CN110060830B - Preparation method of magnetic nano functional material - Google Patents
Preparation method of magnetic nano functional material Download PDFInfo
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- CN110060830B CN110060830B CN201910235984.4A CN201910235984A CN110060830B CN 110060830 B CN110060830 B CN 110060830B CN 201910235984 A CN201910235984 A CN 201910235984A CN 110060830 B CN110060830 B CN 110060830B
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- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000011259 mixed solution Substances 0.000 claims abstract description 44
- 239000002244 precipitate Substances 0.000 claims abstract description 35
- 150000003839 salts Chemical class 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 29
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims abstract description 15
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000004321 preservation Methods 0.000 claims abstract description 11
- 238000007789 sealing Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical group [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 40
- 239000001632 sodium acetate Substances 0.000 claims description 40
- 235000017281 sodium acetate Nutrition 0.000 claims description 40
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 24
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 15
- DVMZCYSFPFUKKE-UHFFFAOYSA-K scandium chloride Chemical compound Cl[Sc](Cl)Cl DVMZCYSFPFUKKE-UHFFFAOYSA-K 0.000 claims description 10
- FEONEKOZSGPOFN-UHFFFAOYSA-K tribromoiron Chemical compound Br[Fe](Br)Br FEONEKOZSGPOFN-UHFFFAOYSA-K 0.000 claims description 9
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 8
- 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 8
- VITRLXDSBBVNCZ-UHFFFAOYSA-K trichloroiron;hydrate Chemical compound O.Cl[Fe](Cl)Cl VITRLXDSBBVNCZ-UHFFFAOYSA-K 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- ZOYIPGHJSALYPY-UHFFFAOYSA-K vanadium(iii) bromide Chemical compound [V+3].[Br-].[Br-].[Br-] ZOYIPGHJSALYPY-UHFFFAOYSA-K 0.000 claims description 5
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 4
- 239000005695 Ammonium acetate Substances 0.000 claims description 4
- 229940043376 ammonium acetate Drugs 0.000 claims description 4
- 235000019257 ammonium acetate Nutrition 0.000 claims description 4
- VXWSFRMTBJZULV-UHFFFAOYSA-H iron(3+) sulfate hydrate Chemical compound O.[Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VXWSFRMTBJZULV-UHFFFAOYSA-H 0.000 claims description 4
- 229920005862 polyol Polymers 0.000 claims description 4
- 150000003077 polyols Chemical class 0.000 claims description 4
- APPHYFNIXVIIJR-UHFFFAOYSA-K scandium bromide Chemical compound Br[Sc](Br)Br APPHYFNIXVIIJR-UHFFFAOYSA-K 0.000 claims description 4
- DBTMQFKUVICLQN-UHFFFAOYSA-K scandium(3+);triacetate Chemical compound [Sc+3].CC([O-])=O.CC([O-])=O.CC([O-])=O DBTMQFKUVICLQN-UHFFFAOYSA-K 0.000 claims description 4
- DFCYEXJMCFQPPA-UHFFFAOYSA-N scandium(3+);trinitrate Chemical compound [Sc+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O DFCYEXJMCFQPPA-UHFFFAOYSA-N 0.000 claims description 4
- 229910021550 Vanadium Chloride Inorganic materials 0.000 claims description 3
- RPESBQCJGHJMTK-UHFFFAOYSA-I pentachlorovanadium Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[V+5] RPESBQCJGHJMTK-UHFFFAOYSA-I 0.000 claims description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 91
- 229910052706 scandium Chemical class 0.000 abstract description 11
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical class [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052720 vanadium Inorganic materials 0.000 abstract description 10
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 4
- 238000001291 vacuum drying Methods 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000005580 one pot reaction Methods 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical class [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 abstract 1
- 239000002131 composite material Substances 0.000 description 85
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 51
- BYLLFXZNSDPWSS-UHFFFAOYSA-N [Sc].[Fe] Chemical compound [Sc].[Fe] BYLLFXZNSDPWSS-UHFFFAOYSA-N 0.000 description 42
- 229910000628 Ferrovanadium Inorganic materials 0.000 description 41
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 41
- 229910052799 carbon Inorganic materials 0.000 description 26
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 16
- 238000001228 spectrum Methods 0.000 description 16
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 15
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 14
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 14
- 238000013507 mapping Methods 0.000 description 14
- 150000002505 iron Chemical class 0.000 description 12
- -1 methyl carbon Chemical compound 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- 239000002994 raw material Substances 0.000 description 11
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 150000003325 scandium Chemical class 0.000 description 10
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical class [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 9
- 229910001935 vanadium oxide Inorganic materials 0.000 description 9
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 8
- 230000005389 magnetism Effects 0.000 description 8
- 238000006722 reduction reaction Methods 0.000 description 8
- 150000003681 vanadium Chemical class 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 230000003321 amplification Effects 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000003199 nucleic acid amplification method Methods 0.000 description 5
