and reduces the material density. The framework formed by the metal-polyphenol can be distributed among the reduced graphene oxide sheets, so that the impedance matching of the reduced graphene oxide is improved, a heterogeneous interface is formed, the interface polarization and dipole polarization are enhanced under the action of an alternating electromagnetic field, the dielectric loss is improved, and the wave absorbing performance is improved. The preparation process is simple, green and environment-friendly, has low equipment requirement and strong controllability, and is a material with wide application prospect.
Disclosure of Invention
The invention aims to provide a preparation method of a reduced graphene oxide/metal-polyphenol framework composite aerogel wave-absorbing material which has low density and functionality and excellent wave-absorbing performance under low addition amount, and the preparation method is simple in preparation process, environment-friendly, easy in raw material acquisition and low in equipment requirement.
In order to achieve the above object, the present invention is realized by the following technical scheme: the preparation method of the functional reduced graphene oxide/metal-polyphenol framework composite aerogel comprises the following steps:
s1, respectively preparing graphene oxide solution with the concentration of 5-10mg/mL, polyphenol solution with the concentration of 5-30mg/mL and metal salt solution with the concentration of 5-30 mg/mL;
S2, under the stirring state, firstly adding a metal salt solution into a polyphenol solution to obtain a metal-polyphenol solution, then adding the metal-polyphenol solution into a graphene oxide solution, and adding ammonia water to adjust the pH to 8-11 to obtain uniform slurry;
s3, transferring the slurry into a tetrafluoroethylene reaction kettle, and performing hydrothermal reduction self-assembly reaction for 24 hours at 200 ℃ to obtain reduced graphene oxide/metal-polyphenol framework gel;
S4, drying the obtained reduced graphene oxide/metal-polyphenol framework gel to obtain reduced graphene oxide/metal-polyphenol framework composite aerogel;
Preferably, the metal salt is water-soluble multivalent salt, wherein the metal ion is one or a combination of several of Fe 2+、Co2+、Ni2+、Cu2+、Zn2 +、Fe3+, the metal salt is one of sulfate, chloride and nitrate, and the polyphenol is one or a combination of several of tannic acid, gallic acid and mashed acid.
Preferably, in S1, ultrasound is applied to the graphene oxide solution, the ultrasound power is 400-600W, the ultrasound frequency is 25-35 kHz, and the ultrasound is conducted for 2-4 hours.
Preferably, in S1, the solvent of the graphene oxide solution is a mixed solution of water and ethanol, wherein the volume of water is ethanol volume=1:1-3:1, and the solvents of the polyphenol solution and the metal salt solution are deionized water.
Preferably, in S1, the polyphenol solution volume: metal salt solution volume=1:1 to 1:5, graphene oxide solution volume: volume of polyphenol solution: metal salt solution volume=1:1:1 to 6:1:5.
Preferably, in the step S4, the drying method is freeze drying, and the drying temperature is-50 to-60 ℃.
Preferably, the metal-polyphenol is one or more of Fe 2+ -tannic acid, co 2+ -tannic acid, ni 2+ -tannic acid, cu 2+ -tannic acid, zn 2+ -tannic acid, fe 3+ -tannic acid, fe 2+ -mashed acid, co 2+ -mashed acid, ni 2+ -mashed acid, cu 2+ -mashed acid, zn 2+ -mashed acid, fe 3+ -mashed acid, fe 2+ -gallic acid, co 2+ -gallic acid, ni 2+ -gallic acid, cu 2+ -gallic acid, zn 2+ -gallic acid and Fe 3+ -gallic acid.
The invention comprises at least the following excellent effects:
(1) The reduced graphene oxide/metal-polyphenol framework composite aerogel provided by the invention is prepared from graphene oxide, polyphenol and soluble metal salt serving as raw materials, water and ethanol serving as green solvents, wherein the graphene oxide is uniformly dispersed through the cohesiveness of the polyphenol to the graphene oxide, and then the graphene oxide/metal-polyphenol framework composite aerogel is combined together through the coordination complexing action of the polyphenol and metal ions, and is subjected to hydrothermal reduction and self-assembly to obtain the reduced graphene oxide/metal-polyphenol framework composite aerogel. The preparation process is simple, the polyphenol is used as a biomass raw material, is environment-friendly and can be operated repeatedly, and the environment-friendly requirement of the prior art is met.
