CN105502286A - Preparation method of porous nano NiFe2O4 - Google Patents
Preparation method of porous nano NiFe2O4 Download PDFInfo
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- CN105502286A CN105502286A CN201610008267.4A CN201610008267A CN105502286A CN 105502286 A CN105502286 A CN 105502286A CN 201610008267 A CN201610008267 A CN 201610008267A CN 105502286 A CN105502286 A CN 105502286A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 229910003264 NiFe2O4 Inorganic materials 0.000 title abstract 5
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 title abstract 5
- 238000000034 method Methods 0.000 claims abstract description 30
- 238000003756 stirring Methods 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- 150000001875 compounds Chemical class 0.000 claims abstract description 19
- 239000003960 organic solvent Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 150000002815 nickel Chemical class 0.000 claims abstract description 14
- 239000012046 mixed solvent Substances 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 claims description 61
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 24
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 19
- 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
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- 230000001699 photocatalysis Effects 0.000 claims description 13
- 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
- 238000005119 centrifugation Methods 0.000 claims description 12
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-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
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-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
- 238000007146 photocatalysis Methods 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
- 238000004821 distillation Methods 0.000 claims description 8
- 229940078494 nickel acetate Drugs 0.000 claims description 8
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 8
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 7
- 230000007547 defect Effects 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 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
- 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 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
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-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
- -1 polyoxyethylene lauryl ether Polymers 0.000 claims description 5
- FEONEKOZSGPOFN-UHFFFAOYSA-K tribromoiron Chemical compound Br[Fe](Br)Br FEONEKOZSGPOFN-UHFFFAOYSA-K 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
- 229940005561 1,4-benzoquinone Drugs 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 241000723346 Cinnamomum camphora Species 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
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 229920001400 block copolymer Polymers 0.000 claims description 3
- 239000000839 emulsion Substances 0.000 claims description 3
- 239000002563 ionic surfactant Substances 0.000 claims description 3
- 239000004530 micro-emulsion Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 claims description 3
- 238000000638 solvent extraction Methods 0.000 claims description 3
- 238000000859 sublimation Methods 0.000 claims description 3
- 230000008022 sublimation Effects 0.000 claims description 3
- 239000004094 surface-active agent Substances 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 2
- 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
- 229940093499 ethyl acetate Drugs 0.000 claims description 2
- 235000019253 formic acid Nutrition 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
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 claims description 2
- 229940011051 isopropyl acetate Drugs 0.000 claims description 2
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 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
- 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
- 238000001914 filtration Methods 0.000 abstract description 3
- 159000000014 iron salts Chemical class 0.000 abstract 3
- 238000002156 mixing Methods 0.000 abstract 3
- 239000012670 alkaline solution Substances 0.000 abstract 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 238000004729 solvothermal method Methods 0.000 abstract 1
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- 239000004065 semiconductor Substances 0.000 description 11
- 239000003054 catalyst Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 5
- 230000001172 regenerating effect Effects 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 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
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012761 high-performance material Substances 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
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005287 template synthesis Methods 0.000 description 1
- 239000010409 thin film Substances 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 preparation method of porous nano NiFe2O4. The method is characterized by mixing iron salts, nickel salts and deionized water, obtaining a mixed solution of iron salts and nickel salts after stirring and dissolving, mixing alkalis with deionized water, stirring for dissolving so as to obtain an alkaline solution, dropwise adding the mixed solution of iron salts and nickel salts to the alkaline solution while stirring, continuously stirring the solutions after dropwise adding is completed until the reaction is complete and carrying out washing and centrifugal separation on the product, thus obtaining NiFe2O4 sol; mixing the NiFe2O4 sol with deionized water, after ultrasonic dispersion, adding organic solvents and sublimable compound templates, after reaction through a water-organic solvent mixed solvothermal method, distilling the product to remove a mixed solvent and then carrying out roasting, cooling, grinding, washing, filtering, drying and grinding processes, thus obtaining the porous nano NiFe2O4 powder. The method is simple and practicable in process and low in investment and is beneficial to popularization and application.
Description
Technical field
The present invention relates to a kind of porous nano NiFe
2o
4preparation method, belong to field of photocatalytic material.
