CN113215828A - Perforated graphene aerogel moisture absorption fiber, and preparation method and application thereof - Google Patents
Perforated graphene aerogel moisture absorption fiber, and preparation method and application thereof Download PDFInfo
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- CN113215828A CN113215828A CN202110649042.8A CN202110649042A CN113215828A CN 113215828 A CN113215828 A CN 113215828A CN 202110649042 A CN202110649042 A CN 202110649042A CN 113215828 A CN113215828 A CN 113215828A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 257
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 257
- 239000000835 fiber Substances 0.000 title claims abstract description 210
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 138
- 239000004964 aerogel Substances 0.000 title claims abstract description 133
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000002250 absorbent Substances 0.000 claims abstract description 38
- 230000002745 absorbent Effects 0.000 claims abstract description 38
- 238000005338 heat storage Methods 0.000 claims abstract description 12
- 238000005057 refrigeration Methods 0.000 claims abstract description 9
- 239000002657 fibrous material Substances 0.000 claims abstract description 6
- 230000004044 response Effects 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims description 37
- 238000001179 sorption measurement Methods 0.000 claims description 35
- 239000000017 hydrogel Substances 0.000 claims description 34
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 33
- 238000001035 drying Methods 0.000 claims description 25
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 18
- 239000003638 chemical reducing agent Substances 0.000 claims description 15
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 14
- 239000004973 liquid crystal related substance Substances 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- 238000009987 spinning Methods 0.000 claims description 12
- 238000002166 wet spinning Methods 0.000 claims description 12
- 238000005530 etching Methods 0.000 claims description 11
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 11
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 10
- 238000011049 filling Methods 0.000 claims description 10
- 239000000499 gel Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 238000004108 freeze drying Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 7
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 7
- 235000010323 ascorbic acid Nutrition 0.000 claims description 7
- 239000011668 ascorbic acid Substances 0.000 claims description 7
- 229960005070 ascorbic acid Drugs 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 7
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 6
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 230000001112 coagulating effect Effects 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 6
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 6
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 6
- 229960005055 sodium ascorbate Drugs 0.000 claims description 6
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims description 6
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000003486 chemical etching Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 5
- 229960003638 dopamine Drugs 0.000 claims description 5
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- 229910019626 (NH4)6Mo7O24 Inorganic materials 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 229910004619 Na2MoO4 Inorganic materials 0.000 claims description 3
- 229910020212 Na2SnO3 Inorganic materials 0.000 claims description 3
- 229910020350 Na2WO4 Inorganic materials 0.000 claims description 3
- 229910020700 Na3VO4 Inorganic materials 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910020881 PMo12O40 Inorganic materials 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 229910010252 TiO3 Inorganic materials 0.000 claims description 3
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- MMCPOSDMTGQNKG-UHFFFAOYSA-N anilinium chloride Chemical compound Cl.NC1=CC=CC=C1 MMCPOSDMTGQNKG-UHFFFAOYSA-N 0.000 claims description 3
- 238000000578 dry spinning Methods 0.000 claims description 3
- 229940012017 ethylenediamine Drugs 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 claims description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000011684 sodium molybdate Substances 0.000 claims description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 3
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 claims description 3
- IHIXIJGXTJIKRB-UHFFFAOYSA-N trisodium vanadate Chemical compound [Na+].[Na+].[Na+].[O-][V]([O-])([O-])=O IHIXIJGXTJIKRB-UHFFFAOYSA-N 0.000 claims description 3
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 3
- 238000004146 energy storage Methods 0.000 abstract description 6
- 238000005485 electric heating Methods 0.000 abstract description 5
- 238000004321 preservation Methods 0.000 abstract description 3
- 230000009102 absorption Effects 0.000 description 109
- 239000000463 material Substances 0.000 description 18
- 239000002131 composite material Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 9
- 239000011358 absorbing material Substances 0.000 description 7
- 230000008859 change Effects 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000013505 freshwater Substances 0.000 description 4
- 229940071870 hydroiodic acid Drugs 0.000 description 4
- 238000000352 supercritical drying Methods 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 230000000638 stimulation Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- -1 lithium chloride-activated carbon fiber Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
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- 239000012188 paraffin wax Substances 0.000 description 1
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- 238000009941 weaving Methods 0.000 description 1
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
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Abstract
The invention discloses a perforated graphene aerogel moisture absorption fiber which comprises a perforated graphene aerogel fiber and a moisture absorbent, wherein the perforated graphene aerogel fiber is a fiber material which is formed by overlapping perforated graphene sheets and has a three-dimensional porous network structure, and the moisture absorbent is wrapped on the perforated graphene sheets and embedded and filled in the three-dimensional porous network structure. The invention also discloses a preparation method and application of the perforated graphene aerogel moisture absorption fiber. The perforated graphene aerogel moisture absorption fiber disclosed by the invention has excellent performances such as flexibility, weavability, moisture absorption, electric heating, photo-thermal energy storage and the like, so that the perforated graphene aerogel moisture absorption fiber can be used for preparing devices for moisture absorption and heat preservation, air water taking, intelligent response, moisture absorption and heat storage, moisture absorption and refrigeration and microwave absorption or flexible wearable devices.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a perforated graphene aerogel moisture absorption fiber, a preparation method thereof and application thereof in the fields of adsorption/absorption type air water taking, moisture absorption and energy storage, microwave absorption and the like.
