CN112426980B - Magnetic response two-dimensional material aerogel microsphere and preparation method thereof - Google Patents
Magnetic response two-dimensional material aerogel microsphere and preparation method thereof Download PDFInfo
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- 239000004005 microsphere Substances 0.000 title claims abstract description 137
- 239000004964 aerogel Substances 0.000 title claims abstract description 94
- 239000000463 material Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 230000004044 response Effects 0.000 title abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 71
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000008367 deionised water Substances 0.000 claims abstract description 30
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 30
- 239000012266 salt solution Substances 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000007590 electrostatic spraying Methods 0.000 claims abstract description 15
- 238000004108 freeze drying Methods 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 239000000654 additive Substances 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 238000007710 freezing Methods 0.000 claims abstract description 14
- 230000008014 freezing Effects 0.000 claims abstract description 14
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- 150000003839 salts Chemical class 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 6
- 230000009467 reduction Effects 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 27
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- 229910021389 graphene Inorganic materials 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 23
- 229910052582 BN Inorganic materials 0.000 claims description 16
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 16
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 7
- -1 GaTe Inorganic materials 0.000 claims description 4
- XNZJTLSFOOXUAS-UHFFFAOYSA-N cobalt hydrochloride Chemical compound Cl.[Co] XNZJTLSFOOXUAS-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000000017 hydrogel Substances 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 4
- 239000003208 petroleum Substances 0.000 claims description 4
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 4
- 229920002401 polyacrylamide Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 4
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 3
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- 229940011182 cobalt acetate Drugs 0.000 claims description 3
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 3
- XATZQMXOIQGKKV-UHFFFAOYSA-N nickel;hydrochloride Chemical compound Cl.[Ni] XATZQMXOIQGKKV-UHFFFAOYSA-N 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 239000000661 sodium alginate Substances 0.000 claims description 3
- 235000010413 sodium alginate Nutrition 0.000 claims description 3
- 229940005550 sodium alginate Drugs 0.000 claims description 3
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 3
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- 235000019698 starch Nutrition 0.000 claims description 3
- 229920002101 Chitin Polymers 0.000 claims description 2
- 229910005543 GaSe Inorganic materials 0.000 claims description 2
- 229910005829 GeS Inorganic materials 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 2
- 229940044175 cobalt sulfate Drugs 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- 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 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- 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 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 229910016001 MoSe Inorganic materials 0.000 claims 1
- 229920002301 cellulose acetate Polymers 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 238000011068 loading method Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000012071 phase Substances 0.000 abstract 3
- 239000008346 aqueous phase Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 239000010941 cobalt Substances 0.000 description 5
- 229910017052 cobalt Inorganic materials 0.000 description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 229910004211 TaS2 Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910002899 Bi2Te3 Inorganic materials 0.000 description 1
- 239000004966 Carbon aerogel Substances 0.000 description 1
- 229910005318 FePS3 Inorganic materials 0.000 description 1
- 229910020073 MgB2 Inorganic materials 0.000 description 1
- 229910016021 MoTe2 Inorganic materials 0.000 description 1
- 229910019742 NbB2 Inorganic materials 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 229910017629 Sb2Te3 Inorganic materials 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 229910004533 TaB2 Inorganic materials 0.000 description 1
- 229910004214 TaSe2 Inorganic materials 0.000 description 1
- 229910003092 TiS2 Inorganic materials 0.000 description 1
- 229910003090 WSe2 Inorganic materials 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
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- 238000006243 chemical reaction Methods 0.000 description 1
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- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
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- 239000002612 dispersion medium Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-N iron;hydrochloride Chemical compound Cl.[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Images
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention provides a magnetic response two-dimensional material aerogel microsphere and a preparation method thereof, wherein deionized water, a two-dimensional material and a polymer additive are prepared into a water phase; dissolving a salt of a magnetic element into a salt solution; mixing an organic solvent and a salt solution to obtain a two-phase receiving bath; loading the injector filled with the aqueous phase dispersion liquid on an electrostatic spraying device, and installing a clip needle; placing the two-phase receiving bath under a needle head, and adding a stirrer for stirring; filtering and washing the obtained mixture to obtain two-dimensional material microspheres; and (3) quickly freezing the liquid nitrogen to obtain the two-dimensional material ice microspheres, and freeze-drying the two-dimensional material ice microspheres to obtain the two-dimensional material aerogel microspheres. And reducing the two-dimensional material aerogel microspheres by using a high-temperature thermal reduction method to obtain the magnetic response two-dimensional material aerogel microspheres. The preparation method provided by the invention is simple to operate, high in production efficiency and safe and reliable in production process.
