CN105731547B - A kind of hydrophobic ferroferric oxide magnetic nano-particles and preparation method thereof - Google Patents
A kind of hydrophobic ferroferric oxide magnetic nano-particles and preparation method thereof Download PDFInfo
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 239000002122 magnetic nanoparticle Substances 0.000 title claims abstract description 73
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims abstract description 17
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 16
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 123
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 25
- 239000002245 particle Substances 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 21
- 241001502050 Acis Species 0.000 claims description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 20
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 20
- 150000002148 esters Chemical class 0.000 claims description 20
- 239000010703 silicon Substances 0.000 claims description 20
- 229910052710 silicon Inorganic materials 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 230000001476 alcoholic effect Effects 0.000 claims description 15
- 239000011734 sodium Substances 0.000 claims description 13
- 230000003647 oxidation Effects 0.000 claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- 230000005307 ferromagnetism Effects 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- -1 trifluoro octyl group trimethoxy silanes Chemical class 0.000 claims description 5
- GZBAUYZREARCNR-UHFFFAOYSA-N C(CCCCCCCCC)[Si](OC)(OC)OC.[F] Chemical compound C(CCCCCCCCC)[Si](OC)(OC)OC.[F] GZBAUYZREARCNR-UHFFFAOYSA-N 0.000 claims description 4
- ONFRHRVYLPVAMA-UHFFFAOYSA-N C(CCCCCCCCC)[Si](OCC)(OCC)OCC.[F] Chemical class C(CCCCCCCCC)[Si](OCC)(OCC)OCC.[F] ONFRHRVYLPVAMA-UHFFFAOYSA-N 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- 150000002688 maleic acid derivatives Chemical class 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 2
- BSYQEPMUPCBSBK-UHFFFAOYSA-N [F].[SiH4] Chemical compound [F].[SiH4] BSYQEPMUPCBSBK-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- 239000003960 organic solvent Substances 0.000 abstract description 9
- 230000007774 longterm Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 56
- 229940056319 ferrosoferric oxide Drugs 0.000 description 23
- 238000013019 agitation Methods 0.000 description 16
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 239000002105 nanoparticle Substances 0.000 description 10
- CMXPERZAMAQXSF-UHFFFAOYSA-M sodium;1,4-bis(2-ethylhexoxy)-1,4-dioxobutane-2-sulfonate;1,8-dihydroxyanthracene-9,10-dione Chemical compound [Na+].O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=CC=C2O.CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC CMXPERZAMAQXSF-UHFFFAOYSA-M 0.000 description 10
- 238000001035 drying Methods 0.000 description 9
- 238000003760 magnetic stirring Methods 0.000 description 9
- 238000010792 warming Methods 0.000 description 9
- 239000003643 water by type Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 5
- 150000004816 dichlorobenzenes Chemical class 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000006249 magnetic particle Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 4
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
- Silicon Compounds (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a kind of hydrophobic ferroferric oxide magnetic nano-particles and preparation method thereof.The present invention carries out silicic acid anhydride on ferroferric oxide magnetic nano-particles surface with silicon fluoride and TEOS, makes SiO on ferroferric oxide magnetic nano-particles Surface coating by one-step method2And long alkyl chain, finally give with hydrophobic ferroferric oxide magnetic nano-particles, the magnetic nano-particle can be scattered in organic solvent steadily in the long term, so that it is no longer restricted because insoluble in organic solvent in actual applications, the application field of ferroferric oxide magnetic nano-particles is expanded, improves its potential value.
Description
Technical field
The present invention relates to a kind of hydrophobic ferroferric oxide magnetic nano-particles and preparation method thereof, belong to nano material preparation
Technical field.
Background technology
The preparation method of ferroferric oxide magnetic nano-particles is simply various, and cheap, has received significant attention.