Background
Currently, many regions of the world face this severe shortage of fresh water. Research has shown that two thirds of the world's population (40 billion people) suffer from a fresh water shortage in one year, while 5 billion people on earth are facing serious water shortage problems all year round. The requirement for water supply by building large-scale infrastructures such as large dams, pipeline transportation or water treatment plants is a main means for solving the problem of water resource shortage in most countries so far, but in remote areas with shortage of traditional freshwater resources, the distributed small-scale water taking technology is more practical due to the fact that the large-scale infrastructures such as large power equipment are not provided.
The adsorption/absorption type air water taking method is that hydroscopic adsorption/absorption agent is used to capture water vapor molecules in air, the water vapor molecules are stored in water absorbent material, after a period of time, the adsorption/absorption agent is heated and regenerated, so that the water vapor in the water vapor is released again, and fresh water is obtained after condensation. Because the partial pressure of water vapor in the atmospheric environment is lower, the lower condensation temperature is needed by adopting direct cooling, and the partial pressure of the water vapor of the desorbed wet air is greatly improved after the adsorption and desorption process, therefore, the adsorption/absorption system essentially improves the partial pressure of the water vapor in the air, namely, the dew point, compared with the direct cooling water taking, the energy consumption of the adsorption/absorption type water taking is lower and the water taking efficiency is higher under the same condensation temperature.
Chinese patent publication No. CN106013330A discloses an air water intake system, which mainly comprises an adsorption bed, a cover plate, a housing, a condenser, a fan, a heater, etc., wherein the adsorption bed is filled with a lithium chloride-activated carbon fiber felt solidified adsorbent, and is filled with a wavy and flat adsorbent in an alternating filling manner, thereby adsorbing moisture in the air. However, such an air intake system has a problem of low adsorption efficiency. Chinese patent publication No. CN103225331A discloses a microfluidic air water intake device and a water intake method, which are used to automatically control the water intake method of the microfluidic air water intake device, so as to achieve the purpose of efficiently taking water, and compared with the existing water intake device, the water intake efficiency is improved by 30% in comparison. However, the microfluidic air water taking device has the problems of complex processing technology and incapability of large-scale mass production.
Disclosure of Invention
The invention aims to provide a perforated graphene aerogel moisture absorption fiber and a preparation method thereof, so as to overcome the defects of the prior art.
In order to solve the technical problems, a first aspect of the present invention provides a perforated graphene aerogel moisture absorption fiber, including a perforated graphene aerogel fiber and a moisture absorbent, wherein the perforated graphene aerogel fiber is a fiber material formed by overlapping perforated graphene sheets and having a three-dimensional porous network structure, and the moisture absorbent is wrapped on the perforated graphene sheets and embedded in and filled in the three-dimensional porous network structure.
Further, in the perforated graphene aerogel moisture absorption fibers, the content of the perforated graphene aerogel fibers is 10-70 wt%, and the porosity of the three-dimensional porous network structure is 1-99%;
the diameter of the perforated graphene aerogel fiber is 10 mu m-1 mm, and the length-diameter ratio is 10-107The specific surface area is 1 to 1200m2The pore volume is 0.1-16 cm3/g。
Furthermore, the perforated graphene sheet layer is provided with nanoscale holes, and the size of the nanoscale holes is 1-50 nm.
Further, in the perforated graphene aerogel moisture absorption fiber, the content of a moisture absorbent is 1-99 wt.%;
the moisture absorbent comprises any one or combination of more of lithium chloride, calcium chloride, ferric chloride, copper nitrate, nickel nitrate, ferric sulfate, lithium sulfate, sodium carbonate, sodium sulfate, copper chloride, nickel acetate and magnesium sulfate.
Furthermore, the water vapor adsorption capacity of the perforated graphene aerogel moisture absorption fibers is 0.1-4.5 g/g.
The second aspect of the invention provides a preparation method of the perforated graphene aerogel moisture absorption fiber, which comprises the following steps:
providing perforated graphene hydrogel fibers or perforated graphene aerogel fibers; and
and filling the perforated graphene hydrogel fiber or the perforated graphene aerogel fiber with a moisture absorbent in a solution filling mode, so that the moisture absorbent enters and is filled in a three-dimensional porous network structure of the gel fiber, and drying to obtain the perforated graphene aerogel moisture absorbent fiber.
Further, the perforated graphene hydrogel fiber is prepared from a perforated graphene oxide dispersion liquid through a spinning method, and the perforated graphene aerogel fiber is obtained by drying the perforated graphene hydrogel fiber;
the perforated graphene oxide is obtained by etching graphene oxide by a chemical etching method, and the adopted etching agent comprises potassium hydroxide, nitric acid, hydrogen peroxide and SnO2、Na2MoO4、Na2WO4、NaAlO2、Na2SnO3、K2TiO3、KMnO4、Na3VO4、(NH4)6Mo7O24、H3PMo12O40Any one of the above;
the spinning method comprises any one of wet spinning, limited sol-gel reaction and freeze-dry spinning; the drying treatment is freeze drying or supercritical fluid drying.