Description
Technical Field
The invention belongs to the field of functional materials, and particularly relates to a magnetic response two-dimensional material aerogel microsphere and a preparation method thereof.
Background
Two-dimensional materials are confined to two-dimensional planes due to their carrier transport and thermal diffusion, making such materials exhibit many unique properties. The adjustable band gap characteristic of the band gap is widely applied in the fields of field effect tubes, photoelectric devices, thermoelectric devices and the like; the controllability of the spin degree of freedom and the valley degree of freedom thereof has led to intensive research in the fields of spintronics and valley electronics; due to the special properties of the crystal structure, different two-dimensional materials have anisotropy of different electrical properties or optical properties, including anisotropy of properties such as Raman spectrum, photoluminescence spectrum, second-order harmonic spectrum, light absorption spectrum, thermal conductivity and electric conductivity, and have great development potential in the fields of polarized photoelectric devices, polarized thermoelectric devices, bionic devices, polarized light detection and the like.
Aerogel, generally referred to as a highly dispersed solid material in which colloidal particles or high polymer molecules are agglomerated with each other to form a nanoporous network structure and the pores are filled with a gaseous dispersion medium, has a very low density. Currently, the common aerogels are all in block shapes. The block aerogel is prepared into microspheres with the diameter of 10-1000 microns, namely the aerogel microspheres. Aerogel microspheres refer to microspheres in an aerogel form, and are not microspheres containing aerogel; aerogel is a description of porous morphology.
The aerogel is made into microspheres, so that the application potential of the aerogel is greatly expanded, for example, various existing carbon aerogel microspheres and SiO2Aerogel microspheres, TiO2/SiO2The composite aerogel microspheres and the two-dimensional material aerogel microspheres with the center divergent structure and the like show more excellent properties than the massive aerogel, and particularly in the application of the environment, the aerogel microspheres have better oil-water separation capacity and adsorption performance than the massive aerogel. However, the traditional two-dimensional material aerogel microspheres only have excellent adsorption capacity and lack the separation capacity from the environment after adsorption in an oil-water coexisting environment, so the practical value is greatly reduced, the magnetic response capacity of the two-dimensional material aerogel microspheres can be greatly improved, and the practical application potential of the two-dimensional material in the fields of environment, energy catalysis and the like, particularly in oil-water separation can be greatly improved, and therefore, the preparation research on the micron-sized two-dimensional material aerogel microspheres with the magnetic response characteristic has extremely important value. Due to the structural characteristics (the porosity is over 90%) and the physical properties (light weight) of the aerogel, regular two-dimensional material aerogel microspheres cannot be obtained by conventional mechanical methods such as ball milling and dispersion; on the other hand, in the production process of the two-dimensional material aerogel microspheres reported previously, a large amount of organic reagents such as ethyl acetate, n-hexane and the like are required, and a large amount of liquid nitrogen is also required, so that the environmental pollution is caused, and the energy is extremely consumed. Therefore, a preparation method of a novel two-dimensional material aerogel microsphere with industrial application prospect and magnetic response is in urgent need to be established.
Disclosure of Invention
The objects of the present invention include:
providing a magnetic two-dimensional material aerogel microsphere;
the aerogel microspheres prepared by the method are regular in shape and adjustable in size, have the capability of interacting with a magnet, have a porous network structure, and are light in weight and small in density.
The specific technical scheme is as follows:
the preparation method of the two-dimensional material aerogel microspheres comprises the following steps:
(1) preparing or preparing a bulk two-dimensional material;
(2) uniformly mixing deionized water, a bulk two-dimensional material and a polymer additive, and then performing ultrasonic irradiation for 15-360min to prepare a water phase, wherein the bulk two-dimensional material is peeled into a two-dimensional material in the ultrasonic process and is uniformly mixed with the polymer additive;
(3) dissolving salt of a magnetic element in deionized water to prepare a salt solution required by a receiving bath;
(4) mixing an organic solvent and the salt solution prepared in the step (3) to prepare a two-phase receiving bath;
(5) loading the injector filled with the dispersion liquid obtained in the step (2) on electrostatic spraying equipment, and installing a clip needle head, wherein the applied voltage is 5-20 kV;
(6) placing the two-phase receiving bath obtained in the step (4) under a needle head, and adding a stirrer for stirring, wherein the stirring speed is 200 and 1200rpm, and the length of the stirrer is 30-50 mm;
(7) filtering and washing the mixture obtained in the step (6) to obtain two-dimensional material microspheres; quickly freezing liquid nitrogen to obtain two-dimensional material ice microspheres, and freeze-drying the two-dimensional material ice microspheres to obtain two-dimensional material aerogel microspheres;
(8) and reducing the two-dimensional material aerogel microspheres by using a high-temperature thermal reduction method to obtain the magnetic response two-dimensional material aerogel microspheres.