(2) According to the reduced graphene oxide/metal-polyphenol framework composite aerogel, polyphenol is used as an adhesive, so that graphene oxide can be dispersed to form a gel porous structure, the material density is reduced, the reduced graphene oxide and the metal-polyphenol framework can be bonded, and the impedance matching property of the reduced graphene oxide is improved. The conductive network formed by the three-dimensional porous structure of the reduced graphene oxide and the metal-polyphenol framework can promote electron migration and jump to enhance resistance loss, oxygen vacancies and defects of the metal-polyphenol framework can be used as polarization centers to induce dipole polarization, and finally, heterogeneous interfaces formed by the reduced graphene oxide and the metal-polyphenol can cause electron aggregation at the heterogeneous interfaces under the action of an alternating electromagnetic field to enhance interface polarization.
(3) The reduced graphene oxide/metal-polyphenol framework composite aerogel provided by the invention has the functions of wave absorption, hydrophobicity (water contact angle is 120-150 ℃), heat insulation and the like.
(4) The density of the reduced graphene oxide/metal-polyphenol framework composite aerogel is 20-50 mg/cm 3, and broadband strong absorption (the effective absorption bandwidth is 3-7 GHz, and the minimum reflection loss is-20 to-70 dB) can be realized under the condition of low addition (5-15 wt%).
Drawings
FIG. 1 is a digital photograph of reduced graphene oxide/Co 2+ -tannin framework composite aerogel prepared in example 1 of the present invention.
FIG. 2 is a graph showing the reflection loss of the reduced graphene oxide/Co 2+ -tannin framework composite aerogel prepared in example 1 of the present invention at a matching thickness of 1-5 mm.
Fig. 3 is a graph showing the effect of water contact angle of the reduced graphene oxide/Co 2+ -tannic acid framework composite aerogel prepared in example 1 of the present invention.
Fig. 4 is a graph showing the heat insulation effect of the reduced graphene oxide/Co 2+ -tannic acid framework composite aerogel prepared in example 1 of the present invention after 60 minutes at a 100 ℃ heat stage.
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. Those skilled in the art, having the benefit of this disclosure, will appreciate that various modifications, adaptations, and variations can be made to the techniques taught by the present disclosure without departing from the spirit and scope of the present disclosure.
Test method
And an N5230A type vector network analyzer is adopted to test electromagnetic parameters of the sample, and the testing method is a coaxial method. Uniformly mixing a sample to be tested with paraffin according to a certain proportion, and pressing into a circular ring with the inner diameter of 3mm, the outer diameter of 7mm and the thickness of 2 mm. Testing electromagnetic parameters in the range of 2-18GHz, fitting by Matlab, and analyzing; measuring the hydrophobicity of the reduced graphene oxide/metal-polyphenol framework composite aerogel by adopting a THX-05 type full-automatic contact angle determinator; and carrying out heat insulation performance analysis by adopting a VanoCam-HD RESEARCH980 type infrared thermal imaging system.