- QUEDYRXQWSDKKG-UHFFFAOYSA-M [O-2].[O-2].[V+5].[OH-] Chemical compound [O-2].[O-2].[V+5].[OH-] QUEDYRXQWSDKKG-UHFFFAOYSA-M 0.000 description 4
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 4
- HJGMWXTVGKLUAQ-UHFFFAOYSA-N oxygen(2-);scandium(3+) Chemical compound [O-2].[O-2].[O-2].[Sc+3].[Sc+3] HJGMWXTVGKLUAQ-UHFFFAOYSA-N 0.000 description 4
- 238000002411 thermogravimetry Methods 0.000 description 4
- 241000968352 Scandia <hydrozoan> Species 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000005057 refrigeration Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ZQVHTTABFLHMPA-UHFFFAOYSA-N 2-(4-chlorophenoxy)-5-nitropyridine Chemical compound N1=CC([N+](=O)[O-])=CC=C1OC1=CC=C(Cl)C=C1 ZQVHTTABFLHMPA-UHFFFAOYSA-N 0.000 description 2
- 229910021551 Vanadium(III) chloride Inorganic materials 0.000 description 2
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000007885 magnetic separation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002077 nanosphere Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 238000001757 thermogravimetry curve Methods 0.000 description 2
- BSWDIMCNYCERGH-UHFFFAOYSA-K trichlorovanadium hydrate Chemical compound O.Cl[V](Cl)Cl BSWDIMCNYCERGH-UHFFFAOYSA-K 0.000 description 2
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 159000000021 acetate salts Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000009461 vacuum packaging Methods 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Compounds Of Iron (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of a magnetic nanometer functional material, which comprises the following steps: (a) mixing a trivalent ferric salt hydrate, a metal salt (comprising metal salts of vanadium and scandium) and acetate to obtain a mixture; (b) adding a polyhydroxy compound into the mixture, stirring and carrying out ultrasonic treatment to obtain a mixed solution; (c) heating the mixed solution to 160-180 ℃, and carrying out heat preservation and sealing reaction for 8-10 h; (d) magnetically separating the reacted mixed solution, collecting precipitate, washing and vacuum drying to obtain the magnetic nanometer material; the magnetic nano functional material prepared by the preparation method has the characteristics of excellent magnetic property, adsorption property, catalytic property and the like related to the types of the loaded metals, and the preparation cost is lower; in addition, the preparation method can promote the growth of the nano material, improve the yield, is simple to operate, only needs one-step reaction, and is beneficial to industrial production.
Description
Technical Field
The invention relates to the field of preparation and application of magnetic nano functional materials, in particular to a preparation method of a magnetic nano functional material.
Background
The nano vanadium trioxide has excellent catalytic performance for dehydrogenation and hydrogenation reactions, has great advantages when being used as an electrode material of a sodium ion battery, and can be used as a temperature sensor element because of sudden change of resistivity and magnetism when the temperature is 160K. The phase change temperature of the vanadium dioxide is 68 ℃, and the phase change is rapid. Vanadium dioxide has conductive properties that make it potentially useful in a wide range of applications in optical devices, electronic devices and optoelectronic devices. Compared with the existing nano scandium oxide material, the material has the property of magnetic ferroferric oxide under the condition of keeping the property of vanadium oxide, and is estimated to have higher value in the fields of catalysis and electrical materials.
The nanometer scandium oxide is widely applied to the fields of luminescence and superconduction as a rare earth nanometer material, and compared with the existing nanometer scandium oxide material, the material has the advantages that the property estimation of magnetic ferroferric oxide is increased under the condition of keeping the scandium oxide property, and the scandium oxide nanometer material has a higher value in the field of optical materials.
Disclosure of Invention
Therefore, the embodiment of the invention aims to provide a preparation method of a magnetic nano functional material, which aims to solve the problem of insufficient magnetism of the existing nano material and is expected to generate value in the development of temperature control electrical elements and catalysts.
In order to achieve the above object, an embodiment of the present invention provides the following:
the preparation method of the magnetic nanometer functional material comprises the following steps:
(a) mixing a trivalent ferric salt hydrate, a metal salt (comprising metal salts of vanadium and scandium) and acetate to obtain a mixture;
(b) adding a polyhydroxy compound into the mixture, stirring and carrying out ultrasonic treatment to obtain a mixed solution;
(c) heating the mixed solution to 160-180 ℃, and carrying out heat preservation and sealing reaction for 8-10 h;
(d) and (3) carrying out magnetic separation (magnetic attraction separation) on the reacted mixed solution, collecting the precipitate, washing and drying in vacuum to obtain the magnetic nano functional material.
In one embodiment of the present invention, the molar ratio of the hydrate of the ferric salt to the metal salt is 10: (0.5-6).
In one embodiment of the invention, the molar ratio of the hydrate of the ferric iron salt to the acetate is 1 to (8-10).
In one embodiment of the present invention, the concentration of the hydrate of the ferric salt in the mixed solution is 0.05-0.083 mol/L.