Further, the chemical etching method for etching graphene oxide specifically includes: mixing the graphene oxide aqueous solution with a hydrogen peroxide aqueous solution, and etching at 90-100 ℃ for 0.5-5 h to obtain perforated graphene oxide; the concentration of the graphene oxide aqueous solution is 1-10 mg/ml;
the wet spinning method comprises the following specific steps: injecting the perforated graphene oxide liquid crystal into a coagulating bath through a needle, and collecting and reducing to obtain perforated graphene hydrogel fibers; wherein the content of graphene oxide in the perforated graphene oxide liquid crystal is 0.01-10 wt%; the inner diameter of the needle head is 30 mu m-5 mm; the coagulating bath comprises calcium chloride solution, aniline hydrochloride solution, dilute hydrochloric acid, dilute sulfuric acid, sodium hydroxide water and ethylAny one or more of alcohol mixed solution, sodium hydroxide water and tert-butyl alcohol mixed solution and reducing agent solution; the reducing agent comprises hydriodic acid, ascorbic acid, sodium ascorbate, hydrazine hydrate, ethylenediamine and Fe-containing2+A combination of any one or more of the compounds and dopamine;
the limited-area sol-gel reaction specifically comprises the following steps:
placing the graphene oxide aqueous solution in a closed container, and reacting at 100-180 ℃ for 12-24 h to obtain the perforated graphene hydrogel fiber; wherein the concentration of the graphene oxide aqueous solution is 1-10 mg/mL;
or placing the mixed aqueous solution containing the graphene oxide and the reducing agent in a closed container, and reacting at the temperature of 30-95 ℃ for 1-12 hours to obtain the perforated graphene hydrogel fiber; the mass ratio of the graphene oxide to the reducing agent is 1: 20-20: 1; the reducing agent comprises hydriodic acid, ascorbic acid, sodium ascorbate, dopamine, ethylenediamine, hydrazine hydrate, sodium borohydride and Fe2+Any one or combination of more of the compounds.
Further, the solution filling specifically comprises: soaking the perforated graphene hydrogel fiber or the perforated graphene aerogel fiber in a moisture absorbent solution for 1-24 h, taking out and drying to obtain the perforated graphene aerogel moisture absorption fiber; wherein the moisture absorbent content in the moisture absorbent solution is 1-70 wt.%; the drying mode comprises drying at the normal pressure of 80-120 ℃ and vacuum freeze drying.
The third aspect of the invention also provides application of the perforated graphene aerogel moisture absorption fiber in preparation of devices or flexible wearable devices for moisture absorption and warm keeping, air water taking, intelligent response, moisture absorption and heat storage, moisture absorption and refrigeration and microwave absorption.
Compared with the prior art, the technical scheme of the invention has the following advantages:
1. the moisture absorption fiber mainly comprises a perforated graphene aerogel fiber and a moisture absorption material, wherein the perforated graphene aerogel fiber has a continuous three-dimensional porous network structure and has an adjustable diameter and a large length-diameter ratio, and the moisture absorption material is wrapped on a graphene sheet layer and exists in a porous structure formed by overlapping the graphene sheet layer. The moisture absorption fiber has excellent electric heating, photo-thermal, energy storage, weaving performance, flexibility and hydrophilicity, and adjustable moisture absorption material load capacity, water vapor adsorption rate and adsorption capacity.
2. The perforated graphene aerogel moisture absorption fiber disclosed by the invention is simple in preparation process, mild and controllable in reaction conditions, low in energy consumption, green and pollution-free, and suitable for large-scale production.
3. The perforated graphene aerogel moisture absorption fiber can be applied to multiple fields of moisture absorption and heat preservation, air water taking, moisture absorption and heat storage/refrigeration, intelligent response, microwave absorption, flexible wearable devices and the like, and has wide application prospects.
Drawings
Fig. 1 is a schematic structural view of a perforated graphene aerogel hygroscopic fiber in an exemplary embodiment of the present invention.
Fig. 2 is a scanning electron microscope photograph of the perforated graphene aerogel hygroscopic fiber prepared in example 1 of the present invention.
Fig. 3 is a contact angle photograph of the perforated graphene aerogel hygroscopic fiber prepared in example 1 of the present invention.
FIG. 4 is a graph showing the absorption kinetics of absorbent fibers prepared in example 5 of the present invention and in comparative example 1.
Fig. 5 is a moisture absorption kinetic curve of the perforated graphene aerogel moisture absorption fiber prepared in example 1 of the present invention at room temperature under different relative humidities.
Fig. 6 is a temperature change curve of the perforated graphene aerogel moisture absorption fiber prepared in example 1 of the present invention under sunlight irradiation.
Fig. 7 is a temperature variation curve of the perforated graphene aerogel moisture absorption fiber prepared in example 1 of the present invention under different voltage stimuli.
Fig. 8 is a graph of the cycle efficiency of the perforated graphene aerogel hygroscopic fiber prepared in example 1 of the present invention under light and electrical stimulation.
Fig. 9 is an adsorption isotherm of the perforated graphene aerogel hygroscopic fiber prepared in example 1 of the present invention for water vapor at different temperatures.
Fig. 10 is a graph showing the change of the average adsorption enthalpy of the porous graphene aerogel moisture absorption fiber prepared in example 1 of the present invention with the adsorption amount.