Example 1: s1, preparing 30mL of graphene oxide solution with the concentration of 5mg/mL (the volume of water is equal to the volume of ethanol=2:1), 5mL of tannic acid solution with the concentration of 7.5mg/mL and 5mL of cobalt chloride hexahydrate solution with the concentration of 7.5mg/mL, and performing ultrasonic treatment on the graphene oxide solution for 2 hours under a 600W ultrasonic cleaner;
S2, under the stirring state, adding a cobalt chloride solution into a tannic acid solution to obtain a Co 2+ -tannic acid solution, then adding the Co 2+ -tannic acid solution into a graphene oxide solution, and adding ammonia water to adjust the pH value to 9 to obtain uniform slurry;
S3, transferring the slurry into a tetrafluoroethylene reaction kettle, and performing hydrothermal reduction self-assembly reaction for 24 hours at 200 ℃ to obtain reduced graphene oxide/Co 2+ -tannic acid framework gel;
S4, freeze-drying the obtained reduced graphene oxide/Co 2+ -tannic acid framework gel at the temperature of 50 ℃ below zero to obtain reduced graphene oxide/Co 2+ -tannic acid framework composite aerogel;
fig. 1 is a digital photograph of the reduced graphene oxide/Co 2+ -tannic acid framework composite aerogel prepared in example 1, fig. 2 is a wave absorbing performance curve of the reduced graphene oxide/Co 2+ -tannic acid framework composite aerogel prepared in example 1 when the addition amount of the reduced graphene oxide/Co 2+ -tannic acid framework composite aerogel in paraffin is 8wt%, fig. 3 is a water contact angle effect graph of the reduced graphene oxide/Co 2+ -tannic acid framework composite aerogel prepared in example 1, and fig. 4 is a heat insulation effect graph of the reduced graphene oxide/Co 2+ -tannic acid framework composite aerogel prepared in example 1 after 60 minutes at a 100 ℃ heat stage; as can be seen from fig. 2, the reduced graphene oxide/Co 2+ -tannic acid framework composite aerogel exhibits excellent wave absorbing performance, the minimum reflection loss of the aerogel is-64.31 dB when the additive amount of the aerogel in paraffin is 8wt%, the minimum reflection loss is-64.31 dB when the matching thickness is 3.7mm, the effective absorption frequency bandwidth is 6.16GHz when the matching thickness is 2.47mm, and the effective absorption frequency bandwidth covers 12.8GHz (5.2-18 GHz) when the thickness is 1-5 mm;
As can be seen from fig. 3, the reduced graphene oxide/Co 2+ -tannic acid framework aerogel has a water contact angle of 134.9 ° and good hydrophobic properties; as can be seen from fig. 4, the reduced graphene oxide/Co 2+ -tannic acid framework aerogel has excellent heat insulation performance after being subjected to a heat stage of 100 ℃ for 1 hour at a surface temperature of 36.3 ℃.
Example 2: s1, preparing 30mL of graphene oxide solution with the concentration of 5mg/mL (the volume of water is ethanol volume=3:1), 5mL of tannic acid solution with the concentration of 5mg/mL and 5mL of nickel nitrate hexahydrate solution with the concentration of 5mg/mL, and performing ultrasonic treatment on the graphene oxide solution for 2 hours under a 600W ultrasonic cleaning machine;
S2, under the stirring state, firstly adding a nickel nitrate solution into a tannic acid solution to obtain a Ni 2+ -tannic acid solution, then adding the Ni 2+ -tannic acid solution into a graphene oxide solution, and adding ammonia water to adjust the pH value to 9 to obtain uniform slurry;
S3, transferring the slurry into a tetrafluoroethylene reaction kettle, and performing hydrothermal reduction self-assembly reaction for 24 hours at 200 ℃ to obtain reduced graphene oxide/Ni 2+ -tannic acid framework gel;
S4, freeze-drying the obtained reduced graphene oxide/Ni 2+ -tannic acid framework gel at the temperature of 50 ℃ below zero to obtain reduced graphene oxide/Ni 2+ -tannic acid framework composite aerogel;
The density of the reduced graphene oxide/Ni 2+ -tannic acid framework composite aerogel is 33mg/cm 3, the water contact angle is 130 degrees, and the heat insulation effect is as follows: after 1h, the surface temperature is 37 ℃; when the addition amount of the aerogel in paraffin is 8wt%, the minimum reflection loss is-49 dB when the matching thickness is 4.4mm, and the effective absorption frequency bandwidth is 5.9GHz.