The two-dimensional material is Bi2Se3、Bi2Te3Black phosphorus, boron nitride, CaPS3、CoPS3、FePS3FeSe, GaS, GaSe, GaTe, GeS, graphite, graphene oxide, InSe, MgB2、MnPS3、MoS2、MoSe2、MoTe2、NbB2、PdTe2、PtTe、ReS2、ReSe2、Sb2Te3、SnS2、SnSe、TaS2、TaB2、TaS2、TaS3、TaS3、TaSe2、TiS2、Tl2S、VB2、WS2、WSe2、ZnPS3、Ti2C3And TiC.
Wherein, the polymer additive in the step (2) is selected from one or more of polyacrylamide, polyvinylpyrrolidone, sodium alginate, sodium carboxymethylcellulose, polyoxyethylene, sodium polyacrylate, polyvinyl alcohol, starch, chitin and sodium acetate cellulose.
In the step (2), deionized water, a bulk phase two-dimensional material and a polymer additive are mixed according to the following mass parts: 90-150 parts of: 0.05-2 parts of: 0.05-2 parts of a stabilizer;
in the step (3), the salt of the magnetic element and the deionized water are mixed according to the mass part: 5-40 parts of: 60-95 parts.
The salt of the magnetic element in the step (3) is one or a combination of more of cobalt acetate, nickel acetate, iron acetate, cobalt hydrochloride, nickel hydrochloride, iron hydrochloride, cobalt nitrate, nickel nitrate, iron nitrate, cobalt sulfate, nickel sulfate and iron sulfate.
The organic solvent in the step (4) is any one or more of n-heptane, petroleum ether, toluene, n-hexane and n-octane.
The diameter of the needle head in the step (6) is 0.3-0.6 mm.
Specifically, the high-temperature thermal reduction method comprises the following steps: and (3) placing the two-dimensional material aerogel microspheres in a tubular furnace, heating to 800 ℃ at a heating rate of 5-10 ℃/min under the Ar atmosphere, and preserving heat for 2-5 h.
The magnetic response two-dimensional material aerogel microspheres obtained by the invention are microspheres which are prepared from two-dimensional materials serving as main components, high polymer materials and iron, cobalt and nickel elements serving as additives and have porous shapes like aerogel; or, the magnetic response two-dimensional material aerogel microspheres of the invention are microspheres which are composed of two-dimensional materials, high molecular materials, iron, cobalt and nickel elements and have a porous appearance like aerogel.
In the preparation method, the initial feeding mass ratio is 0.05-2 parts of two-dimensional material, 0.05-2 parts of polymer additive and 90-150 parts of deionized water, the microspheres are formed by an electrostatic spraying method, an organic solvent and a specific salt solution (containing iron, cobalt and nickel) are used as two-phase receiving baths, the redundant salt solution on the surface can be removed by filtering and washing after the microspheres are formed, and only the two-dimensional material hydrogel microspheres consisting of the two-dimensional material, the polymer additive and the elements of iron, cobalt and nickel are left. The aerogel is endowed with a general porous structure through liquid nitrogen quick freezing and freeze drying, and the two-dimensional material is reduced to obtain the two-dimensional material aerogel microsphere with magnetic response, which consists of the two-dimensional material, a high molecular additive, iron, cobalt and nickel elements. The mass ratio of the two-dimensional material to the polymer additive can be measured by a thermal weight loss method, and the final polymer mass accounts for 0-30%, while the two-dimensional material mass accounts for 70-100%.
The invention has the following advantages:
1. the invention combines the electrostatic spraying method, the sol-gel conversion method and the freeze-drying method for the first time to prepare the magnetic response two-dimensional material aerogel microspheres.