Fig. 11 is a curve of the change of the heat storage capacity of the porous graphene aerogel moisture absorption fiber prepared in example 1 of the present invention with the adsorption capacity.
Fig. 12 shows the adsorption refrigeration efficiency and the adsorption heat storage efficiency of the perforated graphene aerogel moisture absorption fiber prepared in example 1 of the present invention.
Fig. 13 is a microwave absorption curve of the perforated graphene aerogel moisture absorption fiber prepared in example 1 of the present invention under different moisture absorption amounts.
Detailed Description
The invention provides a perforated graphene aerogel moisture absorption fiber. Referring to fig. 1, the perforated graphene aerogel moisture absorption fiber is composed of perforated graphene aerogel fibers and a moisture absorbent, wherein the perforated graphene aerogel fibers are made of a fiber material having a three-dimensional porous network structure and formed by overlapping perforated graphene sheets, and the moisture absorbent is wrapped on the perforated graphene sheets and embedded in the three-dimensional porous network structure.
The graphene aerogel has a three-dimensional porous network structure, is favorable for improving the loading capacity of the adsorbent, is hydrophilic at the same time, and can promote the transmission of moisture, so that the graphene aerogel fiber is adopted as a base material to be favorable for improving the moisture absorption capacity of the material. However, since the graphene sheets in the graphene aerogel are arranged in an anisotropic and regular manner, such a structure is not conducive to the transmission of water between graphene sheet layers, and further improvement of moisture absorption capacity is limited. In the invention, aerogel fibers made of perforated graphene are used as a base material, and the existence of 1-50 nm nano-pores on graphene sheets can promote the transmission of water or other media between graphene sheet layers, thereby being beneficial to further improving the moisture absorption capacity of the material.
In the present invention, the content of the perforated graphene aerogel fibers in the moisture-absorbing fibers is preferably selected as the matrix material of the moisture-absorbing fibersIs 30-60 wt.%. The perforated graphene aerogel fiber has an adjustable diameter and a large length-diameter ratio, the diameter is preferably 10 mu m-1 mm, and the length-diameter ratio is preferably 10-107The specific surface area is preferably 1 to 1200m2The preferred pore volume is 0.1-4.0 cm/g3/g。
In the invention, the porosity of the perforated graphene aerogel fiber is 1-99%. In some embodiments, the perforated graphene aerogel fiber has a continuous graphene three-dimensional porous network structure consisting of micropores with a pore diameter of 2nm or less, mesopores with a pore diameter of 2 to 50nm, and macropores with a pore diameter of 50nm to 500 μm. The perforated graphene aerogel fiber has excellent performances such as flexibility, weavability, moisture absorption, electric heating, photo-thermal energy storage and the like.
In the present invention, the moisture absorbent may be any one or more of moisture absorbent materials commonly used in the art, including but not limited to lithium chloride, calcium chloride, ferric chloride, cupric nitrate, nickel nitrate, ferric sulfate, lithium sulfate, sodium carbonate, sodium sulfate, cupric chloride, nickel acetate, magnesium sulfate, etc. In the perforated graphene aerogel moisture absorption fiber, the content of a moisture absorbent is adjustable and can be 1-99 wt.%, preferably 30-90 wt.%, and particularly preferably 50-70 wt.%.
Furthermore, the contact angle of the perforated graphene aerogel moisture absorption fiber is 20-90 degrees, and the perforated graphene aerogel moisture absorption fiber has good hydrophilic performance and is beneficial to adsorption and transmission of moisture.
The moisture absorption capacity of the perforated graphene aerogel moisture absorption fiber is adjustable and can be adjusted within 0.1-4.5 g/g.
The invention also provides a preparation method of the perforated graphene aerogel moisture absorption fiber, which comprises the following steps:
providing perforated graphene hydrogel fibers or perforated graphene aerogel fibers; and
and filling the perforated graphene hydrogel fiber or the perforated graphene aerogel fiber with a moisture absorbent in a solution filling mode, so that the moisture absorbent enters and is filled in a three-dimensional porous network structure of the gel fiber, and drying to obtain the perforated graphene aerogel moisture absorbent fiber.
According to the invention, the perforated graphene hydrogel fiber is prepared from a perforated graphene oxide dispersion liquid by a spinning method, and the perforated graphene aerogel fiber is obtained by drying the perforated graphene hydrogel fiber. Wherein the perforated graphene oxide is obtained by etching a graphene oxide sheet by a chemical etching method, and the adopted etchant comprises potassium hydroxide, nitric acid, hydrogen peroxide and SnO2、Na2MoO4、Na2WO4、NaAlO2、Na2SnO3、K2TiO3、KMnO4、Na3VO4、(NH4)6Mo7O24、H3PMo12O40Any one of them. In some embodiments, the preparation method of the perforated graphene oxide comprises: mixing the graphene oxide aqueous solution with a hydrogen peroxide aqueous solution, and etching at 90-100 ℃ for 0.5-5 h to obtain perforated graphene oxide; the concentration of the graphene oxide aqueous solution is preferably 1-10 mg/ml, and the etching temperature is preferably 95-100 ℃.
In the invention, the spinning method comprises any one of wet spinning, limited sol-gel reaction or freeze-dry spinning.