According to the method, the ferric iron salt hydrate, the ferric vanadium salt, the acetate and the polyhydroxy compound are selected as raw materials to prepare the magnetic ferrovanadium composite nano material, so that the magnetic ferrovanadium composite nano material has excellent magnetic performance and is low in manufacturing cost; in addition, the invention can promote the growth of the nano material, improve the yield, avoid over reduction and reduce the yield by controlling the reaction conditions; in addition, the preparation method is simple to operate and is beneficial to industrial production.
Wherein, in the step (b), the stirring speed is 360-600 r/min; stirring for 25-35 min;
wherein in the step (b), the ultrasonic frequency adopted by the ultrasonic treatment is 45000-50000 HZ; the treatment time is 15-25 min; according to the invention, through stirring and ultrasonic treatment, all raw materials can be fully and uniformly mixed, so that the full reaction among the raw materials is improved, and the yield is improved.
Wherein, in the step (d), the centrifugation speed is 8000-12000r/min, and the centrifugation time is 5-10 min; the washing agent is methanol, and the washing times are 2-4 times. According to the invention, through centrifugation and washing treatment, impurities such as a solvent on the surface of the prepared magnetic ferrovanadium composite nano material can be removed, and the purity is improved; the amount of each raw material used in the present invention is not strictly limited.
Wherein; the molar ratio of the ferric iron salt hydrate to the trivalent vanadium salt is 10: 2.
Wherein the molar ratio of the ferric iron salt hydrate to the acetate is 1 to (8-10); wherein the concentration of the ferric salt hydrate in the mixed solution is 0.05-0.083 mol/L; the invention can better improve the adsorption performance and the magnetic performance of the prepared magnetic ferrovanadium composite nano material by further limiting the dosage of each raw material.
In one embodiment of the present invention, the ferric salt hydrate is selected from any one of ferric chloride hydrate, ferric bromide hydrate, ferric nitrate hydrate and ferric sulfate hydrate.
In one embodiment of the present invention, the metal salt of vanadium and scandium is selected from any one of hydrated scandium chloride, hydrated scandium nitrate, scandium acetate, scandium bromide, vanadium chloride and vanadium bromide.
In one embodiment of the invention, the acetate salt is selected from sodium acetate or ammonium acetate.
In one embodiment of the invention, the polyol is selected from any one or more of ethylene glycol, glycerol and propylene glycol.
In a fifth aspect of the embodiments of the present invention, there is provided a magnetic ferrovanadium composite nanomaterial prepared by the above preparation method.
The magnetic ferrovanadium composite nano material has stronger magnetic property; in addition, the magnetic ferrovanadium composite nano material can be stored in a sealing manner at room temperature by adopting nitrogen or argon under a dry condition, or stored in a sealing manner by adopting methanol or ethanol soaking, does not need low-temperature refrigeration, and is convenient to store.
The magnetic ferrovanadium composite nano material is in a flower-shaped structure, and the radius of the magnetic ferrovanadium composite nano material is about 4 um;
the magnetic ferrovanadium composite nano material contains four elements of iron, vanadium, carbon and oxygen.
In the design of the present invention, it is,
(a) mixing the trivalent ferric salt hydrate, the trivalent scandium salt and the acetate to obtain a mixture;
(b) adding a polyhydroxy compound into the mixture, stirring and carrying out ultrasonic treatment to obtain a mixed solution;
(c) heating the mixed solution to 160-180 ℃, and carrying out heat preservation and sealing reaction for 8-10 h;
(d) and (3) centrifuging (or magnetically separating) the reacted mixed solution, collecting the precipitate, washing and drying in vacuum to obtain the magnetic scandium-iron composite nano material.
According to the method, the ferric iron salt hydrate, the ferric scandium salt, the acetate and the polyhydroxy compound are selected as raw materials to prepare the magnetic scandium-iron composite nano material, so that the magnetic scandium-iron composite nano material has excellent magnetic performance and is low in manufacturing cost; in addition, the invention can promote the growth of the nano material, improve the yield, avoid over reduction and reduce the yield by controlling the reaction conditions; in addition, the preparation method is simple to operate and is beneficial to industrial production.
Wherein, in the step (b), the stirring speed is 360-600 r/min; stirring for 25-35 min;
wherein in the step (b), the ultrasonic frequency adopted by the ultrasonic treatment is 45000-50000 HZ; the treatment time is 15-25 min.
According to the invention, through stirring and ultrasonic treatment, all raw materials can be fully and uniformly mixed, so that the full reaction among the raw materials is improved, and the yield is improved.
Wherein, in the step (d), the centrifugation speed is 8000-12000r/min, and the centrifugation time is 5-10 min; the washing agent is methanol, and the washing times are 2-4 times. According to the invention, through centrifugation and washing treatment, impurities such as a solvent on the surface of the prepared magnetic scandium-iron composite nano material can be removed, and the purity is improved.
In the invention, the use amount of each raw material is not strictly limited, wherein the molar ratio of the trivalent ferric salt hydrate to the trivalent scandium salt is 10: 2.
Wherein the molar ratio of the ferric iron salt hydrate to the acetate is 1 to (8-10).
