CN105502286B - A kind of porous nano NiFe2O4Preparation method - Google Patents
A kind of porous nano NiFe2O4Preparation method Download PDFInfo
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- CN105502286B CN105502286B CN201610008267.4A CN201610008267A CN105502286B CN 105502286 B CN105502286 B CN 105502286B CN 201610008267 A CN201610008267 A CN 201610008267A CN 105502286 B CN105502286 B CN 105502286B
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- deionized water
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 229910003264 NiFe2O4 Inorganic materials 0.000 claims abstract description 46
- 238000003756 stirring Methods 0.000 claims abstract description 29
- 238000002360 preparation method Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000008367 deionised water Substances 0.000 claims abstract description 22
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 22
- 239000011259 mixed solution Substances 0.000 claims abstract description 20
- 150000001875 compounds Chemical class 0.000 claims abstract description 18
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 18
- 238000000227 grinding Methods 0.000 claims abstract description 16
- 239000003960 organic solvent Substances 0.000 claims abstract description 15
- 150000002815 nickel Chemical class 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 13
- 239000012046 mixed solvent Substances 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 24
- 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 16
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 claims description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 claims description 8
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 8
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 8
- 229940078494 nickel acetate Drugs 0.000 claims description 8
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 5
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 5
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 5
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 5
- 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 5
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 5
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 5
- 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 5
- FEONEKOZSGPOFN-UHFFFAOYSA-K tribromoiron Chemical compound Br[Fe](Br)Br FEONEKOZSGPOFN-UHFFFAOYSA-K 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 claims description 4
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical compound C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 claims description 4
- 241000723346 Cinnamomum camphora Species 0.000 claims description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims description 4
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 claims description 4
- 150000004056 anthraquinones Chemical class 0.000 claims description 4
- 229960000846 camphor Drugs 0.000 claims description 4
- 229930008380 camphor Natural products 0.000 claims description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 4
- WHRBSMVATPCWLU-UHFFFAOYSA-K iron(3+);triformate Chemical compound [Fe+3].[O-]C=O.[O-]C=O.[O-]C=O WHRBSMVATPCWLU-UHFFFAOYSA-K 0.000 claims description 4
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 claims description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 4
- 229940005561 1,4-benzoquinone Drugs 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical group CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 2
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 2
- 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 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- HZPNKQREYVVATQ-UHFFFAOYSA-L nickel(2+);diformate Chemical compound [Ni+2].[O-]C=O.[O-]C=O HZPNKQREYVVATQ-UHFFFAOYSA-L 0.000 claims description 2
- 229940090181 propyl acetate Drugs 0.000 claims description 2
- ILWRPSCZWQJDMK-UHFFFAOYSA-N triethylazanium;chloride Chemical compound Cl.CCN(CC)CC ILWRPSCZWQJDMK-UHFFFAOYSA-N 0.000 claims description 2
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- QOSMNYMQXIVWKY-UHFFFAOYSA-N Propyl levulinate Chemical compound CCCOC(=O)CCC(C)=O QOSMNYMQXIVWKY-UHFFFAOYSA-N 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 238000002242 deionisation method Methods 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- 239000000047 product Substances 0.000 description 11
- 239000003054 catalyst Substances 0.000 description 10
- 230000001699 photocatalysis Effects 0.000 description 10
- 239000004065 semiconductor Substances 0.000 description 9
- 230000007547 defect Effects 0.000 description 7
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 7
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- -1 body Substances 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 230000001172 regenerating effect Effects 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229920001400 block copolymer Polymers 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000002563 ionic surfactant Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000004530 micro-emulsion Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 229910001948 sodium oxide Inorganic materials 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229940093499 ethyl acetate Drugs 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 1
- 229940011051 isopropyl acetate Drugs 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000005287 template synthesis Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Abstract
The invention discloses a kind of porous nano NiFe2O4Preparation method, this method mixes molysite, nickel salt with deionized water, stirring and dissolving obtains the mixed solution of molysite and nickel salt, alkali is mixed with deionized water, stirring and dissolving obtains aqueous slkali, the mixed solution of molysite and nickel salt is added dropwise in aqueous slkali under stirring, continues stirring after dripping to the reaction was complete, product is washed and is centrifugally separating to obtain NiFe2O4Colloidal sol；By NiFe2O4Colloidal sol is mixed with deionized water, after being disperseed with ultrasonic wave, add organic solvent and sublimable compound template, after the hot method reaction of aqueous organic solvent mixed solvent, product is through being distilled off mixed solvent, fired again, cooling, grinding, washing, filtering, dry and grinding technics process, that is, obtain porous nano NiFe2O4Powder.This method is simple for process, and investment is small, is conducive to promote and apply.