Further, the wet spinning specifically comprises: injecting the perforated graphene oxide liquid crystal into a coagulating bath through a needle, and collecting and reducing to obtain perforated graphene hydrogel fibers; the content of graphene oxide in the perforated graphene oxide liquid crystal is preferably 0.01-10 wt%; the inner diameter of the needle is 30 to 5mm, preferably 50 to 1500 μm, and more preferably 100 to 500 μm. The coagulating bath comprises any one or more of a calcium chloride solution, an aniline hydrochloride solution, dilute hydrochloric acid, dilute sulfuric acid, a mixed solution of sodium hydroxide and water and ethanol, a mixed solution of sodium hydroxide and tertiary butanol and a reducing agent solution; the reducing agent includes but is not limited to hydroiodic acid, ascorbic acid, sodium ascorbate, hydrazine hydrate, ethylenediamine, Fe-containing2+Any of the Compounds and dopamineMeans a combination of one or more.
Further, the limited-domain sol-gel reaction specifically comprises: placing the graphene oxide aqueous solution in a closed container, and reacting at 100-180 ℃ for 12-24 h to obtain the perforated graphene hydrogel fiber; wherein the concentration of the graphene oxide aqueous solution is 1-10 mg/mL.
Or, the limited-domain sol-gel reaction is specifically as follows: placing a mixed aqueous solution containing graphene oxide and a reducing agent in a closed container, and reacting at 30-95 ℃ for 1-12 h to obtain the perforated graphene hydrogel fiber; the mass ratio of the graphene oxide to the reducing agent is 1: 20-20: 1; the reducing agent includes, but is not limited to, hydroiodic acid, ascorbic acid, sodium ascorbate, dopamine, ethylenediamine, hydrazine hydrate, sodium borohydride, and Fe-containing2+Any one or combination of more of the compounds.
In the invention, the perforated graphene aerogel fiber is obtained by drying the perforated graphene aerogel fiber, wherein the drying is freeze drying or supercritical fluid drying.
In the invention, the solution filling specifically comprises the following steps: and (3) soaking the perforated graphene hydrogel fiber or the perforated graphene aerogel fiber in a moisture absorbent solution for 5 min-24 h, taking out and drying to obtain the perforated graphene aerogel moisture absorption fiber. Wherein the moisture absorbent content in the moisture absorbent solution is 1-70 wt.%; the drying mode comprises drying for 1-3 h at the normal pressure of 80-120 ℃ and vacuum freeze drying for 12-48 h.
Furthermore, the times of dipping and drying are 1-100 times.
The perforated graphene aerogel moisture absorption fiber material has excellent performances such as flexibility, weavability, moisture absorption, electric heating, photo-thermal energy storage and the like, so that the perforated graphene aerogel moisture absorption fiber material can be used for preparing devices for moisture absorption and heat preservation, air water taking, intelligent response, moisture absorption and heat storage, moisture absorption and refrigeration or flexible wearable devices.
In addition, the perforated graphene aerogel moisture absorption fiber can also be applied to the field of microwave absorption. Due to the fact that the graphene aerogel moisture absorption fibers are combined with water, the effective absorption bandwidth of the material can be remarkably improved due to the addition of the water while the impedance matching capacity of the material is adjusted, and the microwave absorption composite material with excellent performance is obtained. Meanwhile, the fiber has excellent flexibility as a one-dimensional material, long fiber can be used as a wave absorbing material for independent use, short fiber can be used as a wave absorbing agent filler for composite use, and flexible regulation and control of the wave absorbing performance can be easily realized due to the flexible moisture absorption and release characteristics of the fiber.
The present invention is further described below in conjunction with specific examples to enable those skilled in the art to better understand the present invention and to practice it, but the examples are not intended to limit the present invention.
Unless otherwise specified, the reagents according to the examples of the present invention are all commercially available products, and all of them are commercially available.
Example 1
The embodiment provides a perforated graphene aerogel moisture absorption fiber, and the preparation method comprises the following steps:
(1) preparing the perforated graphene oxide: adding aqueous hydrogen peroxide into the graphene oxide dispersion liquid, and reacting for 30min at 100 ℃.
(2) Preparing graphene aerogel fibers: and spinning the perforated graphene oxide liquid crystal into a calcium chloride aqueous solution through wet spinning to obtain the perforated graphene oxide hydrogel fiber, then soaking the perforated graphene oxide hydrogel fiber in a hydriodic acid aqueous solution, and then performing supercritical drying to obtain the perforated graphene aerogel fiber.
(3) Preparing the perforated graphene/moisture-absorbing material composite fiber: soaking the perforated graphene aerogel fiber in 7 wt.% of lithium chloride aqueous solution, standing for 10 hours at normal temperature and normal pressure, and freeze-drying the fiber containing the lithium chloride aqueous solution to obtain the perforated graphene/moisture absorption material composite fiber.
Example 2
The embodiment provides a perforated graphene aerogel moisture absorption fiber, and the preparation method comprises the following steps:
(1) preparing the perforated graphene oxide: adding aqueous hydrogen peroxide into the graphene oxide dispersion liquid, and reacting for 1h at 100 ℃.