2. The preparation method provided by the invention is simple to operate, high in production efficiency and safe and reliable in production process.
3. The magnetic response two-dimensional material aerogel obtained by the preparation method provided by the invention is regular in microspherical shape, uniform in size, high in specific surface area and porous in network structure.
4. The magnetic response two-dimensional material aerogel microspheres prepared by the preparation method can be in non-contact interaction with a magnet.
Drawings
FIG. 1 is a process diagram of example 1 for preparing magnetic-response two-dimensional material aerogel microspheres;
FIG. 2 is a scanning electron microscope image of a magnetically responsive two-dimensional material aerogel microsphere prepared in example 1;
FIG. 3 is a scanning electron microscope image of the surface of a two-dimensional material aerogel microsphere with magnetic response prepared in example 1.
Detailed Description
The present invention is described in detail below by way of examples, it should be noted that the present examples are only illustrative of the present invention, and should not be construed as limiting the scope of the present invention.
Example 1
The preparation method of the magnetic response two-dimensional material aerogel microspheres comprises the following steps:
(1) preparing natural crystalline flake graphite into graphene oxide by a chemical oxidation method;
and (3) uniformly mixing 10g of natural crystalline flake graphite, 6g of potassium permanganate and 300ml of concentrated sulfuric acid, then carrying out oxidation reaction at high temperature, centrifuging, washing and dialyzing the obtained product to obtain a bulk phase two-dimensional material, and drying for later use.
(2) Uniformly mixing 100 parts of deionized water, 0.9 part of graphene oxide and 0.05 part of polyvinyl alcohol, and performing 1600W ultrasonic irradiation for 15min to prepare a water phase;
(3) 5 parts of ferric nitrate is dissolved in 65 parts of deionized water to prepare a salt solution required by a receiving bath;
(4) and (4) mixing toluene and the salt solution prepared in the step (3) to prepare a two-phase receiving bath.
(5) And (3) loading the syringe filled with the dispersion liquid obtained in the step (2) on an electrostatic spraying device, and installing a clip needle, wherein the applied voltage is 5 kV.
(6) Placing the two-phase receiving bath obtained in the step (4) under a needle head, and adding a stirrer for stirring, wherein the stirring speed is 300rpm, and the length of the stirrer is 30mm, as shown in figure 1;
(7) filtering and washing the mixture obtained in the step (6) to obtain graphene oxide microspheres; rapidly freezing with liquid nitrogen to obtain graphene oxide ice microspheres, and freeze-drying (vacuum degree 20Pa, temperature-50 ℃) to obtain graphene oxide aerogel microspheres, as shown in FIG. 2.
(8) And (3) placing the graphene oxide aerogel microspheres in a tubular furnace, heating to 800 ℃ at a heating rate of 6 ℃/min under the atmosphere of Ar, and preserving heat for 3 h.
Observing the magnetic response two-dimensional material aerogel microspheres prepared in the example 1 by using a scanning electron microscope to obtain a morphology map of the microspheres; the results show that: the prepared magnetic response two-dimensional material aerogel microspheres are uniform in size and regular in shape, and have abundant network structures and pore structures. Scanning Electron microscopy asAs shown in fig. 3. The average grain diameter of the two-dimensional material aerogel microspheres is determined to be 247 mu m, and the density is determined to be 5.0kg/m3。
Example 2
The preparation method of the magnetic response two-dimensional material aerogel microspheres comprises the following steps:
(1) uniformly mixing 120 parts of deionized water, 1.2 parts of black phosphorus and 0.1 part of polyvinylpyrrolidone, and performing 600W ultrasonic irradiation for 20min to prepare a water phase;
(2) 10 parts of nickel sulfate is dissolved in 85 parts of deionized water to prepare a salt solution required by a receiving bath;
(3) mixing n-heptane and the salt solution prepared in step (2) to prepare a two-phase receiving bath.
(4) And (2) loading the syringe filled with the dispersion liquid obtained in the step (1) on an electrostatic spraying device, and installing a clip needle, wherein the applied voltage is 12 kV.