Wherein the concentration of the ferric salt hydrate in the mixed solution is 0.05-0.083 mol/L.
According to the invention, the use amount of each raw material is further limited, so that the adsorption performance and the magnetic performance of the prepared magnetic scandium-iron composite nano material can be better improved.
In a design of the present invention, the ferric salt hydrate is selected from any one of ferric chloride hydrate, ferric bromide hydrate, ferric nitrate hydrate and ferric sulfate hydrate.
In a further embodiment of the present invention, the trivalent scandium salt is selected from any one of hydrated scandium chloride, hydrated scandium nitrate, scandium acetate, and scandium bromide.
In a configuration of the invention, the acetate is selected from sodium acetate or ammonium acetate.
In yet another embodiment of the present invention, the polyol is selected from any one or more of ethylene glycol, glycerol and propylene glycol.
In a second aspect of the design scheme of the invention, the magnetic scandium-iron composite nano material is prepared by the preparation method.
The magnetic scandium-iron composite nano material has excellent magnetic property, and can realize the rapid recovery of the material; in addition, the magnetic scandium-iron composite nano material can be stored in a sealed manner at room temperature by adopting nitrogen or argon under a dry condition, or stored in a sealed manner by adopting methanol or ethanol soaking, does not need low-temperature refrigeration, and is convenient to store.
The magnetic scandium-iron composite nano material is of a twist-shaped spherical structure, and the radius of the magnetic scandium-iron composite nano material is about 5 um;
the magnetic scandium-iron composite nano material contains three elements of iron, carbon and oxygen and a small amount of scandium element.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
Fig. 1 is an SEM image of the magnetic ferrovanadium composite nanomaterial prepared in example 4 of the present invention.
FIG. 2 is an EDS spectrum of the magnetic ferrovanadium composite nanomaterial prepared in example 4 of the present invention.
Fig. 3 is an element mapping map of the magnetic ferrovanadium composite nanomaterial prepared in example 4 of the present invention.
Fig. 4 is a mapping chart of vanadium element of the magnetic ferrovanadium composite nano material prepared in embodiment 4 of the invention.
Fig. 5 is a mapping chart of iron element of the magnetic ferrovanadium composite nano material prepared in example 4 of the invention.
Fig. 6 is a mapping chart of carbon elements of the magnetic ferrovanadium composite nanomaterial prepared in example 4 of the present invention.
Fig. 7 is an oxygen mapping map of the magnetic ferrovanadium composite nanomaterial prepared in example 4 of the present invention.
Fig. 8 is an XPS spectrum of the magnetic ferrovanadium composite nanomaterial prepared in example 4 of the present invention.
Fig. 9 is an XPS local magnified map of the magnetic ferrovanadium composite nanomaterial prepared in example 4 of the present invention.
Fig. 10 is an XPS local magnified map of the magnetic ferrovanadium composite nanomaterial prepared in example 4 of the present invention.
Fig. 11 is an XPS local amplification spectrum of the magnetic ferrovanadium composite nanomaterial prepared in example 4 of the present invention.
Fig. 12 is an XPS local magnified map of the magnetic ferrovanadium composite nanomaterial prepared in example 4 of the present invention.
Fig. 13 is a thermogravimetric analysis curve of the magnetic ferrovanadium composite nanomaterial prepared in example 4 of the present invention.
Fig. 14 is an SEM image of the magnetic scandium-iron composite nanomaterial prepared in example 7 of the present invention.
Fig. 15 is an EDS spectrum of the magnetic scandium-iron composite nanomaterial prepared in example 7 of the present invention.
Fig. 16 is an element mapping map of the magnetic scandium-iron composite nanomaterial prepared in embodiment 7 of the present invention.
Fig. 17 is a scandium mapping spectrum of the magnetic scandium-iron composite nanomaterial prepared in embodiment 7 of the present invention.
Fig. 18 is an iron element mapping spectrum of the magnetic scandium-iron composite nanomaterial prepared in embodiment 7 of the present invention.
Fig. 19 is a mapping spectrum of carbon elements of the magnetic scandium-iron composite nanomaterial prepared in embodiment 7 of the present invention.
Fig. 20 is an oxygen element mapping spectrum of the magnetic scandium-iron composite nanomaterial prepared in embodiment 7 of the present invention.
Fig. 21 is an XPS spectrum of the magnetic scandium-iron composite nanomaterial prepared in example 7 of the present invention.
Fig. 22 is an XPS local amplification spectrum of the magnetic scandium-iron composite nanomaterial prepared in example 7 of the present invention.
Fig. 23 is an XPS local amplification spectrum of the magnetic scandium-iron composite nanomaterial prepared in example 7 of the present invention.
Fig. 24 is an XPS local amplification spectrum of the magnetic scandium-iron composite nanomaterial prepared in example 7 of the present invention.
Fig. 25 is an XPS local amplification spectrum of the magnetic scandium-iron composite nanomaterial prepared in example 7 of the present invention.
Fig. 26 is a thermogravimetric analysis curve of the magnetic scandium-iron composite nanomaterial prepared in example 7 of the present invention.