Example 3: s1, preparing 20mL of graphene oxide solution with the concentration of 8mg/mL (the volume of water is ethanol volume=1:1), 10mL of tannic acid solution with the concentration of 10mg/mL and 10mL of copper sulfate pentahydrate solution with the concentration of 10mg/mL, and performing ultrasonic treatment on the graphene oxide solution for 2 hours under a 600W ultrasonic cleaning machine;
S2, under the stirring state, firstly adding a copper sulfate solution into a tannic acid solution to obtain a Cu 2+ -tannic acid solution, then adding the Cu 2+ -tannic acid solution into a graphene oxide solution, and adding ammonia water to adjust the pH to 10 to obtain uniform slurry;
S3, transferring the slurry into a tetrafluoroethylene reaction kettle, and performing hydrothermal reduction self-assembly reaction for 24 hours at 200 ℃ to obtain reduced graphene oxide/Cu 2+ -tannic acid framework gel;
S4, freeze-drying the obtained reduced graphene oxide/Cu 2+ -tannic acid framework gel at the temperature of 50 ℃ below zero to obtain reduced graphene oxide/Cu 2+ -tannic acid framework composite aerogel;
The density of the reduced graphene oxide/Cu 2+ -tannic acid framework composite aerogel is 35mg/cm 3, the water contact angle is 136 degrees, and the heat insulation effect is as follows: after 1h, the surface temperature is 36 ℃; when the addition amount of the aerogel in paraffin is 5wt%, the minimum reflection loss is-43 dB when the matching thickness is 3mm, and the effective absorption frequency bandwidth is 4.2GHz.
Example 4: s1, preparing 30mL of graphene oxide solution with the concentration of 5mg/mL (the volume of water is equal to the volume of ethanol=2:1), 5mL of tannic acid solution with the concentration of 10mg/mL and 5mL of ferric chloride hexahydrate solution with the concentration of 10mg/mL, and performing ultrasonic treatment on the graphene oxide solution for 2 hours under a 600W ultrasonic cleaning machine;
S2, under the stirring state, firstly adding an iron chloride solution into a tannic acid solution to obtain an Fe 3+ -tannic acid solution, then adding the Fe 3+ -tannic acid solution into a graphene oxide solution, and adding ammonia water to adjust the pH value to 9 to obtain uniform slurry;
S3, transferring the slurry into a tetrafluoroethylene reaction kettle, and performing hydrothermal reduction self-assembly reaction for 24 hours at 200 ℃ to obtain reduced graphene oxide/Fe 3+ -tannic acid framework gel;
s4, freeze-drying the obtained reduced graphene oxide/Fe 3+ -tannic acid framework gel at the temperature of 50 ℃ below zero to obtain reduced graphene oxide/Fe 3+ -tannic acid framework composite aerogel;
The density of the reduced graphene oxide/Fe 3+ -tannic acid framework composite aerogel is 33mg/cm 3, the water contact angle is 133 degrees, and the heat insulation effect is as follows: after 1h, the surface temperature is 39 ℃; when the addition amount of the aerogel in paraffin is 10wt%, the minimum reflection loss is-47 dB when the matching thickness is 2.5mm, and the effective absorption frequency bandwidth is 4.4GHz.
Example 5: s1, preparing 30mL of graphene oxide solution with the concentration of 5mg/mL (water volume: ethanol volume=2:1), 5mL of gallic acid solution with the concentration of 10mg/mL and 5mL of zinc nitrate hexahydrate solution with the concentration of 10mg/mL, and performing ultrasonic treatment on the graphene oxide solution for 2 hours under a 600W ultrasonic cleaning machine;
S2, under the stirring state, firstly adding a zinc nitrate solution into a gallic acid solution to obtain a Zn 2+ -gallic acid solution, then adding the Zn 2+ -gallic acid solution into a graphene oxide solution, and adding ammonia water to adjust the pH to 9 to obtain uniform slurry;
S3, transferring the slurry into a tetrafluoroethylene reaction kettle, and performing hydrothermal reduction self-assembly reaction for 24 hours at 200 ℃ to obtain reduced graphene oxide/Zn 2+ -gallic acid framework gel;
S4, freeze-drying the obtained reduced graphene oxide/Zn 2+ -gallic acid framework gel at the temperature of 50 ℃ below zero to obtain reduced graphene oxide/Zn 2+ -gallic acid framework composite aerogel;
The density of the reduced graphene oxide/Zn 2+ -gallic acid framework composite aerogel is 35mg/cm 3, the water contact angle is 131 degrees, and the heat insulation effect is as follows: after 1h, the surface temperature is 37 ℃; when the addition amount of the aerogel in paraffin is 8wt%, the minimum reflection loss is-43 dB when the matching thickness is 3.5mm, and the effective absorption frequency bandwidth is 3.8GHz.