Background technology
Along with the quickening of process of industrialization, energy crisis and environmental crisis are day by day serious, and the exploitation of renewable new forms of energy receives much concern.Solar energy, as a kind of clean energy resource, is the energy that inexhaustible, nexhaustible, pollution-free, cheap, world community all can freely be utilized peacefully, be also various regenerative resource as other energy such as biomass energy, wind energy, ocean energy, water energy 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 that a class develops solar energy indispensability.At present, of a great variety by the semiconductor light-catalyst of scientists study, as TiO
2, CdS, SrTiO
3, RuO
2, ZnO and Fe
2o
3deng.NiFe
2o
4as a based semiconductor photochemical catalyst, have that good stability, indissoluble, environmental friendliness, band gap are narrow, aboundresources and the feature such as application cost is low, especially time with other semiconductors coupling, effectively can improve photocatalytic activity, be one of good photochemical catalyst of application prospect.
The Structure and Properties of material is closely related, structures shape performance, and the controlled synthesis of material structure is the hot research direction of material science, is the important means preparing high performance material.Research report at present about nano material controllable method for preparing is a lot.Since the people such as Penner in 1987 propose the template synthesis method of nano material, technique is simple, easy to operate, low power consumption and other advantages because having for template, receives and pays close attention to widely.Utilizing template, shape and the controlled nano material of size can be obtained by changing the diameter of template and other technological parameter.At present for the preparation of the materials such as nanocrystalline, nano thin-film, semiconductor, nanotube and nano wire, in field of nano material preparation, there is consequence, become the important means preparing high-performance nano material.
NiFe
2o
4nanometer and porous improve NiFe
2o
4one of effective ways of photocatalysis efficiency.Prepare porous nano NiFe
2o
4can adopt template, template mainly contains microemulsion template, emulsion template, ionic surfactant template, nonionic surface active agent template, block copolymer template, composition template (as polyoxyethylene lauryl ether and polyethylene glycol) and monodisperse polymer particles template etc.By solgel reaction, NiFe
2o
4colloidal sol forms skeleton structure with secondary bond and template action, then takes solvent extraction or high-temperature roasting method removing template, thus obtains the hole suitable with template size.But, use above-mentioned traditional Template preparation porous nano NiFe
2o
4time, be adopt roasting method or extraction to remove template all to there is major defect.During roasting method removing template, because the temperature that will eliminate template is high, caving in of duct can be caused, make the porous nano NiFe made
2o
4semiconductor light-catalyst blemish is too many, becomes the complex centre of electron-hole, reduces photocatalysis efficiency.Extraction rule is difficult to thoroughly eliminate template, makes porous nano NiFe
2o
4the purity of semiconductor light-catalyst reduces, and causes photocatalysis performance to decline.Therefore, how to prepare duct without caving in, surperficial zero defect, template noresidue and high-specific surface area porous nano NiFe
2o
4semiconductor light-catalyst is an important topic.
Easily remove because sublimate easily distils, therefore, the present invention is Template preparation NiFe by the compound adopting sublimation temperature suitable
2o
4colloidal sol, then heating makes template distillation removing can obtain porous nano NiFe
2o
4.Compared with traditional template, the present invention adopt sublimate be template can prepare structure-controllable, duct without caving in, surperficial zero defect, template noresidue and the large porous nano NiFe of specific area
2o
4semiconductor light-catalyst.At present, about with sublimable compound for Template preparation porous nano NiFe
2o
4the method of semiconductor light-catalyst there is not yet bibliographical information, is porous nano NiFe
2o
4preparation open a new way, there is important practical significance.
Summary of the invention
A kind of porous nano NiFe of the present invention
2o
4preparation method, provide a kind of with molysite, nickel salt, alkali, deionized water for raw material, prepare NiFe by stirring reaction
2o
4colloidal sol; NiFe
2o
4colloidal sol is after ultrasonic disperse, add organic solvent and sublimable compound template according to a certain percentage, after the hot method reaction of water-organic solvent mixed solvent, product, through distillation removing mixed solvent, the sublimable compound template of heating removing, cooling, washing, drying and grinding technics process, namely obtains porous nano NiFe
2o
4.