According to the embodiment of the invention, the invention has the following advantages:
(1) the preparation method can lead the magnetic functional nano material to have excellent magnetic property and specific morphology structure through the selection of specific raw materials, and has lower manufacturing cost.
(2) The preparation method can promote the growth of the nano material and improve the yield by controlling the reaction conditions; in addition, the preparation method is simple to operate, only needs one-step reaction, and is beneficial to industrial production.
(3) The material obtained by the preparation method can be stored in a sealing way at room temperature by adopting nitrogen or argon under a dry condition, or stored in a sealing way by adopting methanol or ethanol soaking, or stored in a vacuum packaging bag, does not need low-temperature refrigeration, and is convenient to store.
Detailed Description
Other advantages and features of the present invention will become readily apparent to those skilled in the art from the following detailed description, wherein it is to be understood that the invention is not limited to the specific embodiments disclosed, but is to be construed as limited only by the appended claims. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation method of the magnetic nanometer functional material comprises the following steps:
(a) mixing a trivalent ferric salt hydrate, a metal salt (comprising metal salts of vanadium and scandium) and acetate to obtain a mixture;
(b) adding a polyhydroxy compound into the mixture, stirring and carrying out ultrasonic treatment to obtain a mixed solution;
(c) heating the mixed solution to 160-180 ℃, and carrying out heat preservation and sealing reaction for 8-10 h;
(d) and (3) carrying out magnetic separation (magnetic attraction separation) on the reacted mixed solution, collecting the precipitate, washing and drying in vacuum to obtain the magnetic nano functional material.
In one preferred embodiment, the molar ratio of the hydrate of the ferric salt to the metal salt is 10 to (0.5-6).
In one preferred embodiment, the molar ratio of the hydrate of the ferric salt to the acetate is 1: 8-10.
In a preferred embodiment, the concentration of the hydrate of the ferric salt in the mixed solution is 0.05-0.083 mol/L.
In a preferred embodiment, the hydrate of the ferric salt is selected from any one of ferric chloride hydrate, ferric bromide hydrate, ferric nitrate hydrate and ferric sulfate hydrate.
In a preferred embodiment, the vanadium and scandium metal salt is selected from any one of hydrated scandium chloride, hydrated scandium nitrate, scandium acetate, scandium bromide, vanadium chloride and vanadium bromide.
In one preferred embodiment, the acetate is selected from sodium acetate or ammonium acetate.
In one preferred embodiment, the polyol is selected from any one or more of ethylene glycol, glycerol and propylene glycol.
Example 2
The embodiment is a preparation method of a magnetic ferrovanadium composite nano material, which comprises the following steps:
(a) mixing ferric chloride hydrate, vanadium (III) bromide and sodium acetate to obtain a mixture, wherein the molar ratio of the ferric chloride hydrate to the vanadium (III) bromide is 10: 2; the molar ratio of the hydrated ferric chloride to the sodium acetate is 1: 8;
(b) adding glycerol into the mixture, stirring for 25min at 600r/min, and performing ultrasonic treatment for 25min at 45000HZ ultrasonic wave to obtain a mixed solution, wherein the concentration of hydrated ferric bromide in the mixed solution is 0.06 mol/L;
(c) heating the mixed solution to 160 ℃, and carrying out heat preservation and closed reaction for 10 hours;
(d) centrifuging the reacted mixed solution for 10min at 8000r/min, collecting precipitate, adding methanol into the precipitate, stirring, centrifuging, collecting precipitate, repeating the operations of adding methanol, stirring, centrifuging and collecting precipitate for 1 time, and vacuum drying the collected precipitate to obtain the magnetic ferrovanadium composite nano material. The material has good magnetism.
And weighing the obtained magnetic ferrovanadium composite nano material, and calculating the yield according to the yield = the mass of the magnetic ferrovanadium composite nano material/the mass of a theoretical product multiplied by 100%, wherein the mass of the theoretical product = the mass of methyl carbon in added sodium acetate + the mass of theoretical ferroferric oxide + the mass of theoretical vanadium oxide. The methyl carbon amount in the added sodium acetate is = (mass of sodium acetate/molar mass of sodium acetate). times.12; theoretical ferroferric oxide mass = (hydrated iron salt mass/hydrated iron salt molar mass) ÷ 3 × ferroferric oxide molar mass; theoretical vanadium oxide mass = (vanadium salt mass/hydrated vanadium salt molar mass) ÷ 2 × vanadium trioxide molar mass. The settlement yield result was 58.91%.