(2) Preparing graphene aerogel fibers: and spinning the perforated graphene oxide liquid crystal into a hydrochloric acid/ascorbic acid mixed aqueous solution through wet spinning to obtain perforated graphene hydrogel fibers, and then performing supercritical drying on the hydrogel fibers to obtain the perforated graphene aerogel fibers.
(3) Preparing the perforated graphene/moisture-absorbing material composite fiber: soaking the perforated graphene aerogel fiber in 5 wt.% of lithium chloride aqueous solution, standing for 15h at normal temperature and normal pressure, and placing the fiber containing the lithium chloride aqueous solution in a drying oven at 100 ℃ to obtain the perforated graphene/moisture absorption material composite fiber.
Example 3
The embodiment provides a perforated graphene aerogel moisture absorption fiber, and the preparation method comprises the following steps:
(1) preparing the perforated graphene oxide: and adding aqueous hydrogen peroxide into the graphene oxide dispersion liquid, and reacting for 1.5h at 100 ℃.
(2) Preparing graphene aerogel fibers: and spinning the perforated graphene oxide liquid crystal into a hydrochloric acid/hydroiodic acid mixed aqueous solution through wet spinning to obtain perforated graphene hydrogel fibers, and then freeze-drying the perforated graphene hydrogel fibers to obtain the graphene aerogel fibers.
(3) Preparing the perforated graphene/moisture-absorbing material composite fiber: soaking the perforated graphene aerogel fiber in 3 wt.% of lithium chloride aqueous solution, standing for 20h at normal temperature and normal pressure, and placing the fiber containing the lithium chloride aqueous solution in a drying oven at 100 ℃ to obtain the perforated graphene/moisture absorption material composite fiber.
Example 4
The embodiment provides a perforated graphene aerogel moisture absorption fiber, and the preparation method comprises the following steps:
(1) preparing the perforated graphene oxide: adding aqueous hydrogen peroxide into the graphene oxide dispersion liquid, and reacting for 2h at 100 ℃.
(2) Preparing graphene aerogel fibers: and spinning the perforated graphene oxide liquid crystal into a hydrochloric acid/hydroiodic acid mixed aqueous solution through wet spinning to obtain perforated graphene hydrogel fibers, and then freeze-drying the perforated graphene hydrogel fibers to obtain the graphene aerogel fibers.
(3) Preparing the perforated graphene/moisture-absorbing material composite fiber: soaking the perforated graphene aerogel fiber in 7 wt.% of lithium chloride aqueous solution, standing for 10 hours at normal temperature and normal pressure, and freeze-drying the fiber containing the lithium chloride aqueous solution to obtain the perforated graphene/moisture absorption material composite fiber.
Example 5
The embodiment provides a perforated graphene aerogel moisture absorption fiber, and the preparation method comprises the following steps:
(1) preparing the perforated graphene oxide: and adding aqueous hydrogen peroxide into the graphene oxide dispersion liquid, and reacting for 2.5h at 100 ℃.
(2) Preparing graphene aerogel fibers: and spinning the perforated graphene oxide liquid crystal into an acetone/water mixed solution through wet spinning to obtain the perforated graphene oxide hydrogel fiber, then soaking the perforated graphene oxide hydrogel fiber in a hydriodic acid aqueous solution, and then performing supercritical drying to obtain the perforated graphene aerogel fiber.
(3) Preparing the perforated graphene/moisture-absorbing material composite fiber: soaking the perforated graphene aerogel fiber in 7 wt.% of lithium chloride aqueous solution, standing for 5 hours at normal temperature and normal pressure, and freeze-drying the fiber containing the lithium chloride aqueous solution to obtain the perforated graphene/moisture absorption material composite fiber.
Comparative example 1
The embodiment provides a graphene aerogel moisture absorption fiber, and a preparation method thereof comprises the following steps:
(1) preparing graphene aerogel fibers: and spinning the graphene oxide liquid crystal into an acetone/water mixed solution through wet spinning to obtain the perforated graphene oxide hydrogel fiber, then soaking the perforated graphene oxide hydrogel fiber in a hydriodic acid aqueous solution, and then performing supercritical drying to obtain the graphene aerogel fiber.
(2) Preparing the graphene/moisture-absorbing material composite fiber: soaking the graphene aerogel fibers in 7 wt.% of lithium chloride aqueous solution, standing for 5 hours at normal temperature and normal pressure, and freeze-drying the fibers containing the lithium chloride aqueous solution to obtain the graphene/moisture absorption material composite fibers.
Testing of fiber Properties
1. Scanning electron microscope tests are carried out on the perforated graphene aerogel moisture absorption fibers prepared in example 1, and the obtained results are shown in fig. 2. As can be seen from fig. 2, the moisture absorbent lithium chloride is uniformly coated on the surface of the graphene nanoplatelets.
2. The hydrophilicity and hydrophobicity of the perforated graphene aerogel hygroscopic fiber prepared in example 1 were measured, and the results are shown in fig. 3. As can be seen from fig. 3, the water contact angle of the perforated graphene aerogel moisture absorption fiber is 67.3 °, and the perforated graphene aerogel moisture absorption fiber has good hydrophilicity, so that the perforated graphene aerogel moisture absorption fiber is beneficial to capture water vapor.
3. The perforated graphene aerogel moisture absorption fibers prepared in examples 1 to 5 were subjected to moisture absorption tests, and the results are shown in the following table.