A kind of porous nano NiFe of the present invention
2o
4preparation method, obtained porous nano NiFe
2o
4under visible ray and sunshine are the condition of light source, photocatalysis degradation organic contaminant and photocatalytic hydrogen production by water decomposition can be directly used in, also by the method with other semiconductors coupling, obtained active higher photochemical catalyst further, under visible ray and sunshine are the condition of light source, for photocatalysis degradation organic contaminant and photocatalytic hydrogen production by water decomposition;
A kind of porous nano NiFe of the present invention
2o
4preparation method, adopt following technical scheme:
1, by molysite, nickel salt, alkali, deionized water, the mass percent of organic solvent and sublimable compound template is (0.001% ~ 70%): (0.00001% ~ 70%): (0.001% ~ 55%): (0.001% ~ 90%): (0.001% ~ 90%): the ratio of (0.001% ~ 90%), by molysite, one meromict of nickel salt and the total consumption of deionized water, stirring and dissolving obtains the mixed solution of molysite and nickel salt, second half of total to alkali and deionized water consumption is mixed, stirring and dissolving obtains aqueous slkali, under stirring, the mixed solution of molysite and nickel salt is added dropwise in aqueous slkali, drip rear continuation stirring reaction 1 ~ 24h, product through centrifugation and washing operation and in triplicate, centrifugation obtains NiFe again
2o
4colloidal sol, by NiFe
2o
4after the ratio that colloidal sol and the mass ratio of deionized water are 1: 2 ~ 20 mixes, be 20KHz ~ 1MHz by frequency, power is the ultrasonic wave dispersion 0.1h ~ 24h of 30W ~ 15KW, add organic solvent and sublimable compound template, at 100 ~ 250 DEG C, 0.5 ~ 24h is reacted by water-hot method of organic solvent mixed solvent, product is after distillation removing mixed solvent, 400 ~ 600 DEG C are warmed up to by the programming rate of 0.5 ~ 3 DEG C per minute, heat 0.5 ~ 24h and remove sublimable compound template, again through cooling, grinding, washing, filter, drying and grinding technics process, namely porous nano NiFe is obtained
2o
4powder.
2, a kind of porous nano NiFe of the present invention
2o
4preparation method, its outstanding feature is: adopt the templates such as traditional microemulsion template, emulsion template, ionic surfactant template, nonionic surface active agent template, block copolymer template, composition template (as polyoxyethylene lauryl ether and polyethylene glycol) and monodisperse polymer particles template, make NiFe by solgel reaction
2o
4colloidal sol forms skeleton structure with secondary bond and template action, when then taking solvent extraction or high-temperature roasting method removing template, problems such as all there is major defect, caving in as caused duct, the low and template of blemish, specific area is residual, reduces photocatalysis efficiency; Compared with traditional template, when taking sublimate as template, sublimate easily distils and easily eliminates, and therefore, is Template preparation NiFe by the compound adopting sublimation temperature suitable
2o
4colloidal sol, then heat removing sublimate, go template can obtain structure-controllable, duct without caving in, surperficial zero defect, template noresidue and the large porous nano NiFe of specific area
2o
4, be conducive to improving photocatalysis efficiency.
3, a kind of porous nano NiFe of the present invention
2o
4preparation method, the molysite reacting used is any one or more in ferric trichloride, ferric bromide, ferric sulfate, ferric nitrate, ferric formate and ferric acetate.
4, a kind of porous nano NiFe of the present invention
2o
4preparation method, the nickel salt reacting used is any one or more in nickel chloride, nickelous bromide, nickelous sulfate, nickel nitrate, nickel formate and nickel acetate.
5, a kind of porous nano NiFe of the present invention
2o
4preparation method, the alkali reacting used is any one or more in lithium hydroxide, NaOH, potassium hydroxide, ammoniacal liquor and barium hydroxide.
6, a kind of porous nano NiFe of the present invention
2o
4preparation method, the sublimable compound template of reacting used is any one or more in 1,4-benzoquinone, melamine, iodine, hexa, camphor, anthraquinone, naphthalene, anthracene, metaformaldehyde and triethylamine hydrochloride.
7, a kind of porous nano NiFe of the present invention
2o
4preparation method, the organic solvent reacting used is any one or more in methyl alcohol, ethanol, isopropyl alcohol, ether, isopropyl ether, formic acid, acetic acid, carrene, chloroform, carbon tetrachloride, acetone, cyclohexanone, methyl ethyl ketone, benzene, toluene, methyl acetate, ethyl acetate, propyl acetate and isopropyl acetate.