Example 3
The embodiment is a preparation method of a magnetic ferrovanadium composite nano material, which comprises the following steps:
(a) mixing hydrated ferric bromide, vanadium (III) chloride and sodium acetate to obtain a mixture, wherein the molar ratio of the hydrated ferric bromide to the vanadium (III) chloride is 10: 2; the molar ratio of the hydrated ferric bromide to the sodium acetate is 1: 10;
(b) adding propylene glycol into the mixture, stirring for 25min at 360r/min, and performing ultrasonic treatment for 15min at 50000HZ ultrasonic wave to obtain a mixed solution, wherein the concentration of hydrated ferric bromide in the mixed solution is 0.083 mol/L;
(c) heating the mixed solution to 170 ℃, and carrying out heat preservation and sealing reaction for 8 hours;
(d) centrifuging the reacted mixed solution for 5min at 12000r/min, collecting the precipitate, adding methanol into the precipitate, stirring, centrifuging, collecting the precipitate, repeating the operations of adding methanol, stirring, centrifuging and collecting the precipitate for 3 times, and drying the collected precipitate in vacuum to obtain the magnetic ferrovanadium composite nano material. The material has good magnetism.
And weighing the obtained magnetic ferrovanadium composite nano material, and calculating the yield according to the yield = the mass of the magnetic ferrovanadium composite nano material/the mass of a theoretical product multiplied by 100%, wherein the mass of the theoretical product = the mass of methyl carbon in added sodium acetate + the mass of theoretical ferroferric oxide + the mass of theoretical vanadium oxide. The methyl carbon amount in the added sodium acetate is = (mass of sodium acetate/molar mass of sodium acetate). times.12; theoretical ferroferric oxide mass = (hydrated iron salt mass/hydrated iron salt molar mass) ÷ 3 × ferroferric oxide molar mass; theoretical vanadium oxide mass = (vanadium salt mass/hydrated vanadium salt molar mass) ÷ 2 × vanadium trioxide molar mass. The settlement yield result was 61.29%.
Example 4
The embodiment is a preparation method of a magnetic ferrovanadium composite nano material, which comprises the following steps:
(a) mixing ferric chloride hydrate, vanadium (III) chloride hydrate and sodium acetate to obtain a mixture, wherein the molar ratio of the ferric chloride hydrate to the vanadium (III) chloride hydrate is 10: 2; the molar ratio of the hydrated ferric chloride to the sodium acetate is 1: 9;
(b) adding ethylene glycol into the mixture, stirring for 30min at 500r/min, and performing ultrasonic treatment for 20min at 50000HZ ultrasonic wave to obtain a mixed solution, wherein the concentration of the hydrated ferric chloride in the mixed solution is 0.05 mol/L;
(c) heating the mixed solution to 180 ℃, and carrying out heat preservation and sealed reaction for 9 hours;
(d) centrifuging the reacted mixed solution at 10000r/min for 8min, collecting precipitate, adding methanol into the precipitate, stirring, centrifuging, collecting precipitate, repeating the operations of adding methanol, stirring, centrifuging and collecting precipitate for 2 times, and vacuum drying the collected precipitate to obtain the magnetic ferrovanadium composite nano material. The material has good magnetism.
And weighing the obtained magnetic ferrovanadium composite nano material, and calculating the yield according to the yield = the mass of the magnetic ferrovanadium composite nano material/the mass of a theoretical product multiplied by 100%, wherein the mass of the theoretical product = the mass of methyl carbon in added sodium acetate + the mass of theoretical ferroferric oxide + the mass of theoretical vanadium oxide. The methyl carbon amount in the added sodium acetate is = (mass of sodium acetate/molar mass of sodium acetate). times.12; theoretical ferroferric oxide mass = (hydrated iron salt mass/hydrated iron salt molar mass) ÷ 3 × ferroferric oxide molar mass; theoretical vanadium oxide mass = (vanadium salt mass/hydrated vanadium salt molar mass) ÷ 2 × vanadium trioxide molar mass. The settlement yield result was 75.27%.
Detecting the prepared magnetic ferrovanadium composite nano material to respectively obtain an SEM (scanning electron microscope) spectrum, an EDS (electronic discharge spectroscopy) spectrum, an element mapping spectrum, TG thermogravimetric analysis and X-ray photoelectron spectroscopy XPS (X-ray photoelectron spectroscopy) of the magnetic ferrovanadium composite nano material;
wherein, the SEM atlas is shown in figure 12, and as can be seen from figure 12, the magnetic ferrovanadium composite nano material is in a flower-shaped structure, and the diameter of the flower-shaped structure is 3-5 um.
An EDS spectrum is shown in FIG. 13, and as can be seen from FIG. 13, the magnetic ferrovanadium composite nano-material comprises four elements of oxygen, iron, vanadium and carbon.
The mapping patterns of the elements are shown in fig. 14-18, and it can be known from fig. 14-18 that four elements of oxygen, iron, vanadium and carbon are uniformly distributed in the nanospheres.
As shown in fig. 19 to 22, from fig. 19 to 22, it can be known that the iron element in the material exists in two valence states, namely positive divalent valence and positive trivalent valence (the peak value at 710eV and the satellite peak around 725 eV), the vanadium element mainly exists in three valence states and four valence states (the peak values at 516.5eV, 524eV and 531 eV), the carbon element mainly exists in zero valence state (the peak value at 284.6 eV), and the oxygen element mainly exists in negative divalent state (the peak value around 530 eV), so that the material can be inferred to be the simple substance carbon-ferroferric oxide-vanadium oxide composite nano material.