In the last few years, as that studies ferroferric oxide magnetic nano-particles deepens continuously, not only sent out its scientific meaning
Exhibition, also makes it in magnetic storage, magnetic recording, magnetic fluid material, nano-magnetic medicinal, electric wave absorption（It is stealthy）Many fields such as material
It is applied, while ferroferric oxide magnetic nano-particles also have wide practical use in biotechnology and medical domain.So
And because ferroferric oxide magnetic nano-particles particle diameter is small, specific surface area is big, itself has magnetic, this make its be easy to reunite with
Oxidation by air and because it is not easy to disperse in non-polar solven, this make it that its application is significantly limited.
Therefore, the surface of ferroferric oxide magnetic nano-particles is carried out into silicic acid anhydride to be particularly important.
The method for preparing the ferroferric oxide magnetic nano-particles being dispersed among in non-polar solution at present is usually to it
Surface modification is carried out, so that particle has different surfaces characteristic and functional group.Lin Benlan oleic acid is to the oxidation of nanometer four three
Fe nanometer particles carry out surface modification, and it is coated, and outer surface is formed protective layer and prevent particle aggregation, modified
Ferriferrous oxide nano-particle has lipophile（Referring to：Inorganic chemicals industry, 2006,38 (3)：19-21）, but after Coated with Oleic Acid
The stability of ferriferrous oxide nano-particle in organic solvent is bad, and can only be scattered in some specific organic solvents.
Also there is researcher by elder generation in ferroso-ferric oxide Surface coating inorganic material, then hydrophobization is carried out to it under high temperature nitrogen protection
Processing, the reaction use two-step method, and reaction is complicated cumbersome, and severe reaction conditions, and under needing in high temperature and thering is nitrogen to protect
Carry out, be not suitable for production amplification.
The content of the invention
The invention provides a kind of preparation method of hydrophobic ferroferric oxide magnetic nano-particles, i.e., by one-step method four
Fe 3 O magnetic nano-particle Surface coating SiO2And long alkyl chain, due to the presence of long alkyl chain, make its intermolecular long distance
Strengthen from repulsive force, be easy to disperse in non-polar solven；Solve in the prior art, ferroferric oxide magnetic nano-particles grain
Footpath is small, specific surface area is big, itself has magnetic, and is easy to reunion and oxidation by air, and is not easy in non-polar solven point
The defects of dissipating, has expanded the application of ferroferric oxide magnetic nano-particles significantly.
To achieve the above object of the invention, the technical solution adopted by the present invention is a kind of hydrophobic ferroferric oxide magnetic nano
The preparation method of particle, silicic acid anhydride specially is carried out to nano ferriferrous oxide with silicon fluoride and esters of silicon acis and obtains hydrophobic four
Fe 3 O magnetic nano-particle.
In above-mentioned technical proposal, the mol ratio of silicon fluoride and esters of silicon acis is 1: 10~100；Esters of silicon acis and the oxidation of nanometer four three
The mass ratio of iron is 1: 50~500.
In above-mentioned technical proposal, silicon fluoride be tridecafluoro-n-octyltriethoxysilane, ten trifluoro octyl group trimethoxy silanes,
17 fluorine decyl triethoxysilanes or 17 fluorine decyl trimethoxy silanes；The esters of silicon acis is tetraethyl orthosilicate
(TEOS), methyl silicate（TMOS）, tetrapropoxysilane (TPOS) etc..
In above-mentioned technical proposal, specific silicic acid anhydride is that nano ferriferrous oxide is scattered in deionized water, then
Add small molecular alcohol；Then ammoniacal liquor is added；Esters of silicon acis alcoholic solution is added after stirring；Then silicon fluoride alcoholic solution is added；Reaction
90~120 min, obtain hydrophobic ferroferric oxide magnetic nano-particles, wherein, the volumetric concentration of esters of silicon acis alcoholic solution for 1~
5%；The mass concentration of the silicon fluoride alcoholic solution is 1~3%；The mass concentration of the ammoniacal liquor is 25~28%.It is disclosed by the invention
It is complete that reaction time is beneficial to hydrophobic treatment reaction.