Example 6: s1, preparing 30mL of graphene oxide solution with the concentration of 5mg/mL (water volume: ethanol volume=2:1), 5mL of gallic acid solution with the concentration of 10mg/mL and 5mL of cupric chloride dihydrate with the concentration of 10mg/mL, and performing ultrasonic treatment on the graphene oxide solution for 2 hours under a 600W ultrasonic cleaning machine;
S2, under the stirring state, firstly adding a copper chloride solution into a gallic acid solution to obtain a Cu 2+ -gallic acid solution, then adding the Cu 2+ -gallic acid solution into a graphene oxide solution, and adding ammonia water to adjust the pH to 9 to obtain uniform slurry;
S3, transferring the slurry into a tetrafluoroethylene reaction kettle, and performing hydrothermal reduction self-assembly reaction for 24 hours at 200 ℃ to obtain reduced graphene oxide/Cu 2+ -gallic acid framework gel;
S4, freeze-drying the obtained reduced graphene oxide/Cu 2+ -gallic acid framework gel at the temperature of 50 ℃ below zero to obtain reduced graphene oxide/Cu 2+ -gallic acid framework composite aerogel;
the density of the reduced graphene oxide/Cu 2+ -gallic acid framework composite aerogel is 34mg/cm 3, the water contact angle is 130 degrees, and the heat insulation effect is as follows: after 1h, the surface temperature is 37 ℃; when the addition amount of the aerogel in paraffin is 5wt%, the minimum reflection loss is-38 dB when the matching thickness is 3.5mm, and the effective absorption frequency bandwidth is 4.2GHz.
Example 7: s1, preparing 30mL of graphene oxide solution with the concentration of 5mg/mL (the volume of water is equal to the volume of ethanol=2:1), 5mL of ellagic acid solution with the concentration of 10mg/mL and 5mL of cobalt nitrate hexahydrate solution with the concentration of 10mg/mL, and performing ultrasonic treatment on the graphene oxide solution for 2 hours under a 600W ultrasonic cleaning machine;
S2, under the stirring state, adding a cobalt nitrate solution into an ellagic acid solution to obtain a Co 2+ -ellagic acid solution, then adding the Co 2+ -ellagic acid solution into a graphene oxide solution, and adding ammonia water to adjust the pH value to 9 to obtain uniform slurry;
S3, transferring the slurry into a tetrafluoroethylene reaction kettle, and carrying out hydrothermal reduction self-assembly reaction for 24 hours at 200 ℃ to obtain reduced graphene oxide/Co 2+ -ellagic acid framework gel;
S4, freeze-drying the obtained reduced graphene oxide/Co 2+ -ellagic acid framework gel at the temperature of 50 ℃ below zero to obtain reduced graphene oxide/Co 2+ -ellagic acid framework composite aerogel;
The density of the reduced graphene oxide/Co 2+ -ellagic acid framework composite aerogel is 36mg/cm 3, the water contact angle is 131 degrees, and the heat insulation effect is as follows: after 1h, the surface temperature is 40 ℃; when the addition amount of the aerogel in paraffin is 15wt%, the minimum reflection loss is-41 dB when the matching thickness is 4mm, and the effective absorption frequency bandwidth is 4.8GHz.
Example 8: s1, preparing 30mL of graphene oxide solution (the volume of water is equal to the volume of ethanol=2:1), 5mL of mixed solution of tannic acid and gallic acid with the concentration of 20mg/mL, the mass ratio of tannic acid to gallic acid is 1:1,5mL of copper chloride dihydrate solution with the concentration of 10mg/mL, and ultrasonic treating the graphene oxide solution for 2 hours under a 600W ultrasonic cleaner;
S2, under the stirring state, firstly adding a copper chloride solution into tannic acid and gallic acid solution to obtain Cu 2+ -tannic acid-gallic acid solution, then adding the Cu 2+ -tannic acid-gallic acid solution into graphene oxide solution, and adding ammonia water to adjust the pH to 10 to obtain uniform slurry;
S3, transferring the slurry into a tetrafluoroethylene reaction kettle, and performing hydrothermal reduction self-assembly reaction for 24 hours at 200 ℃ to obtain reduced graphene oxide/Cu 2+ -tannic acid-gallic acid framework gel;
S4, freeze-drying the obtained reduced graphene oxide/Cu 2+ -tannic acid-gallic acid framework gel at the temperature of minus 60 ℃ to obtain reduced graphene oxide/Cu 2+ -tannic acid-gallic acid framework composite aerogel;
The density of the reduced graphene oxide/Cu 2+ -tannic acid-gallic acid framework composite aerogel is 38mg/cm 3, the water contact angle is 129 degrees, and the heat insulation effect is as follows: after 1h, the surface temperature is 39 ℃; when the addition amount of the aerogel in paraffin is 8wt%, the minimum reflection loss is-53 dB when the matching thickness is 3mm, and the effective absorption frequency bandwidth is 3.2GHz.