8, a kind of porous nano NiFe of the present invention
2o
4preparation method, porous nano NiFe
2o
4preparation process in the frequency of ultrasonic disperser used be 20KHz ~ 1MHz, power is 30W ~ 15KW.
Detailed description of the invention
Here is a kind of porous nano NiFe of the present invention
2o
4the non-limiting example of preparation method.The providing of these examples is only used to the object illustrated, can not be interpreted as limitation of the invention.Because without departing from the spirit and scope of the present invention, many conversion can be carried out to the present invention.In these embodiments, unless stated otherwise, all percentage all refers to mass percent.
Embodiment 1
Porous nano NiFe
2o
4preparation:
According to above-mentioned mass percent, by ferric trichloride, ferric bromide, nickelous sulfate, one meromict of nickelous bromide and the total consumption of deionized water, stirring and dissolving obtains ferric trichloride, ferric bromide, the mixed solution of nickelous sulfate and nickelous bromide, second half of potassium hydroxide and NaOH and the total consumption of deionized water is mixed, stirring and dissolving obtains the mixed solution of potassium hydroxide and NaOH, by ferric trichloride under stirring, ferric bromide, the mixed solution of nickelous sulfate and nickelous bromide is added dropwise in the mixed solution of potassium hydroxide and NaOH, drip rear continuation stirring reaction 2.5h, product through centrifugation and washing operation and in triplicate, centrifugation obtains NiFe again
2o
4colloidal sol, by NiFe
2o
4after the ratio that colloidal sol and the mass ratio of deionized water are 1: 8 mixes, be 28KHz by frequency, power is the ultrasonic wave dispersion 1.5h of 2KW, add isopropyl alcohol, benzene, after anthraquinone and hexa, at 150 DEG C, 6h is reacted by water-hot method of organic solvent mixed solvent, product removes after desolventizing through distillation, 500 DEG C are warmed up to by the programming rate of 1 DEG C per minute, 10h is heated at 500 DEG C, after removing anthraquinone and the sublimable compound template of hexa, again through cooling, grinding, washing, filter, drying and grinding technics process, namely porous nano NiFe is obtained
2o
4powder.
Embodiment 2
Porous nano NiFe
2o
4preparation:
According to above-mentioned mass percent, by ferric nitrate, one meromict of ferric formate and nickel nitrate and the total consumption of deionized water, stirring and dissolving obtains ferric nitrate, the mixed solution of ferric formate and nickel nitrate, second half of NaOH and lithium hydroxide and the total consumption of deionized water is mixed, stirring and dissolving obtains the mixed solution of NaOH and lithium hydroxide, by ferric nitrate under stirring, the mixed solution of ferric formate and nickel nitrate is added dropwise in the mixed solution of NaOH and lithium hydroxide, drip rear continuation stirring reaction 3h, product through centrifugation and washing operation and in triplicate, centrifugation obtains NiFe again
2o
4colloidal sol, by NiFe
2o
4after the ratio that colloidal sol and the mass ratio of deionized water are 1: 7 mixes, with frequency be 68KHz, power be 3KW ultrasonic wave dispersion 2h, after adding ethanol, toluene, 1,4-benzoquinone and camphor, at 160 DEG C, 5h is reacted by water-hot method of organic solvent mixed solvent, product removes after desolventizing through distillation, 550 DEG C are warmed up to by the programming rate of 0.5 DEG C per minute, 8h is heated at 550 DEG C, after removing 1,4-benzoquinone and the sublimable compound template of camphor, again through cooling, grinding, washing, filtration, dry and grinding technics process, namely obtain porous nano NiFe
2o
4powder.