In preferable technical scheme, esters of silicon acis alcoholic solution and silicon fluoride alcoholic solution slowly drip by several times during dropwise addition
Add, all to be added portionwise, it is a collection of to be spaced addition in 4.5~5.5 minutes to add the 15%~20% of total amount for every batch of addition.This hair
In bright, esters of silicon acis and silicon fluoride are dispersed in ethanol solution, are made into the solution of low solubility, and esters of silicon acis alcoholic solution and silicon fluoride alcohol are molten
Liquid is slowly added dropwise by several times during dropwise addition, avoids processing material from easily reuniting, wrap up the defects of uneven.
In above-mentioned technical proposal, surface-hydrophobicized processing is carried out to nano ferriferrous oxide with silicon fluoride according to example below
Carry out：
Take the 1 ml nanometer Fe 3 O 4 magnetic particle aqueous solution（The mg of particle containing ferroso-ferric oxide 25）Add to 100 ml
Three-necked flask in, and add 20 ml ethanol, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 25% ammoniacal liquor,
Continue to stir 15 min, the ethanol solution that 5 ml contain 100 μ l TEOS is slowly added dropwise by several times afterwards, continue by several times after dripping
The ethanol solution of 5 ml 2wt% tridecafluoro-n-octyltriethoxysilanes is slowly added dropwise, reacts 90 min, obtains hydrophobic four oxidation three
Ferromagnetism nanometer particle.
Take the 1 ml nanometer Fe 3 O 4 magnetic particle aqueous solution（The mg of particle containing ferroso-ferric oxide 25）Add to 100 ml
Three-necked flask in, and add 20 ml ethanol, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 25% ammoniacal liquor,
Continue to stir 15 min, the ethanol solution that 5 ml contain 100 μ l TEOS is slowly added dropwise by several times afterwards, continues after dripping point
The secondary ethanol solution that 10 ml 1wt% tridecafluoro-n-octyltriethoxysilanes are slowly added dropwise, 90 min are reacted, obtain hydrophobic four oxygen
Change three ferromagnetism nanometer particles.
Take the 1 ml nanometer Fe 3 O 4 magnetic particle aqueous solution（The mg of particle containing ferroso-ferric oxide 25）Add to 100 ml
Three-necked flask in, and add 20 ml ethanol, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 28% ammoniacal liquor,
Continue to stir 15 min, the ethanol solution that 5 ml contain 200 μ l TMOS is slowly added dropwise by several times afterwards, continues after dripping point
The secondary ethanol solution that 10 ml 2wt% tridecafluoro-n-octyltriethoxysilanes are slowly added dropwise, 120 min are reacted, obtain hydrophobic four oxygen
Change three ferromagnetism nanometer particles.
Take the 1 ml nanometer Fe 3 O 4 magnetic particle aqueous solution（The mg of particle containing ferroso-ferric oxide 25）Add to 100 ml
Three-necked flask in, and add 20 ml ethanol, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 28% ammoniacal liquor,
Continue to stir 15min, the ethanol solution that 10 ml contain 200 μ l TEOS is slowly added dropwise by several times afterwards, continue by several times after dripping
The ethanol solution of 20ml 1wt% tridecafluoro-n-octyltriethoxysilanes is slowly added dropwise, reacts 120 min, obtains hydrophobic four oxidation
Three ferromagnetism nanometer particles.
Take the 1 ml nanometer Fe 3 O 4 magnetic nano-particle aqueous solution（The mg of particle containing ferroso-ferric oxide 25）Add extremely
In 100 ml three-necked flask, and 20 ml ethanol are added, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml's 28%
Ammoniacal liquor, continue to stir 15 min, the ethanol solution that 5 ml contain 100 μ l TEOS is slowly added dropwise by several times afterwards, drips follow-up
The ethanol solution of the trifluoro octyl group trimethoxy silanes of 5 ml 1wt% ten is slowly added dropwise in continuous gradation, reacts 90 min, obtains hydrophobic four
Fe 3 O magnetic nano-particle.