4. The moisture absorption performance test was performed on the moisture absorption fibers prepared in example 5 and comparative example 1, and the result is shown in fig. 4.
As can be seen from the figure, the moisture absorption amount of the absorbent fiber of comparative example 1 is significantly lower than that of the absorbent fiber of example 5 due to the use of the non-perforated graphene. The nano holes on the perforated graphene sheets can promote the transmission of water among graphene sheet layers, so that the moisture absorption performance of the moisture absorption fiber is improved.
Use of moisture-absorbing fibres
1. Air water taking
1) Testing the moisture absorption capacity in high, medium and low humidity environments: the perforated graphene aerogel moisture absorption fiber prepared in example 1 is placed in an oven at 100 ℃ for 5 hours to enable the fiber to be in a complete desorption state, 0.5g of the fiber is placed in a constant temperature and humidity cabinet for 6 hours, the change of the sample mass with time is recorded, the test is respectively carried out under a low humidity condition (30 RH%), a medium humidity condition (60 RH%) and a high humidity condition (90 RH%), the test temperature is 25 ℃, and the change curve of the adsorption amount with time is shown in figure 5.
As can be seen from fig. 5, the fibers have moisture absorptions of 0.57, 1.43 and 4.17g/g at 30%, 60% and 90% relative humidity, respectively, and have a fast kinetics, reaching an equilibrium state within 6 h.
2) And (3) carrying out desorption water release test after moisture absorption balance: the fiber is flatly laid under a sunlight simulator, and a photothermal water release test is carried out under standard sunlight irradiance, wherein the surface temperature of the fiber under the illumination condition is shown in figure 6; 10 fibers of 5cm are arranged in parallel, are connected with a direct current power supply in parallel, and are subjected to electric hot water release tests under the voltage of 5V, 6V, 7V, 10V and 12V respectively, wherein the surface temperature of the fibers under the electric heating condition is shown in figure 7.
As can be seen from fig. 6, the temperature of the fiber can be rapidly raised after the fiber is irradiated with solar light, and the temperature can be stabilized at about 50 ℃. As can be seen from fig. 7, a rapid temperature rise can also be achieved after applying a voltage to the fibers; wherein the temperature can be rapidly raised to more than 80 ℃ when a voltage of 10V is applied.
Fig. 8 is a graph of the circulation efficiency of the perforated graphene aerogel hygroscopic fiber under light and electric stimulation. As can be seen from the figure, the fiber still maintains high photo-thermal cycle efficiency after multiple times of light and electric stimulation.
2. Adsorption type heat storage and adsorption type refrigeration
The perforated graphene aerogel moisture absorption fiber prepared in example 1 is subjected to vacuum degassing at 100 ℃ for 6h to remove adsorbates adsorbed in the environment. Then, 100mg of the sample was taken and the adsorption isotherm of water vapor was measured at 30 ℃ and 40 ℃ respectively using a vapor adsorption apparatus, and adsorption heat data was obtained. The adsorption isotherm is shown in fig. 9, the change of the average adsorption enthalpy with the adsorption amount is shown in fig. 10, the change of the heat storage capacity with the adsorption amount is shown in fig. 11, and the adsorption refrigeration and adsorption heat storage efficiencies are shown in fig. 12.
As can be seen from fig. 9, the moisture absorption amount of the perforated graphene aerogel moisture absorption fiber is up to 9855ml/g at a relative vapor pressure of 95%. From FIG. 10, it can be seen that the heat storage capacity of the composite fiber increases with the increase in the amount of moisture absorption, and the maximum capacity is 9.77 KJ/g.
3. Microwave absorption
The water content is respectively 0, 1g-1、2g·g-1The perforated graphene aerogel moisture absorption fibers and the paraffin wax are blended according to the mass ratio of 3:7 to prepare a sample with the thickness of 2mm, the microwave absorption performance of the sample is tested on a vector analyzer by a coaxial method, and the obtained result is shown in fig. 13.
As can be seen from FIG. 13, at a loading of 2g/g, the effective absorption bandwidth of the absorbent fiber was 10.93GHz, and the maximum reflection loss reached-27.89 dB.
In conclusion, the perforated graphene aerogel moisture absorption fiber prepared by the invention has adjustable moisture absorption material loading capacity, water vapor adsorption rate and adsorption capacity, excellent flexibility, moisture absorption, energy storage, microwave absorption and other performances, can be applied to multiple fields of air water taking, moisture absorption heat storage/refrigeration and microwave absorption, and has wide application prospects.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. The perforated graphene aerogel moisture absorption fiber is characterized by comprising perforated graphene aerogel fibers and a moisture absorbent, wherein the perforated graphene aerogel fibers are made of fiber materials which are formed by overlapping perforated graphene sheets and have a three-dimensional porous network structure, and the moisture absorbent is wrapped on the perforated graphene sheets and is embedded and filled in the three-dimensional porous network structure.
2. The perforated graphene aerogel moisture absorption fiber according to claim 1, wherein the perforated graphene aerogel moisture absorption fiber contains perforated graphene aerogel fibers in an amount of 10 wt.% to 70 wt.%, and the porosity of the three-dimensional porous network structure is 1 to 99%;
the diameter of the perforated graphene aerogel fiber is 10 mu m-1 mm, and the length-diameter ratio is 10-107The specific surface area is 1 to 1200m2The pore volume is 0.1-16 cm3/g。
3. The perforated graphene aerogel moisture absorption fiber according to claim 1, wherein the perforated graphene sheet layer has nanometer-scale holes, and the size of the nanometer-scale holes is 1-50 nm.