Embodiment 3
Porous nano NiFe
2o
4preparation:
According to above-mentioned mass percent, by ferric sulfate, one meromict of nickel chloride and nickel acetate and the total consumption of deionized water, stirring and dissolving obtains ferric sulfate, the mixed solution of nickel chloride and nickel acetate, second half of lithium hydroxide and barium hydroxide and the total consumption of deionized water is mixed, stirring and dissolving obtains lithium hydroxide and barium hydroxide mixed solution, by ferric sulfate under stirring, the mixed solution of nickel chloride and nickel acetate is added dropwise in lithium hydroxide and barium hydroxide mixed solution, drip rear continuation stirring reaction 3h, product through centrifugation and washing operation and in triplicate, centrifugation obtains NiFe again
2o
4colloidal sol, by NiFe
2o
4after the ratio that colloidal sol and the mass ratio of deionized water are 1: 10 mixes, be 40KHz by frequency, power is the ultrasonic wave dispersion 2.5h of 1.5KW, add ethyl acetate, methyl ethyl ketone, acetone, naphthalene, after metaformaldehyde and anthracene, at 170 DEG C, 5h is reacted by water-hot method of organic solvent mixed solvent, product removes after desolventizing through distillation, 480 DEG C are warmed up to by the programming rates of 1.5 DEG C per minute, 12h is heated at 480 DEG C, removing naphthalene, after metaformaldehyde and the sublimable compound template of anthracene, again through cooling, grinding, washing, filter, drying and grinding technics process, namely porous nano NiFe is obtained
2o
4powder.
Embodiment 4
Porous nano NiFe
2o
4preparation:
According to above-mentioned mass percent, by ferric nitrate, ferric trichloride, one meromict of nickel acetate and nickelous sulfate and the total consumption of deionized water, stirring and dissolving obtains ferric nitrate, ferric trichloride, the mixed solution of nickel acetate and nickelous sulfate, second half of NaOH and ammoniacal liquor and the total consumption of deionized water is mixed, stirring and dissolving obtains the mixed solution of NaOH and ammoniacal liquor, by ferric nitrate under stirring, ferric trichloride, the mixed solution of nickel acetate and nickelous sulfate is added dropwise in the mixed solution of NaOH and ammoniacal liquor, drip rear continuation stirring reaction 2.5h, product through centrifugation and washing operation and in triplicate, centrifugation obtains NiFe again
2o
4colloidal sol, by NiFe
2o
4after the ratio that colloidal sol and the mass ratio of deionized water are 1: 6 mixes, with frequency be 50KHz, power be 2.5KW ultrasonic wave dispersion 2.5h, after adding ethanol and anthracene, at 180 DEG C, 4h is reacted by water-hot method of organic solvent mixed solvent, product removes after desolventizing through distillation, 520 DEG C are warmed up to by the programming rates of 2 DEG C per minute, 8h is heated at 520 DEG C, after the sublimable compound template of removing anthracene, again through cooling, grinding, washing, filtration, dry and grinding technics process, namely obtain porous nano NiFe
2o
4powder.
Claims (8)
1. a porous nano NiFe
2o
4preparation method, it is characterized in that: by molysite, nickel salt, alkali, deionized water, the mass percent of organic solvent and sublimable compound template is (0.001% ~ 70%): (0.00001% ~ 70%): (0.001% ~ 55%): (0.001% ~ 90%): (0.001% ~ 90%): the ratio of (0.001% ~ 90%), by molysite, one meromict of nickel salt and the total consumption of deionized water, stirring and dissolving obtains the mixed solution of molysite and nickel salt, second half of total to alkali and deionized water consumption is mixed, stirring and dissolving obtains aqueous slkali, under stirring, the mixed solution of molysite and nickel salt is added dropwise in aqueous slkali, drip rear continuation stirring reaction 1 ~ 24h, product through centrifugation and washing operation and in triplicate, centrifugation obtains NiFe again
2o
4colloidal sol, by NiFe
2o
4after the ratio that colloidal sol and the mass ratio of deionized water are 1: 2 ~ 20 mixes, be 20KHz ~ 1MHz by frequency, power is the ultrasonic wave dispersion 0.1h ~ 24h of 30W ~ 15KW, add organic solvent and sublimable compound template, at 100 ~ 250 DEG C, 0.5 ~ 24h is reacted by water-hot method of organic solvent mixed solvent, product is after distillation removing mixed solvent, 400 ~ 600 DEG C are warmed up to by the programming rate of 0.5 ~ 3 DEG C per minute, heat 0.5 ~ 24h and remove sublimable compound template, again through cooling, grinding, washing, filter, drying and grinding technics process, namely porous nano NiFe is obtained
2o
4powder.