(5) Placing the two-phase receiving bath obtained in the step (3) under a needle head, and adding a stirrer for stirring, wherein the stirring speed is 450rpm, and the length of the stirrer is 35 mm;
(6) filtering and washing the mixture obtained in the step (5) to obtain black phosphorus microspheres; and (3) quickly freezing the liquid nitrogen to obtain the black phosphorus ice microspheres, and freeze-drying (the vacuum degree is 20Pa, and the temperature is-50 ℃) the black phosphorus ice microspheres to obtain the black phosphorus aerogel microspheres. The average grain diameter of the black phosphorus microspheres is 450 mu m, and the density is 6.8kg/m3。
(7) Placing the black phosphorus aerogel microspheres in a tubular furnace, heating to 800 ℃ at a heating rate of 7 ℃/min under the Ar atmosphere, and keeping the temperature for 4 h.
Example 3
The preparation method of the magnetic response two-dimensional material aerogel microspheres comprises the following steps:
(1) uniformly mixing 110 parts of deionized water, 0.8 part of boron nitride and 0.8 part of polyvinylpyrrolidone, and performing 800W ultrasonic irradiation for 25min to prepare a water phase;
(2) dissolving 20 parts of cobalt hydrochloride in 70 parts of deionized water to prepare a salt solution required by a receiving bath;
(3) and (3) mixing n-octane and the salt solution prepared in the step (2) to prepare a two-phase receiving bath.
(4) And (2) loading the syringe filled with the dispersion liquid obtained in the step (1) on an electrostatic spraying device, and installing a clip needle, wherein the applied voltage is 15 kV.
(5) Placing the two-phase receiving bath obtained in the step (3) under a needle head, and adding a stirrer for stirring, wherein the stirring speed is 650rpm, and the length of the stirrer is 40 mm;
(6) filtering and washing the mixture obtained in the step (5) to obtain boron nitride microspheres; and (3) quickly freezing the liquid nitrogen to obtain boron nitride ice microspheres, and freeze-drying (the vacuum degree is 20Pa, and the temperature is-50 ℃) the boron nitride ice microspheres to obtain the boron nitride aerogel microspheres. The average particle diameter of the boron nitride microspheres is 550 mu m, and the density is 7.2kg/m3。
(7) Placing the boron nitride aerogel microspheres in a tube furnace, heating to 800 ℃ at a heating rate of 8 ℃/min under the atmosphere of Ar, and preserving heat for 5 h.
Example 4
The preparation method of the magnetic response two-dimensional material aerogel microspheres comprises the following steps:
(1) uniformly mixing 105 parts of deionized water, 0.9 part of graphene oxide and 0.8 part of polyacrylamide, and performing ultrasonic irradiation at 500W for 35min to prepare a water phase;
(2) dissolving 25 parts of nickel hydrochloride in 75 parts of deionized water to prepare a salt solution required by a receiving bath;
(3) and (3) mixing normal hexane and the salt solution prepared in the step (2) to prepare a two-phase receiving bath.
(4) And (2) loading the syringe filled with the dispersion liquid obtained in the step (1) on an electrostatic spraying device, and installing a clip needle, wherein the applied voltage is 10 kV.
(5) Placing the two-phase receiving bath obtained in the step (3) under a needle head, and adding a stirrer for stirring, wherein the stirring speed is 750rpm, and the length of the stirrer is 45 mm;
(6) filtering and washing the mixture obtained in the step (5) to obtain graphene oxide microspheres; and (3) quickly freezing liquid nitrogen to obtain graphene oxide ice microspheres, and freeze-drying (vacuum degree of 20Pa, temperature of-50 ℃) the graphene oxide ice microspheres to obtain the graphene oxide aerogel microspheres. The average grain diameter of the graphene oxide microspheres is 500 mu m, and the density is 8kg/m3。
(7) And (3) placing the graphene oxide aerogel microspheres in a tubular furnace, heating to 800 ℃ at a heating rate of 9 ℃/min under the atmosphere of Ar, and preserving heat for 4 h.
Example 5
The preparation method of the magnetic response two-dimensional material aerogel microspheres comprises the following steps:
(1) uniformly mixing 130 parts of deionized water, 1.4 parts of black phosphorus and 2 parts of sodium polyacrylate, and performing 400W ultrasonic irradiation for 30min to prepare a water phase;
(2) dissolving 40 parts of cobalt hydrochloride in 60 parts of deionized water to prepare a salt solution required by a receiving bath;
(3) and (3) mixing toluene and the salt solution prepared in the step (2) to prepare a two-phase receiving bath.
(4) And (2) loading the syringe filled with the dispersion liquid obtained in the step (1) on an electrostatic spraying device, and installing a clip needle, wherein the applied voltage is 12 kV.