Description
Technical field
The present invention relates to a kind of porous nano NiFe2O4Preparation method, belong to field of photocatalytic material.
Background technology
With the quickening of process of industrialization, energy crisis and environmental crisis getting worse, the exploitation of renewable new energy is standby
It is concerned.Solar energy is inexhaustible, nexhaustible, pollution-free, cheap, world community can as a kind of clean energy resource
The energy freely utilized peacefully, and various regenerative resources for example biomass energy, wind energy, ocean energy, water can etc. other energy it
This.National governments all attach great importance to the exploitation of regenerative resource, and regenerative resource is the hot research field that various countries invest energetically.
Photochemical catalyst is the semi-conducting material of a kind of utilization solar energy indispensability.At present, by scientists study
Semiconductor light-catalyst species is various, such as TiO2、CdS、SrTiO3、RuO2, ZnO and Fe2O3Deng.NiFe2O4Partly led as one kind
Body photochemical catalyst, has the characteristics that good stability, indissoluble, environmental-friendly, band gap is narrow, aboundresources and application cost are low, especially
When being with other semiconductors couplings, photocatalytic activity can be effectively improved, is one of the photochemical catalyst that application prospect is had an optimistic view of.
The structure of material and performance are closely related, structures shape performance, and the controllable preparation of material structure is material science neck
The hot research direction in domain, is the important means for preparing high performance material.Grinding on nano material controllable method for preparing at present
It is many to study carefully report.Since Penner in 1987 et al. proposes the template synthesis method of nano material, template is because having work
Skill is simple and convenient to operate, low power consumption and other advantages, is had received widespread attention.Using template, by varying template diameter and
Other technological parameters can obtain the controllable nano material of shapes and sizes.Nanocrystalline, nano thin-film is had been used at present, is partly led
The preparation of the materials such as body, nanotube and nano wire, has consequence in field of nano material preparation, becomes preparation high-performance
The important means of nano material.
NiFe2O4Nanosizing and porous are to improve NiFe2O4One of effective ways of photocatalysis efficiency.Prepare porous receive
Rice NiFe2O4Can use template, template mainly have microemulsion template, emulsion template, ionic surfactant template, it is non-from
Subtype surfactant templates, block copolymer template, composition template (such as polyoxyethylene lauryl ether and polyethylene glycol)
With monodisperse polymer particles template etc..Pass through solgel reaction, NiFe2O4Colloidal sol forms bone with secondary bond and template action
Frame structure, then takes solvent extraction or high-temperature roasting method to remove template, so as to obtain the hole suitable with template size.But
It is to prepare porous nano NiFe using above-mentioned traditional template2O4When, template is either removed using roasting method or extraction
All there are major defect.When roasting method removes template, since the temperature of template to be eliminated is high, caving in for duct can be caused, makes system
Into porous nano NiFe2O4Semiconductor light-catalyst surface defect is too many, becomes the complex centre of electron-hole, reduces light and urges
Change efficiency.Extraction rule is difficult to thoroughly eliminate template so that porous nano NiFe2O4The purity of semiconductor light-catalyst reduces, and leads
Photocatalysis performance is caused to decline.Therefore, how to prepare duct without cave in, surface zero defect, template noresidue and high-specific surface area
Porous nano NiFe2O4Semiconductor light-catalyst is an important topic.
Easily removed since sublimate easily distils, the present invention is by using the appropriate compound of sublimation temperature
Template prepares NiFe2O4Colloidal sol, reheating make template distillation removing can be prepared by porous nano NiFe2O4.With traditional template
Compare, the present invention use sublimate for template can preparation structure is controllable, duct without cave in, surface zero defect, template noresidue and
The big porous nano NiFe of specific surface area2O4Semiconductor light-catalyst.At present, on being prepared by template of sublimable compound
Porous nano NiFe2O4The method of semiconductor light-catalyst is there is not yet document report, is porous nano NiFe2O4Preparation open up
One new way, has an important practical significance.