2. preparation method according to claim 1, its outstanding feature is: adopt the templates such as traditional microemulsion template, emulsion template, ionic surfactant template, nonionic surface active agent template, block copolymer template, composition template (as polyoxyethylene lauryl ether and polyethylene glycol) and monodisperse polymer particles template, make NiFe by solgel reaction
2o
4colloidal sol forms skeleton structure with secondary bond and template action, when then taking solvent extraction or high-temperature roasting method removing template, problems such as all there is major defect, caving in as caused duct, the low and template of blemish, specific area is residual, reduces photocatalysis efficiency; Compared with traditional template, when taking sublimate as template, sublimate easily distils and easily eliminates, and therefore, is Template preparation NiFe by the compound adopting sublimation temperature suitable
2o
4colloidal sol, then heat removing sublimate template can obtain structure-controllable, duct without caving in, surperficial zero defect, template noresidue and the large porous nano NiFe of specific area
2o
4, be conducive to improving photocatalysis efficiency.
3. preparation method according to claim 1, is characterized in that reacting molysite used is any one or more in ferric trichloride, ferric bromide, ferric sulfate, ferric nitrate, ferric formate and ferric acetate.
4. preparation method according to claim 1, is characterized in that reacting nickel salt used is any one or more in nickel chloride, nickelous bromide, nickelous sulfate, nickel nitrate, nickel formate and nickel acetate.
5. preparation method according to claim 1, is characterized in that reacting alkali used is any one or more in lithium hydroxide, NaOH, potassium hydroxide, ammoniacal liquor and barium hydroxide.
6. preparation method according to claim 1, is characterized in that reacting sublimable compound template used is any one or more in 1,4-benzoquinone, melamine, iodine, hexa, camphor, anthraquinone, naphthalene, anthracene, metaformaldehyde and triethylamine hydrochloride.
7. preparation method according to claim 1, is characterized in that reacting organic solvent used is any one or more in methyl alcohol, ethanol, isopropyl alcohol, ether, isopropyl ether, formic acid, acetic acid, carrene, chloroform, carbon tetrachloride, acetone, cyclohexanone, methyl ethyl ketone, benzene, toluene, methyl acetate, ethyl acetate, propyl acetate and isopropyl acetate.
8. preparation method according to claim 1, is characterized in that the frequency of ultrasonic disperser used in course of reaction is 20KHz ~ 1MHz, power is 30W ~ 15KW.
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| CN106277076A (en) * | 2016-08-16 | 2017-01-04 | 贵州省分析测试研究院 | The synthetic method of a kind of spinel type compound and application thereof |
| 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 |
| CN109292829A (en) * | 2018-10-22 | 2019-02-01 | 安徽理工大学 | A kind of porous nano CoFe2O4The preparation method of nanoparticle |
| CN110479286A (en) * | 2019-09-09 | 2019-11-22 | 井冈山大学 | A kind of preparation method of the high hydrogen evolution activity elctro-catalyst of ferrotianium nickel |
| CN110560679A (en) * | 2019-08-08 | 2019-12-13 | 安徽师范大学 | Ni-Co alloy material with three-dimensional polyhedral structure and preparation method and application thereof |
| CN110828787A (en) * | 2019-10-09 | 2020-02-21 | 中国科学院福建物质结构研究所 | NiFe2O4Nano composite material and preparation method and application thereof |
| CN111036213A (en) * | 2018-12-27 | 2020-04-21 | 宁夏大学 | Hollow spherical nickel ferrite 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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| 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 |
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| 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 |
| CN109292829A (en) * | 2018-10-22 | 2019-02-01 | 安徽理工大学 | A kind of porous nano CoFe2O4The preparation method of nanoparticle |
| 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 |
| CN110560679A (en) * | 2019-08-08 | 2019-12-13 | 安徽师范大学 | Ni-Co alloy material with three-dimensional polyhedral structure and preparation method and application thereof |
| CN110479286A (en) * | 2019-09-09 | 2019-11-22 | 井冈山大学 | A kind of preparation method of the high hydrogen evolution activity elctro-catalyst of ferrotianium nickel |
| CN110479286B (en) * | 2019-09-09 | 2022-03-08 | 井冈山大学 | Preparation method of titanium-iron-nickel high hydrogen evolution active electrocatalyst |
| CN110828787A (en) * | 2019-10-09 | 2020-02-21 | 中国科学院福建物质结构研究所 | NiFe2O4Nano composite material and preparation method and application thereof |
| 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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