Take 1 ml nanometer Fe 3 O 4 magnetic nano-particle solutions（The mg of particle containing ferroso-ferric oxide 25）Add to 100
In ml three-necked flask, and 20 ml ethanol are added, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 28% ammonia
Water, continue to stir 15 min, the ethanol solution that 5 ml contain 100 μ l TPOS is slowly added dropwise by several times afterwards, continues after dripping
The ethanol solution of 10 ml 2wt% tridecafluoro-n-octyltriethoxysilanes is slowly added dropwise by several times, reacts 90 min, obtains hydrophobic four
Fe 3 O magnetic nano-particle.
Take 1 ml nanometer Fe 3 O 4 magnetic nano-particle solutions（The mg of particle containing ferroso-ferric oxide 25）Add to 100
In ml three-necked flask, and 20 ml ethanol are added, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 28% ammonia
Water, continue to stir 15 min, the ethanol solution that 10 ml contain 200 μ l TEOS is slowly added dropwise by several times afterwards, continues after dripping
The ethanol solution of the fluorine decyl triethoxysilanes of 10 ml 2wt% 17 is slowly added dropwise by several times, reacts 120 min, obtains hydrophobic four
Fe 3 O magnetic nano-particle.
Take 1 ml nanometer Fe 3 O 4 magnetic nano-particle solutions（The mg of particle containing ferroso-ferric oxide 25）Add to 100
In ml three-necked flask, and 20 ml ethanol are added, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 28% ammonia
Water, continue to stir 15 min, the ethanol solution that 5 ml contain 100 μ l TEOS is slowly added dropwise by several times afterwards, continues after dripping
The ethanol solution of the fluorine decyl trimethoxy silanes of 5 ml 1wt% 17 is slowly added dropwise by several times, reacts 90 min, obtains hydrophobic four oxygen
Change three ferromagnetism nanometer particles.
, will be poly- under stirring in above-mentioned technical proposal（4- styrene sulfonic acids-common maleic acid）Sodium salt is added in ethylene glycol；
Add FeCl3·6H2O and CH3CH2Na, obtain rufous liquid；Then rufous liquid is transferred in autoclave,
In 180~220 DEG C, 8~24 h are reacted, are subsequently cooled to room temperature；Reactant cleaned with ethanol and deionized water after by strong magnetic
The isolated average grain diameter of iron is 147 nm nano ferriferrous oxide.Wherein, gather（4- styrene sulfonic acids-common maleic acid）Sodium
Salt, FeCl3·6H2O and CH3CH2Na mass ratio is 1: 1.08: 3.
Such as：0.5 g PSSMA are weighed, under magnetic stirring, is added in 20 ml EG, stirs to be clarified
Solution, 0.54 g FeCl are added afterwards3·6H2O and 1.5 g CH3CH2Na, uniform rufous liquid is finally given, so
After be transferred in autoclave, and be placed in thermostatic drying chamber, be warming up to 200 DEG C, react 10 h, then cool down
Clean repeatedly to room temperature, and with ethanol and deionized water, separated by strong magnet, it is receiving for 167 nm to obtain average grain diameter
Rice ferroso-ferric oxide, is finally dispersed in 6 ml deionized waters.
The invention also discloses the hydrophobic ferroferric oxide magnetic nano-particles prepared according to above-mentioned preparation method；By nanometer
Ferroso-ferric oxide Surface coating SiO2Formed with long alkyl chain.
Hydrophobic ferroferric oxide magnetic nano-particles structure is as shown in Figure 8.
First passage one-step method of the present invention, is carried out at hydrophobization with silicon fluoride and esters of silicon acis on nano ferriferrous oxide surface
Reason, makes SiO on ferroferric oxide magnetic nano-particles Surface coating2And long alkyl chain, the hydrophobic ferroso-ferric oxide finally given
Magnetic nano-particle, it can be scattered in organic solvent steadily in the long term；The present invention can solve existing four oxygen only with one-step method
To change three ferromagnetism nanometer particles easily reunion and oxidation by air, and the defects of scattered is not easy in non-polar solven, method is simple,
Strong operability, reaction condition are gentle.The hydrophobic ferroferric oxide magnetic nano-particles being prepared by the present invention can be dispersed in
In organic solvent, such as：Acetone, toluene, dichloro-benzenes, dichloromethane, tetrahydrofuran, chloroform etc., so as to expand ferroso-ferric oxide
The application field of magnetic nano-particle, it is set no longer to be restricted in actual applications because insoluble in organic solvent.