The content of the invention
A kind of porous nano NiFe of the present invention2O4Preparation method, there is provided it is a kind of with molysite, nickel salt, alkali, go from
Sub- water is raw material, and NiFe is prepared by stirring reaction2O4Colloidal sol；NiFe2O4Colloidal sol is after ultrasonic disperse, by certain ratio
Example adds organic solvent and sublimable compound template, and after the hot method reaction of water-organic solvent mixed solvent, product is through steaming
Distillation removes mixed solvent, heats removing sublimable compound template, cooling, washing, drying and grinding technics process, i.e.,
Obtain porous nano NiFe2O4。
A kind of porous nano NiFe of the present invention2O4Preparation method, obtained porous nano NiFe2O4, can
Light and sunlight are seen under conditions of light source, to can be directly used for photocatalysis degradation organic contaminant and photocatalytic hydrogen production by water decomposition,
Also the photochemical catalyst of active higher by the method with other semiconductors couplings, can further be made, in visible ray and sunlight
Under conditions of light source, for photocatalysis degradation organic contaminant and photocatalytic hydrogen production by water decomposition；
A kind of porous nano NiFe of the present invention2O4Preparation method, adopt the following technical scheme that：
1st, it is by the mass percent of molysite, nickel salt, alkali, deionized water, organic solvent and sublimable compound template
(0.001%~70%): (0.00001%~70%): (0.001%~55%): (0.001%~90%): (0.001%~
90%): the ratio of (0.001%~90%), by a meromict of molysite, nickel salt and the total dosage of deionized water, stirring and dissolving obtains
To molysite and the mixed solution of nickel salt, by another meromict of alkali and the total dosage of deionized water, stirring and dissolving obtains aqueous slkali, stirs
The lower mixed solution by molysite and nickel salt is mixed to be added dropwise in aqueous slkali, continue after dripping stirring reaction 1~24h, product pass through from
The heart separates and washing operation and in triplicate, then is centrifugally separating to obtain NiFe2O4Colloidal sol；By NiFe2O4Colloidal sol and deionized water
After the ratio mixing that mass ratio is 1: 2~20, disperseed with the ultrasonic wave that frequency is 20KHz~1MHz, power is 30W~15KW
0.1h~24h, adds organic solvent and sublimable compound template, by water-hot method of organic solvent mixed solvent 100
0.5~24h is reacted at~250 DEG C, product heats up after mixed solvent is distilled off by 0.5~3 DEG C per minute of programming rate
To 400~600 DEG C, heat 0.5~24h and remove sublimable compound template, then through cooling down, grinding, washing, filtering,
Dry and grinding technics process, that is, obtain porous nano NiFe2O4Powder.
2nd, a kind of porous nano NiFe of the present invention2O4Preparation method, its outstanding feature is：Using traditional
Microemulsion template, emulsion template, ionic surfactant template, nonionic surface active agent template, block copolymer mould
Plate, composition template (such as polyoxyethylene lauryl ether and polyethylene glycol) and monodisperse polymer particles template template, lead to
Crossing solgel reaction makes NiFe2O4Colloidal sol forms skeleton structure with secondary bond and template action, then take solvent extraction or
When high-temperature roasting method removes template, all there are major defect, duct is such as caused to cave in, surface defect, specific surface area are low and template
The problems such as residual, reduce photocatalysis efficiency；Compared with traditional template, during using sublimate as template, sublimate easily distils and holds
Easily eliminate, therefore, NiFe is prepared for template by using the appropriate compound of sublimation temperature2O4Colloidal sol, reheats processing and removes liter
Magnificent thing, go template can be prepared by structure-controllable, duct without cave in, that surface zero defect, template noresidue and specific surface area are big is more
Hole nano-Ni/Fe2O4, be conducive to improve photocatalysis efficiency.
3rd, a kind of porous nano NiFe of the present invention2O4Preparation method, the molysite for reacting used be ferric trichloride,
Any of ferric bromide, ferric sulfate, ferric nitrate, ferric formate and ferric acetate are a variety of.
4th, a kind of porous nano NiFe of the present invention2O4Preparation method, the nickel salt for reacting used is nickel chloride, bromine
Change any of nickel, nickel sulfate, nickel nitrate, nickel formate and nickel acetate or a variety of.
5th, a kind of porous nano NiFe of the present invention2O4Preparation method, the alkali for reacting used is lithium hydroxide, hydrogen
Any of sodium oxide molybdena, potassium hydroxide, ammonium hydroxide and barium hydroxide are a variety of.