Thermogravimetric analysis is carried out on the magnetic ferrovanadium composite nano material prepared by the method under the protection of argon by adopting a thermogravimetric analyzer, the analysis result is shown in fig. 26, as can be seen from fig. 26, the magnetic ferrovanadium composite nano material contains simple substance carbon, and the exothermic peak and the mass reduction phenomenon at about 322.14 ℃ are derived from reduction of ferroferric oxide and vanadium oxide by carbon elements (the reduction reaction is caused at a lower temperature due to the nanometer size).
Example 5
The embodiment is a preparation method of a magnetic scandium-iron composite nano material, which comprises the following steps:
(a) mixing hydrated ferric chloride, hydrated scandium chloride and sodium acetate to obtain a mixture, wherein the molar ratio of the hydrated ferric chloride to the hydrated scandium chloride is 10: 2; the molar ratio of the hydrated ferric chloride to the sodium acetate is 1: 8;
(b) adding ethylene glycol into the mixture, stirring for 25min at 600r/min, and then carrying out ultrasonic treatment for 25min at 45000HZ ultrasonic waves to obtain a mixed solution, wherein the concentration of the hydrated ferric chloride in the mixed solution is 0.06 mol/L;
(c) heating the mixed solution to 160 ℃, and carrying out heat preservation and closed reaction for 10 hours;
(d) and centrifuging the reacted mixed solution for 10min at 8000r/min, collecting precipitates, adding methanol into the precipitates, stirring, centrifuging, collecting the precipitates, repeating the operations of adding methanol, stirring, centrifuging and collecting the precipitates for 1 time, and performing vacuum drying on the collected precipitates to obtain the magnetic scandium-iron composite nano material with good material magnetism.
And weighing the obtained magnetic scandium-iron composite nano material, and calculating the yield according to the yield = the mass of the magnetic scandium-iron composite nano material/the mass of a theoretical product multiplied by 100%, wherein the mass of the theoretical product = the mass of methyl carbon in added sodium acetate + the mass of theoretical ferroferric oxide + the mass of theoretical scandium oxide. The methyl carbon amount in the added sodium acetate is = (mass of sodium acetate/molar mass of sodium acetate). times.12; theoretical ferroferric oxide mass = (hydrated iron salt mass/hydrated iron salt molar mass) ÷ 3 × ferroferric oxide molar mass; theoretical scandium oxide mass = (scandium salt mass/hydrated scandium salt molar mass) ÷ 2 × scandia trioxide molar mass. The settlement yield result was 49.25%.
Example 6
The embodiment is a preparation method of a magnetic scandium-iron composite nano material, which comprises the following steps:
(a) mixing hydrated ferric chloride, hydrated scandium chloride and sodium acetate to obtain a mixture, wherein the molar ratio of the hydrated ferric chloride to the hydrated scandium chloride is 10: 2; the molar ratio of the hydrated ferric chloride to the sodium acetate is 1: 10;
(b) adding ethylene glycol into the mixture, stirring for 35min at 360r/min, and performing ultrasonic treatment for 15min at 50000HZ ultrasonic wave to obtain a mixed solution, wherein the concentration of the hydrated ferric chloride in the mixed solution is 0.083 mol/L;
(c) heating the mixed solution to 170 ℃, and carrying out heat preservation and sealing reaction for 8 hours;
(d) centrifuging the reacted mixed solution for 5min at 12000r/min, collecting precipitates, adding methanol into the precipitate, stirring, centrifuging, collecting the precipitates, repeating the operations of adding methanol, stirring, centrifuging and collecting the precipitates for 3 times, and drying the collected precipitates in vacuum to obtain the magnetic scandium-iron composite nano material with good material magnetism.
And weighing the obtained magnetic scandium-iron composite nano material, and calculating the yield according to the yield = the mass of the magnetic scandium-iron composite nano material/the mass of a theoretical product multiplied by 100%, wherein the mass of the theoretical product = the mass of methyl carbon in added sodium acetate + the mass of theoretical ferroferric oxide + the mass of theoretical scandium oxide. The methyl carbon amount in the added sodium acetate is = (mass of sodium acetate/molar mass of sodium acetate). times.12; theoretical ferroferric oxide mass = (hydrated iron salt mass/hydrated iron salt molar mass) ÷ 3 × ferroferric oxide molar mass; theoretical scandium oxide mass = (scandium salt mass/hydrated scandium salt molar mass) ÷ 2 × scandia trioxide molar mass. The settlement yield result was 55.41%.