Brief description of the drawings
Fig. 1 is the XRD of nano ferriferrous oxide prepared by embodiment one；
Fig. 2 is the SEM figures of hydrophobic ferriferrous oxide nano-particle prepared by embodiment one；
Fig. 3 is that hydrophobic ferroferric oxide magnetic nano-particles prepared by embodiment one disperse photo figure in non-polar solven
Fig. 4 is the SEM figures of hydrophobic ferriferrous oxide nano-particle prepared by embodiment two；
Fig. 5 is that hydrophobic ferroferric oxide magnetic nano-particles prepared by embodiment two disperse photo figure in non-polar solven；
Fig. 6 is the SEM figures of hydrophobic ferriferrous oxide nano-particle prepared by embodiment three；
Fig. 7 is that hydrophobic ferroferric oxide magnetic nano-particles prepared by embodiment three disperse photo figure in non-polar solven；
Fig. 8 is hydrophobic ferroferric oxide magnetic nano-particles structure.
Embodiment
Technical solution of the present invention is described in detail with reference to embodiments.
Embodiment one
（1）0.5 g PSSMA are weighed, under magnetic stirring, are added in 20 ml EG, are stirred molten to obtain clarifying
Liquid, 0.54 g FeCl are added afterwards3·6H2O and 1.5 g CH3CH2Na, uniform rufous liquid is finally given, then
It is transferred in autoclave, and is placed in thermostatic drying chamber, be warming up to 200 DEG C, reacts 10 h, be subsequently cooled to
Room temperature, and cleaned repeatedly with ethanol and deionized water, separated by strong magnet, be finally dispersed in 6 ml deionized waters
In, obtain the nano ferriferrous oxide aqueous solution；
（2）Take 1 ml steps（1）In obtained ferroferric oxide magnetic nano-particles solution add to three mouthfuls of 100 ml
In flask, and 20 ml ethanol are added, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 25% ammoniacal liquor, continue to stir
15 min are mixed, the ethanol solution that 5 ml contain 100 μ l TEOS is slowly added dropwise by several times afterwards, continue by several times slowly drop after dripping
Add the ethanol solution of 5 ml 2wt% tridecafluoro-n-octyltriethoxysilanes, react 90 min, obtain hydrophobic Fe 3 O 4 magnetic
Nano-particle.
Referring to accompanying drawing 1, for the XRD spectra of above-mentioned nano ferriferrous oxide, its XRD diffraction maximum is with ferroso-ferric oxide XRD's
Standard spectrogram is completely corresponding, and 9 diffraction maximums correspond to ferroso-ferric oxide respectively（111）、（220）、（311）、（222）、
（400）、（422）、（511）、（440）、（533）The diffraction maximum of crystal face, show to be prepared is strictly ferriferrous oxide nano
Particle.
Accompanying drawing 2 is the SEM figures of above-mentioned ferriferrous oxide nano-particle, it is known that, ferroso-ferric oxide particle is well dispersed and divides
Cloth is uniform, and average grain diameter is 170 nm.
Fig. 3 is that above-mentioned hydrophobic ferroferric oxide magnetic nano-particles disperse photo figure in non-polar solven；Wherein Fig. 3 a are
Hydrophobic ferroferric oxide magnetic nano-particles are in dichloro-benzenes is scattered in；Fig. 3 b are hydrophobic ferroferric oxide magnetic nano-particles point
Dissipate in lower floor's dichloro-benzenes, upper strata is deionized water；Understand to pass through four oxidations after silicic acid anhydride of the present invention from these figures
Three-iron has excellent hydrophobic effect.