6th, a kind of porous nano NiFe of the present invention2O4Preparation method, react sublimable compound mould used
Plate is in 1,4-benzoquinone, melamine, iodine, hexa, camphor, anthraquinone, naphthalene, anthracene, metaformaldehyde and triethylamine hydrochloride
It is any one or more.
7th, a kind of porous nano NiFe of the present invention2O4Preparation method, the organic solvent for reacting used be methanol,
Ethanol, isopropanol, ether, isopropyl ether, formic acid, acetic acid, dichloromethane, chloroform, carbon tetrachloride, acetone, cyclohexanone, Methylethyl
Any of ketone, benzene, toluene, methyl acetate, ethyl acetate, propyl acetate and isopropyl acetate are a variety of.
8th, a kind of porous nano NiFe of the present invention2O4Preparation method, porous nano NiFe2O4Preparation process
In used ultrasonic disperser frequency be 20KHz~1MHz, power be 30W~15KW.
Embodiment
Here is a kind of porous nano NiFe of the present invention2O4Preparation method non-limiting example.These examples
Be only given for illustrative purposes, limitation of the invention can not be interpreted as.Because the essence of the present invention is not being departed from
God can carry out many conversion with the basis of scope to the present invention.In these embodiments, unless stated otherwise, it is all
Percentage is all referring to mass percent.
Embodiment 1
Porous nano NiFe2O4Preparation：
According to above-mentioned mass percent, by ferric trichloride, ferric bromide, nickel sulfate, nickelous bromide and the total dosage of deionized water
One meromict, stirring and dissolving obtain the mixed solution of ferric trichloride, ferric bromide, nickel sulfate and nickelous bromide, by potassium hydroxide and hydrogen
Sodium oxide molybdena and another meromict of the total dosage of deionized water, stirring and dissolving obtain the mixed solution of potassium hydroxide and sodium hydroxide,
The mixed solution of ferric trichloride, ferric bromide, nickel sulfate and nickelous bromide is added dropwise to the mixed of potassium hydroxide and sodium hydroxide under stirring
Close in solution, continue stirring reaction 2.5h after dripping, product is centrifuged with washing operation and in triplicate, then is centrifuged point
From obtaining NiFe2O4Colloidal sol；By NiFe2O4After colloidal sol and the ratio mixing that the mass ratio of deionized water is 1: 8, it is with frequency
28KHz, the ultrasonic wave that power is 2KW disperse 1.5h, after adding isopropanol, benzene, anthraquinone and hexa, by water-have
The hot method of solvent mixed solvent reacts 6h at 150 DEG C, and product is after being distilled off solvent, by 1 DEG C per minute of programming rate
500 DEG C are warming up to, heats 10h at 500 DEG C, after removing anthraquinone and the sublimable compound template of hexa, then
Through cooling down, grinding, washing, filtering, dry and grinding technics process, that is, obtain porous nano NiFe2O4Powder.
Embodiment 2
Porous nano NiFe2O4Preparation：
According to above-mentioned mass percent, by a meromict of ferric nitrate, ferric formate and nickel nitrate and the total dosage of deionized water,
Stirring and dissolving obtains the mixed solution of ferric nitrate, ferric formate and nickel nitrate, and sodium hydroxide and lithium hydroxide and deionized water is total
Another meromict of dosage, stirring and dissolving obtain the mixed solution of sodium hydroxide and lithium hydroxide, by ferric nitrate, formic acid under stirring
The mixed solution of iron and nickel nitrate is added dropwise in the mixed solution of sodium hydroxide and lithium hydroxide, continues stirring reaction after dripping
3h, product are centrifuged with washing operation and in triplicate, then are centrifugally separating to obtain NiFe2O4Colloidal sol；By NiFe2O4Colloidal sol
After the ratio for being 1: 7 with the mass ratio of deionized water mixes, disperse 2h with the ultrasonic wave that frequency is 68KHz, power is 3KW, add
After entering ethanol, toluene, 1,4-benzoquinone and camphor, 5h, product warp are reacted at 160 DEG C by water-hot method of organic solvent mixed solvent
After solvent is distilled off, 550 DEG C are warming up to by 0.5 DEG C per minute of programming rate, heats 8h at 550 DEG C, removes to benzene
After quinone and the sublimable compound template of camphor, then through cooling down, grinding, washing, filtering, dry and grinding technics process, to obtain the final product
To porous nano NiFe2O4Powder.