Claims (6)
1. The preparation method of the functional reduced graphene oxide/metal-polyphenol framework composite aerogel is characterized by comprising the following steps of:
s1, respectively preparing graphene oxide solution with the concentration of 5-10mg/mL, polyphenol solution with the concentration of 5-30mg/mL and metal salt solution with the concentration of 5-30 mg/mL;
s2, under the stirring state, firstly adding a metal salt solution into a polyphenol solution to obtain a metal-polyphenol framework solution, then adding the metal salt solution into a graphene oxide solution, and adding ammonia water to adjust the pH to 8-11 to obtain uniform slurry;
s3, transferring the slurry into a tetrafluoroethylene reaction kettle, and performing hydrothermal reduction self-assembly reaction for 24 hours at 200 ℃ to obtain reduced graphene oxide/metal-polyphenol framework gel;
s4, freeze-drying the obtained reduced graphene oxide/metal-polyphenol framework gel at the temperature of between 50 ℃ below zero and 60 ℃ below zero to obtain reduced graphene oxide/metal-polyphenol framework composite aerogel;
The density of the reduced graphene oxide/metal-polyphenol framework composite aerogel is 20-50 mg/cm 3, the water contact angle is 120-150 degrees, the minimum reflection loss of the aerogel is-20-70 dB when the aerogel is used as a wave absorbing material, and the effective wave absorbing bandwidth is 3-7 GHz.
2. The method for preparing reduced graphene oxide/metal-polyphenol framework composite aerogel according to claim 1, wherein the metal salt is water-soluble multivalent salt, wherein the metal ion is one or a combination of more than one of Fe 2+、Co2+、Ni2+、Cu2+、Zn2+、Fe3+, the metal salt is one of sulfate, chloride and nitrate, and the polyphenol is one or a combination of more than one of tannic acid, gallic acid and mashed acid.
3. The method for preparing reduced graphene oxide/metal-polyphenol framework composite aerogel according to claim 1, wherein ultrasound is applied to the graphene oxide solution, the ultrasonic power is 400-600W, the ultrasonic frequency is 25-35 kHz, and the ultrasonic time is 2-4 hours.
4. The method for preparing the reduced graphene oxide/metal-polyphenol framework composite aerogel according to claim 1, wherein the solvent of the graphene oxide solution is a mixture of water and ethanol, wherein the volume of water is ethanol volume=1:1-3:1, and the solvents of the polyphenol solution and the metal salt solution are deionized water.
5. The method of preparing a reduced graphene oxide/metal-polyphenol framework composite aerogel of claim 1, wherein the volume of the polyphenol solution: metal salt solution volume=1:1 to 1:5, graphene oxide solution volume: volume of polyphenol solution: metal salt solution volume=1:1:1 to 6:1:5.
6. The method of preparing a reduced graphene oxide/metal-polyphenol framework composite aerogel of claim 1, wherein the metal-polyphenol framework is one or a combination of Fe 2+ -tannic acid, co 2+ -tannic acid, ni 2+ -tannic acid, cu 2+ -tannic acid, zn 2+ -tannic acid, fe 3+ -tannic acid, fe 2+ -mashed acid, co 2+ -mashed acid, ni 2+ -mashed acid, cu 2+ -mashed acid, zn 2+ -mashed acid, fe 3+ -mashed acid, fe 2+ -gallic acid, co 2+ -gallic acid, ni 2+ -gallic acid, cu 2+ -gallic acid, zn 2+ -gallic acid, fe 3+ -gallic acid.
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