(5) Placing the two-phase receiving bath obtained in the step (3) under a needle head, and adding a stirrer for stirring, wherein the stirring speed is 550rpm, and the length of the stirrer is 45 mm;
(6) filtering and washing the mixture obtained in the step (5) to obtain black phosphorus microspheres; and (3) quickly freezing the liquid nitrogen to obtain the black phosphorus ice microspheres, and freeze-drying (the vacuum degree is 20Pa, and the temperature is-50 ℃) the black phosphorus ice microspheres to obtain the black phosphorus aerogel microspheres. The average grain diameter of the black phosphorus microspheres is 650 mu m, and the density is 8.6kg/m3。
(7) Placing the black phosphorus aerogel microspheres in a tubular furnace, heating to 800 ℃ at a heating rate of 6 ℃/min under the Ar atmosphere, and keeping the temperature for 3 h.
Example 6
The preparation method of the magnetic response two-dimensional material aerogel microspheres comprises the following steps:
(1) uniformly mixing 135 parts of deionized water, 1.5 parts of boron nitride and 1.2 parts of sodium carboxymethylcellulose, and performing 600W ultrasonic irradiation for 55min to prepare a water phase;
(2) dissolving 20 parts of ferric hydrochloride in 80 parts of deionized water to prepare a salt solution required by a receiving bath;
(3) and (3) mixing normal hexane and the salt solution prepared in the step (2) to prepare a two-phase receiving bath.
(4) The syringe containing the dispersion obtained in step (1) was loaded on an electrostatic spraying apparatus, and a hollow needle was attached thereto with an applied voltage of 14 kV.
(5) Placing the two-phase receiving bath obtained in the step (3) under a needle head, and adding a stirrer for stirring, wherein the stirring speed is 850rpm, and the length of the stirrer is 50 mm;
(6) filtering and washing the mixture obtained in the step (5) to obtain boron nitride microspheres; and (3) quickly freezing the liquid nitrogen to obtain boron nitride ice microspheres, and freeze-drying (the vacuum degree is 20Pa, and the temperature is-50 ℃) the boron nitride ice microspheres to obtain the boron nitride aerogel microspheres. The average grain diameter of the boron nitride microspheres is measured to be 350 mu m, and the density is measured to be 6.6kg/m3。
(7) Placing the boron nitride aerogel microspheres in a tube furnace, heating to 800 ℃ at a heating rate of 8 ℃/min under the atmosphere of Ar, and preserving heat for 4 h.
Example 7
The preparation method of the magnetic response two-dimensional material aerogel microspheres comprises the following steps:
(1) uniformly mixing 140 parts of deionized water, 1.3 parts of TiC and 1.5 parts of sodium polyacrylate, and performing 550W ultrasonic irradiation for 45min to prepare a water phase;
(2) dissolving 25 parts of ferric sulfate in 75 parts of deionized water to prepare a salt solution required by a receiving bath;
(3) mixing petroleum ether and the salt solution prepared in the step (2) to prepare a two-phase receiving bath.
(4) And (2) loading the syringe filled with the dispersion liquid obtained in the step (1) on an electrostatic spraying device, and installing a clip needle, wherein the applied voltage is 17 kV.
(5) Placing the two-phase receiving bath obtained in the step (3) under a needle head, and adding a stirrer for stirring, wherein the stirring speed is 950rpm, and the length of the stirrer is 40 mm;
(6) filtering and washing the mixture obtained in the step (5) to obtain TiC microspheres; rapidly freezing the liquid nitrogen to obtain TiC ice microspheres, and freeze-drying (the vacuum degree is 20Pa, and the temperature is-50 ℃) the TiC ice microspheres to obtain the TiC aerogel microspheres. The average grain diameter of the TiC microspheres is measured to be 450 mu m, and the density is measured to be 6.2kg/m3。
(7) Placing the TiC aerogel microspheres in a tube furnace, heating to 800 ℃ at a heating rate of 7 ℃/min under the atmosphere of Ar, and preserving heat for 3 h.
Example 8
The preparation method of the magnetic response two-dimensional material aerogel microspheres comprises the following steps:
(1) uniformly mixing 125 parts of deionized water, 0.7 part of graphene oxide and 1.5 parts of polyacrylamide, and performing 650W ultrasonic irradiation for 55min to prepare a water phase;
(2) dissolving 15 parts of nickel sulfate in 85 parts of deionized water to prepare a salt solution required by a receiving bath;
(3) and (3) mixing n-octane and the salt solution prepared in the step (2) to prepare a two-phase receiving bath.