Embodiment 3
Porous nano NiFe2O4Preparation：
According to above-mentioned mass percent, by a meromict of ferric sulfate, nickel chloride and nickel acetate and the total dosage of deionized water,
Stirring and dissolving obtains the mixed solution of ferric sulfate, nickel chloride and nickel acetate, and lithium hydroxide and barium hydroxide and deionized water is total
Another meromict of dosage, stirring and dissolving obtain lithium hydroxide and barium hydroxide mixed solution, by ferric sulfate, nickel chloride under stirring
It is added dropwise to the mixed solution of nickel acetate in lithium hydroxide and barium hydroxide mixed solution, continues stirring reaction 3h after dripping,
Product is centrifuged with washing operation and in triplicate, then is centrifugally separating to obtain NiFe2O4Colloidal sol；By NiFe2O4Colloidal sol is with going
After the ratio mixing that the mass ratio of ionized water is 1: 10, disperse 2.5h with the ultrasonic wave that frequency is 40KHz, power is 1.5KW, add
After entering ethyl acetate, methyl ethyl ketone, acetone, naphthalene, metaformaldehyde and anthracene, by water-hot method of organic solvent mixed solvent 170
5h is reacted at DEG C, product is warming up at 480 DEG C, 480 DEG C by 1.5 DEG C per minute of programming rate and added after solvent is distilled off
12h is heat-treated, after removing naphthalene, metaformaldehyde and the sublimable compound template of anthracene, then through cooling down, grinding, washing, filtering, doing
Dry and grinding technics process, that is, obtain porous nano NiFe2O4Powder.
Embodiment 4
Porous nano NiFe2O4Preparation：
According to above-mentioned mass percent, by ferric nitrate, ferric trichloride, nickel acetate and nickel sulfate and the total dosage of deionized water
One meromict, stirring and dissolving obtain the mixed solution of ferric nitrate, ferric trichloride, nickel acetate and nickel sulfate, by sodium hydroxide and ammonia
Water and another meromict of the total dosage of deionized water, stirring and dissolving obtain the mixed solution of sodium hydroxide and ammonium hydroxide, will under stirring
Ferric nitrate, ferric trichloride, the mixed solution of nickel acetate and nickel sulfate are added dropwise in the mixed solution of sodium hydroxide and ammonium hydroxide, are added dropwise
Continue stirring reaction 2.5h after complete, product is centrifuged with washing operation and in triplicate, then is centrifugally separating to obtain NiFe2O4
Colloidal sol；By NiFe2O4After the ratio mixing that colloidal sol and the mass ratio of deionized water are 1: 6, with frequency be 50KHz, power be
The ultrasonic wave of 2.5KW disperses 2.5h, after adding ethanol and anthracene, by water-hot method of organic solvent mixed solvent at 180 DEG C it is anti-
4h is answered, product is warming up to 520 DEG C after solvent is distilled off, by 2 DEG C per minute of programming rate, heats 8h at 520 DEG C,
After removing the sublimable compound template of anthracene, then through cooling down, grinding, washing, filtering, dry and grinding technics process, that is, obtain
Porous nano NiFe2O4Powder.