4. The perforated graphene aerogel moisture absorption fiber according to claim 1, wherein the moisture absorption agent is contained in the perforated graphene aerogel moisture absorption fiber in an amount of 1 to 99 wt.%;
the moisture absorbent comprises any one or combination of more of lithium chloride, calcium chloride, ferric chloride, copper nitrate, nickel nitrate, ferric sulfate, lithium sulfate, sodium carbonate, sodium sulfate, copper chloride, nickel acetate and magnesium sulfate.
5. The perforated graphene aerogel moisture absorption fiber according to claim 1, wherein the water vapor adsorption capacity of the perforated graphene aerogel moisture absorption fiber is 0.1-4.5 g/g.
6. The preparation method of the perforated graphene aerogel moisture absorption fiber according to any one of claims 1 to 5, which is characterized by comprising the following steps:
providing perforated graphene hydrogel fibers or perforated graphene aerogel fibers; and
and filling the perforated graphene hydrogel fiber or the perforated graphene aerogel fiber with a moisture absorbent in a solution filling mode, so that the moisture absorbent enters and is filled in a three-dimensional porous network structure of the gel fiber, and drying to obtain the perforated graphene aerogel moisture absorbent fiber.
7. The method for preparing the perforated graphene aerogel moisture absorption fiber according to claim 6, wherein the perforated graphene aerogel fiber is prepared from a perforated graphene oxide dispersion liquid by a spinning method, and the perforated graphene aerogel fiber is obtained by drying the perforated graphene aerogel fiber;
the perforated graphene oxide is obtained by etching graphene oxide by a chemical etching method, and the adopted etching agent comprises potassium hydroxide, nitric acid, hydrogen peroxide and SnO2、Na2MoO4、Na2WO4、NaAlO2、Na2SnO3、K2TiO3、KMnO4、Na3VO4、(NH4)6Mo7O24、H3PMo12O40Any one of the above;
the spinning method comprises any one of wet spinning, limited sol-gel reaction or freeze dry spinning; the drying treatment is freeze drying or supercritical fluid drying.
8. The method for preparing the perforated graphene aerogel moisture absorption fiber according to claim 7, wherein the step of etching the graphene oxide by a chemical etching method specifically comprises the following steps: mixing the graphene oxide aqueous solution with a hydrogen peroxide aqueous solution, and etching at 90-100 ℃ for 0.5-5 h to obtain perforated graphene oxide; the concentration of the graphene oxide aqueous solution is 1-10 mg/ml;
the wet spinning method comprises the following specific steps: injecting the perforated graphene oxide liquid crystal into a coagulating bath through a needle, and collecting and reducing to obtain perforated graphene hydrogel fibers; wherein the content of graphene oxide in the perforated graphene oxide liquid crystal is 0.01-10 wt%; the inner diameter of the needle head is 30 mu m-5 mm; the coagulating bath comprises any one or more of a calcium chloride solution, an aniline hydrochloride solution, dilute hydrochloric acid, dilute sulfuric acid, a mixed solution of sodium hydroxide and water and ethanol, a mixed solution of sodium hydroxide and tert-butyl alcohol and a reducing agent solution; the reducing agent comprises hydriodic acid, ascorbic acid, sodium ascorbate, hydrazine hydrate, ethylenediamine and Fe-containing2+A combination of any one or more of the compounds and dopamine;
the limited-area sol-gel reaction specifically comprises the following steps:
placing the graphene oxide aqueous solution in a closed container, and reacting at 100-180 ℃ for 12-24 h to obtain the perforated graphene hydrogel fiber; wherein the concentration of the graphene oxide aqueous solution is 1-10 mg/mL;
or placing the mixed aqueous solution containing the graphene oxide and the reducing agent in a closed container, and reacting at the temperature of 30-95 ℃ for 1-12 hours to obtain the perforated graphene hydrogel fiber; the mass ratio of the graphene oxide to the reducing agent is 1: 20-20: 1; the reducing agent comprises hydriodic acid, ascorbic acid, sodium ascorbate, dopamine, ethylenediamine, hydrazine hydrate, sodium borohydride and Fe2+Any one or combination of more of the compounds.
9. The method for preparing the perforated graphene aerogel moisture absorption fiber according to claim 6, wherein the solution filling specifically comprises: soaking the perforated graphene hydrogel fiber or the perforated graphene aerogel fiber in a moisture absorbent solution for 1-24 h, taking out and drying to obtain the perforated graphene aerogel moisture absorption fiber; wherein the moisture absorbent content in the moisture absorbent solution is 1-70 wt.%; the drying mode comprises drying at the normal pressure of 80-120 ℃ and vacuum freeze drying.
10. Use of the perforated graphene aerogel moisture absorption fiber according to any one of claims 1 to 5 in preparation of devices for moisture absorption and warm keeping, air water taking, smart response, moisture absorption and heat storage, moisture absorption and refrigeration, microwave absorption or flexible wearable devices.
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