Embodiment two
（1）0.5 g PSSMA are weighed, under magnetic stirring, are added in 20 ml EG, are stirred molten to obtain clarifying
Liquid, 0.54 g FeCl are added afterwards3·6H2O and 1.5 g CH3CH2Na, uniform rufous liquid is finally given, then
It is transferred in autoclave, and is placed in thermostatic drying chamber, be warming up to 200 DEG C, reacts 10 h, be subsequently cooled to
Room temperature, and cleaned repeatedly with ethanol and deionized water, separated by strong magnet, be finally dispersed in 6 ml deionized waters
In；
（2）Take 1 ml steps（1）In obtained ferroferric oxide magnetic nano-particles solution add to three mouthfuls of 100 ml
In flask, and 20 ml ethanol are added, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 25% ammoniacal liquor, continue to stir
15 min are mixed, the ethanol solution that 5 ml contain 100 μ l TEOS is slowly added dropwise by several times afterwards, are continued after dripping slow by several times
The ethanol solution of 10 ml 1wt% tridecafluoro-n-octyltriethoxysilanes is added dropwise, reacts 90 min, obtains hydrophobic ferroso-ferric oxide
Magnetic nano-particle.
Accompanying drawing 4 is schemed for the SEM of above-mentioned ferriferrous oxide nano-particle, it is known that, ferroso-ferric oxide particle is well dispersed and divides
Cloth is uniform, and average grain diameter is 152 nm.
Fig. 5 is that above-mentioned hydrophobic ferroferric oxide magnetic nano-particles disperse photo figure in non-polar solven；Wherein；Fig. 5 a are
Hydrophobic ferroferric oxide magnetic nano-particles are scattered in upper toluene, and lower floor is deionized water；Fig. 5 b are hydrophobic four oxidations three
Ferromagnetism nanometer particle is scattered in lower floor's dichloro-benzenes, upper toluene, and intermediate layer is deionized water.
Embodiment three
（1）0.5 g PSSMA are weighed, under magnetic stirring, are added in 20 ml EG, are stirred molten to obtain clarifying
Liquid, 0.54 g FeCl are added afterwards3·6H2O and 1.5 g CH3CH2Na, uniform rufous liquid is finally given, then
It is transferred in autoclave, and is placed in thermostatic drying chamber, be warming up to 200 DEG C, reacts 10 h, be subsequently cooled to
Room temperature, and cleaned repeatedly with ethanol and deionized water, separated by strong magnet, be finally dispersed in 6 ml deionized waters
In；
（2）Take 1 ml steps（1）In obtained ferroferric oxide magnetic nano-particles solution add to three mouthfuls of 100 ml
In flask, and 20 ml ethanol are added, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 28% ammoniacal liquor, continue to stir
15 min are mixed, the ethanol solution that 5 ml contain 200 μ l TMOS is slowly added dropwise by several times afterwards, continue by several times slowly drop after dripping
Add the ethanol solution of the wt% tridecafluoro-n-octyltriethoxysilanes of 10 ml 2, react 120 min, obtain hydrophobic ferroso-ferric oxide
Magnetic nano-particle.
Accompanying drawing 6 is schemed for the SEM of above-mentioned ferriferrous oxide nano-particle, it is known that, ferroso-ferric oxide particle is well dispersed and divides
Cloth is uniform, and average grain diameter is 172 nm.
Fig. 7 is that above-mentioned hydrophobic ferroferric oxide magnetic nano-particles disperse photo figure in non-polar solven；Wherein Fig. 7 a are
Hydrophobic ferroferric oxide magnetic nano-particles are in tetrahydrofuran is scattered in；Fig. 7 b are hydrophobic ferroferric oxide magnetic nano-particles
In chloroform is scattered in.