Claims (4)
- A kind of 1. porous nano NiFe2O4Preparation method, it is characterised in that：By trivalent iron salt, divalent nickel salt, alkali, deionization The mass percent of water, organic solvent and sublimable compound template is (10.9%~13.2%): (4.4%~5.1%): (6.0%~10.8%): (51.5%~58.7%): (17.0%~18.0%): the ratio of (1.8%~3.0%), by trivalent One meromict of molysite, divalent nickel salt and the total dosage of deionized water, stirring and dissolving obtain the mixing of trivalent iron salt and divalent nickel salt Solution, by another meromict of alkali and the total dosage of deionized water, stirring and dissolving obtains aqueous slkali, by trivalent iron salt and two under stirring The mixed solution of valency nickel salt is added dropwise in aqueous slkali, continues stirring 1~24h of reaction after dripping, and product is centrifuged and washes Operation and in triplicate is washed, then is centrifugally separating to obtain NiFe2O4Colloidal sol；By NiFe2O4Colloidal sol and the mass ratio of deionized water are 1: 2~20 ratio is by the deionized water separately taken and NiFe2O4After colloidal sol mixing, with frequency be 20KHz~1MHz, power be 30W~ The ultrasonic wave of 15KW disperses 0.1h~24h, adds organic solvent and sublimable compound template, is mixed by water-organic solvent The hot method of bonding solvent reacts 0.5~24h at 100~250 DEG C, and product is after being distilled off mixed solvent, by per minute 0.5~3 DEG C programming rate be warming up to 400~600 DEG C, heat 0.5~24h and remove sublimable compound template, then through cooling, Grinding, washing, filtering, dry and grinding technics process, that is, obtain porous nano NiFe2O4Powder；Wherein, the sublimable compound template be 1,4-benzoquinone, melamine, iodine, hexa, camphor, anthraquinone, Any of naphthalene, anthracene, metaformaldehyde and triethylamine hydrochloride are a variety of；Wherein, the organic solvent is methanol, ethanol, isopropanol, ether, isopropyl ether, formic acid, acetic acid, dichloromethane, chlorine Imitative, carbon tetrachloride, acetone, cyclohexanone, methyl ethyl ketone, benzene, toluene, methyl acetate, ethyl acetate, propyl acetate and acetic acid are different Any of propyl ester is a variety of.
- 2. the preparation method described in claim 1, it is characterised in that the trivalent iron salt for reacting used be ferric trichloride, ferric bromide, Any of ferric sulfate, ferric nitrate, ferric formate and ferric acetate are a variety of.
- 3. the preparation method described in claim 1, it is characterised in that the divalent nickel salt for reacting used is nickel chloride, nickelous bromide, sulphur Any of sour nickel, nickel nitrate, nickel formate and nickel acetate are a variety of.
- 4. the preparation method described in claim 1, it is characterised in that the alkali for reacting used is lithium hydroxide, sodium hydroxide, hydrogen-oxygen Change any of potassium, ammonium hydroxide and barium hydroxide or a variety of.
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| CN106277076B (en) * | 2016-08-16 | 2018-02-02 | 贵州省分析测试研究院 | A kind of synthetic method of spinel type compound and its application |
| CN108793486A (en) * | 2018-04-24 | 2018-11-13 | 苏州麦普菲环境技术有限公司 | A method of removal nickel in waste electroplating water ion |
| CN109292829B (en) * | 2018-10-22 | 2021-06-29 | 安庆泽远化工有限公司 | Porous nano CoFe2O4Process for preparing nanoparticles |
| CN111036213A (en) * | 2018-12-27 | 2020-04-21 | 宁夏大学 | Hollow spherical nickel ferrite and preparation method and application thereof |
| CN110560679B (en) * | 2019-08-08 | 2021-10-29 | 安徽师范大学 | Ni-Co alloy material with three-dimensional polyhedral structure and preparation method and application thereof |
| CN110479286B (en) * | 2019-09-09 | 2022-03-08 | 井冈山大学 | Preparation method of titanium-iron-nickel high hydrogen evolution active electrocatalyst |
| CN110828787B (en) * | 2019-10-09 | 2021-09-21 | 中国科学院福建物质结构研究所 | NiFe2O4Nano composite material and preparation method and application thereof |
| CN111454579A (en) * | 2020-04-26 | 2020-07-28 | 张荣虎 | Nano nickel ferrite loaded graphene-based wave-absorbing material and preparation method thereof |
| CN114395396A (en) * | 2022-01-24 | 2022-04-26 | 济南市中蓝德新材料技术中心 | Preparation and application of soil remediation modifier |
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| CN101215010A (en) * | 2007-12-27 | 2008-07-09 | 哈尔滨工业大学 | Self-spreading high temperature method for synthesizing NiFe2O4 powder and sintering NiFe2O4 |
| CN102153155A (en) * | 2010-07-29 | 2011-08-17 | 兰州理工大学 | Method for preparing spinel NiFe2O4 nano powder |
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| JPS6347908A (en) * | 1986-08-16 | 1988-02-29 | Sony Corp | Nickel ferrite-system spinel thin film |
| CN101215010A (en) * | 2007-12-27 | 2008-07-09 | 哈尔滨工业大学 | Self-spreading high temperature method for synthesizing NiFe2O4 powder and sintering NiFe2O4 |
| CN102153155A (en) * | 2010-07-29 | 2011-08-17 | 兰州理工大学 | Method for preparing spinel NiFe2O4 nano powder |
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