(4) And (2) loading the syringe filled with the dispersion liquid obtained in the step (1) on an electrostatic spraying device, and installing a clip needle, wherein the applied voltage is 17 kV.
(5) Placing the two-phase receiving bath obtained in the step (3) under a needle head, and adding a stirrer for stirring, wherein the stirring speed is 850rpm, and the length of the stirrer is 45 mm;
(6) filtering and washing the mixture obtained in the step (5) to obtain graphene oxide microspheres; and (3) quickly freezing liquid nitrogen to obtain graphene oxide ice microspheres, and freeze-drying (vacuum degree of 20Pa, temperature of-50 ℃) the graphene oxide ice microspheres to obtain the graphene oxide aerogel microspheres. The average grain diameter of the graphene oxide microspheres is 650 mu m, and the density is 9.2kg/m3。
(7) And (3) placing the graphene oxide aerogel microspheres in a tubular furnace, heating to 800 ℃ at a heating rate of 6 ℃/min under the atmosphere of Ar, and preserving heat for 4 h.
Example 9
The preparation method of the magnetic response two-dimensional material aerogel microspheres comprises the following steps:
(1) uniformly mixing 115 parts of deionized water, 0.9 part of black phosphorus and 1 part of starch, and performing 700W ultrasonic irradiation for 45min to prepare a water phase;
(2) dissolving 20 parts of cobalt acetate in 80 parts of deionized water to prepare a salt solution required by a receiving bath;
(3) mixing petroleum ether and the salt solution prepared in the step (2) to prepare a two-phase receiving bath.
(4) And (2) loading the syringe filled with the dispersion liquid obtained in the step (1) on an electrostatic spraying device, and installing a clip needle, wherein the applied voltage is 17 kV.
(5) Placing the two-phase receiving bath obtained in the step (3) under a needle head, and adding a stirrer for stirring, wherein the stirring speed is 800rpm, and the length of the stirrer is 35 mm;
(6) filtering and washing the mixture obtained in the step (5) to obtain black phosphorus microspheres; and (3) quickly freezing the liquid nitrogen to obtain the black phosphorus ice microspheres, and freeze-drying (the vacuum degree is 20Pa, and the temperature is-50 ℃) the black phosphorus ice microspheres to obtain the black phosphorus aerogel microspheres. The average grain diameter of the black phosphorus microspheres is 550 mu m, and the density is 8.4kg/m3。
(7) Placing the black phosphorus aerogel microspheres in a tubular furnace, heating to 800 ℃ at a heating rate of 7 ℃/min under the Ar atmosphere, and keeping the temperature for 3 h.
Example 10
The preparation method of the magnetic response two-dimensional material aerogel microspheres comprises the following steps:
(1) uniformly mixing 120 parts of deionized water, 1 part of TiC and 1 part of sodium alginate, and performing 750W ultrasonic irradiation for 25min to prepare a water phase;
(2) dissolving 30 parts of ferric acetate in 70 parts of deionized water to prepare a salt solution required by a receiving bath;
(3) mixing n-heptane and the salt solution prepared in step (2) to prepare a two-phase receiving bath.
(4) And (2) loading the syringe filled with the dispersion liquid obtained in the step (1) on an electrostatic spraying device, and installing a clip needle, wherein the applied voltage is 17 kV.
(5) Placing the two-phase receiving bath obtained in the step (3) under a needle head, and adding a stirrer for stirring, wherein the stirring speed is 700rpm, and the length of the stirrer is 30 mm;
(6) filtering and washing the mixture obtained in the step (5) to obtain TiC microspheres; rapidly freezing the liquid nitrogen to obtain TiC ice microspheres, and freeze-drying (the vacuum degree is 20Pa, and the temperature is-50 ℃) the TiC ice microspheres to obtain the TiC aerogel microspheres. The average grain diameter of the TiC microspheres is measured to be 450 mu m, and the density is measured to be 6.8kg/m3。
(7) Placing the TiC aerogel microspheres in a tube furnace, heating to 800 ℃ at a heating rate of 7 ℃/min under the atmosphere of Ar, and preserving heat for 3 h.
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