Example IV
（1）0.5 g PSSMA are weighed, under magnetic stirring, are added in 20 ml EG, are stirred molten to obtain clarifying
Liquid, 0.54 g FeCl are added afterwards3·6H2O and 1.5 g CH3CH2Na, uniform rufous liquid is finally given, then
It is transferred in autoclave, and is placed in thermostatic drying chamber, be warming up to 200 DEG C, reacts 10 h, be subsequently cooled to
Room temperature, and cleaned repeatedly with ethanol and deionized water, separated by strong magnet, be finally dispersed in 6 ml deionized waters
In；
（2）Take 1 ml steps（1）In obtained ferroferric oxide magnetic nano-particles solution add to three mouthfuls of 100 ml
In flask, and 20 ml ethanol are added, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 28% ammoniacal liquor, continue to stir
15 min are mixed, the ethanol solution that 10 ml contain 200 μ l TEOS is slowly added dropwise by several times afterwards, are continued after dripping slow by several times
The ethanol solution of 10 ml 2wt% tridecafluoro-n-octyltriethoxysilanes is added dropwise, reacts 120 min, obtains hydrophobic ferroso-ferric oxide
Magnetic nano-particle.
Embodiment five
（1）0.5 g PSSMA are weighed, under magnetic stirring, are added in 20 ml EG, are stirred molten to obtain clarifying
Liquid, 0.54 g FeCl are added afterwards3·6H2O and 1.5 g CH3CH2Na, uniform rufous liquid is finally given, then
It is transferred in autoclave, and is placed in thermostatic drying chamber, be warming up to 200 DEG C, reacts 10 h, be subsequently cooled to
Room temperature, and cleaned repeatedly with ethanol and deionized water, separated by strong magnet, be finally dispersed in 6 ml deionized waters
In；
（2）Take 1 ml steps（1）In obtained ferroferric oxide magnetic nano-particles solution add to three mouthfuls of 100 ml
In flask, and 20 ml ethanol are added, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 28% ammoniacal liquor, continue to stir
15 min are mixed, the ethanol solution that 5 ml contain 100 μ l TEOS is slowly added dropwise by several times afterwards, continue by several times slowly drop after dripping
Add the ethanol solution of the trifluoro octyl group trimethoxy silanes of 5 ml 1wt% ten, react 90 min, obtain hydrophobic Fe 3 O 4 magnetic
Nano-particle.
Embodiment six
（1）0.5 g PSSMA are weighed, under magnetic stirring, are added in 20 ml EG, are stirred molten to obtain clarifying
Liquid, 0.54 g FeCl are added afterwards3·6H2O and 1.5 g CH3CH2Na, uniform rufous liquid is finally given, then
It is transferred in autoclave, and is placed in thermostatic drying chamber, be warming up to 200 DEG C, reacts 10 h, be subsequently cooled to
Room temperature, and cleaned repeatedly with ethanol and deionized water, separated by strong magnet, be finally dispersed in 6 ml deionized waters
In；
（2）Take 1 ml steps（1）In obtained ferroferric oxide magnetic nano-particles solution add to three mouthfuls of 100 ml
In flask, and 20 ml ethanol are added, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 28% ammoniacal liquor, continue to stir
15 min are mixed, the ethanol solution that 5 ml contain 100 μ l TPOS is slowly added dropwise by several times afterwards, are continued after dripping slow by several times
The ethanol solution of 10 ml 1wt% tridecafluoro-n-octyltriethoxysilanes is added dropwise, reacts 90 min, obtains hydrophobic ferroso-ferric oxide
Magnetic nano-particle.