Example 7
The embodiment is a preparation method of a magnetic scandium-iron composite nano material, which comprises the following steps:
(a) mixing hydrated ferric chloride, hydrated scandium chloride and sodium acetate to obtain a mixture, wherein the molar ratio of the hydrated ferric chloride to the hydrated scandium chloride is 10: 2; the molar ratio of the hydrated ferric chloride to the sodium acetate is 1: 9;
(b) adding ethylene glycol into the mixture, stirring for 30min at 500r/min, and performing ultrasonic treatment for 20min at 50000HZ ultrasonic wave to obtain a mixed solution, wherein the concentration of the hydrated ferric chloride in the mixed solution is 0.05 mol/L;
(c) heating the mixed solution to 180 ℃, and carrying out heat preservation and sealed reaction for 9 hours;
(d) centrifuging the reacted mixed solution at 10000r/min for 8min, collecting precipitates, adding methanol into the precipitates, stirring, centrifuging, collecting the precipitates, repeating the operations of adding methanol, stirring, centrifuging and collecting the precipitates for 2 times, and drying the collected precipitates in vacuum to obtain the magnetic scandium-iron composite nano material with good material magnetism.
And weighing the obtained magnetic scandium-iron composite nano material, and calculating the yield according to the yield = the mass of the magnetic scandium-iron composite nano material/the mass of a theoretical product multiplied by 100%, wherein the mass of the theoretical product = the mass of methyl carbon in added sodium acetate + the mass of theoretical ferroferric oxide + the mass of theoretical scandium oxide. The methyl carbon amount in the added sodium acetate is = (mass of sodium acetate/molar mass of sodium acetate). times.12; theoretical ferroferric oxide mass = (hydrated iron salt mass/hydrated iron salt molar mass) ÷ 3 × ferroferric oxide molar mass; theoretical scandium oxide mass = (scandium salt mass/hydrated scandium salt molar mass) ÷ 2 × scandia trioxide molar mass. The settlement yield result was 72.49%.
Detecting the prepared magnetic scandium-iron composite nano material to respectively obtain an SEM (scanning electron microscope) spectrum, an EDS (electronic discharge spectroscopy) spectrum, an element mapping spectrum, TG (transient temperature variation) thermogravimetric analysis and X-ray photoelectron spectroscopy XPS (X-ray photoelectron spectroscopy) of the magnetic scandium-iron composite nano material;
wherein, in SEM atlas, the magnetic scandium-iron composite nano material is in a twist spherical structure, and the grain diameter is 50-150 nm.
As shown in fig. 1, the EDS spectrum of fig. 1 shows that the magnetic scandium-iron composite nanomaterial includes four elements of oxygen, iron, scandium, and carbon.
The mapping spectra of the elements are shown in fig. 2-6, and it can be known from fig. 2-6 that four elements of oxygen, iron, scandium, and carbon are uniformly distributed in the nanospheres.
As shown in fig. 7 to 10, from fig. 7 to 10, it can be known that the iron element in the material exists in two valence states, namely, a positive divalent valence state and a positive trivalent valence state (a peak value at 710eV and a satellite peak value around 725 eV), the scandium element mainly exists in a trivalent valence state (a peak value at around 401.5 eV), the carbon element mainly exists in a zero valence state (a peak value at 284.6 eV), and the oxygen element mainly exists in a negative divalent valence state (a peak value around 530 eV), so that the material can be inferred to be the elemental carbon-ferroferric oxide-scandium trioxide composite nanomaterial.
Thermogravimetric analysis is performed on the magnetic scandium-iron composite nano material prepared in the above way under the protection of argon by using a thermogravimetric analyzer, and the analysis result is shown in fig. 11, as can be seen from fig. 11, the magnetic scandium-iron composite nano material contains simple substance carbon, and the exothermic peak and the mass reduction phenomenon at about 319.53 ℃ are derived from reduction of ferroferric oxide and scandium trioxide by carbon elements (the reduction reaction is caused at a lower temperature due to the nanometer size).
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (4)
1. The preparation method of the magnetic nanometer functional material is characterized by comprising the following steps:
(a) mixing a ferric iron salt hydrate, a metal salt and an acetate to obtain a mixture; the ferric salt hydrate is selected from any one of ferric chloride hydrate, ferric bromide hydrate, ferric nitrate hydrate and ferric sulfate hydrate; the metal salt is selected from any one of hydrated scandium chloride, hydrated scandium nitrate, scandium acetate, scandium bromide, vanadium chloride and vanadium bromide; the molar ratio of the trivalent ferric salt hydrate to the metal salt is 10 to (0.5-6); the molar ratio of the ferric iron salt hydrate to the acetate is 1: 8-10;
(b) adding a polyhydroxy compound into the mixture, stirring and carrying out ultrasonic treatment to obtain a mixed solution;
(c) heating the mixed solution to 160-180 ℃, and carrying out heat preservation and sealing reaction for 8-10 h;
(d) and magnetically separating the reacted mixed solution, collecting the precipitate, washing and drying in vacuum to obtain the magnetic nano functional material.
2. The method for preparing a magnetic nano functional material according to claim 1, wherein the concentration of the ferric salt hydrate in the mixed solution is 0.05-0.083 mol/L.
3. The method for preparing a magnetic nano-functional material according to claim 1 or 2, wherein the acetate is selected from sodium acetate or ammonium acetate.
4. The method for preparing a magnetic nano-functional material according to claim 1 or 2, wherein the polyol is selected from any one or more of ethylene glycol, glycerol and propylene glycol.
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