Embodiment seven
（1）0.5 g PSSMA are weighed, under magnetic stirring, are added in 20 ml EG, are stirred molten to obtain clarifying
Liquid, 0.54 g FeCl are added afterwards3·6H2O and 1.5 g CH3CH2Na, uniform rufous liquid is finally given, then
It is transferred in autoclave, and is placed in thermostatic drying chamber, be warming up to 200 DEG C, reacts 10 h, be subsequently cooled to
Room temperature, and cleaned repeatedly with ethanol and deionized water, separated by strong magnet, be finally dispersed in 6 ml deionized waters
In；
（2）Take 1 ml steps（1）In obtained ferroferric oxide magnetic nano-particles solution add to three mouthfuls of 100 ml
In flask, and 20 ml ethanol are added, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 28% ammoniacal liquor, continue to stir
15 min are mixed, the ethanol solution that 10 ml contain 200 μ l TEOS is slowly added dropwise by several times afterwards, are continued after dripping slow by several times
The ethanol solution of the fluorine decyl triethoxysilanes of 10 ml 2wt% 17 is added dropwise, reacts 120 min, obtains hydrophobic ferroso-ferric oxide
Magnetic nano-particle.
Embodiment eight
（1）0.5 g PSSMA are weighed, under magnetic stirring, are added in 20 ml EG, are stirred molten to obtain clarifying
Liquid, 0.54 g FeCl are added afterwards3·6H2O and 1.5 g CH3CH2Na, uniform rufous liquid is finally given, then
It is transferred in autoclave, and is placed in thermostatic drying chamber, be warming up to 200 DEG C, reacts 10 h, be subsequently cooled to
Room temperature, and cleaned repeatedly with ethanol and deionized water, separated by strong magnet, be finally dispersed in 6 ml deionized waters
In；
（2）Take 1 ml steps（1）In obtained ferroferric oxide magnetic nano-particles solution add to three mouthfuls of 100 ml
In flask, and 20 ml ethanol are added, the min of mechanical agitation 15, after being uniformly dispersed, add 1 ml 28% ammoniacal liquor, continue to stir
15 min are mixed, the ethanol solution that 5 ml contain 100 μ l TEOS is slowly added dropwise by several times afterwards, continue by several times slowly drop after dripping
Add the ethanol solution of the fluorine decyl trimethoxy silanes of 5 ml 1wt% 17, react 90 min, obtain hydrophobic Fe 3 O 4 magnetic
Nano-particle.
To sum up it can be found that the present invention by one-step method by esters of silicon acis, silicon fluoride and ferroferric oxide magnetic nano-particles
Reaction, finally makes its Surface coating SiO2And long alkyl chain, so that the ferroferric oxide magnetic nano-particles have hydrophobicity.
One-step method of the present invention is simple to operate, less demanding to reaction condition, without high temperature anoxybiotic.It is prepared by the present invention hydrophobic
Ferroferric oxide magnetic nano-particles are dispersible and are stable in the presence of in organic solvent, such as：Acetone, toluene, dichloro-benzenes, dichloromethane
Alkane etc., so that it is no longer restricted because insoluble in organic solvent in actual applications, expand Fe 3 O 4 magnetic
The application field of nano-particle, improve its potential value.
Claims (5)
- A kind of 1. preparation method of hydrophobic ferroferric oxide magnetic nano-particles, it is characterised in that：With silicon fluoride and esters of silicon acis pair Nano ferriferrous oxide carries out silicic acid anhydride and obtains hydrophobic ferroferric oxide magnetic nano-particles；The silicon fluoride and esters of silicon acis Mol ratio be 1: 10~100；The mass ratio of esters of silicon acis and nano ferriferrous oxide is 1: 50~500；Nanometer four is aoxidized three Iron is scattered in deionized water, adds small molecular alcohol；Then ammoniacal liquor is added；Esters of silicon acis alcoholic solution is added after stirring；Then again Add silicon fluoride alcoholic solution；90~120 min are reacted, obtain hydrophobic ferroferric oxide magnetic nano-particles；Esters of silicon acis alcoholic solution Feed postition to be added portionwise, every batch of addition is that esters of silicon acis alcoholic solution adds the 15%~20% of total amount, interval 4.5~5.5 Minute adds a collection of；For the feed postition of silicon fluoride alcoholic solution to be added portionwise, every batch of addition is that esters of silicon acis alcoholic solution adds always The 15%~20% of amount, it is a collection of to be spaced addition in 4.5~5.5 minutes；The volumetric concentration of the esters of silicon acis alcoholic solution is 1~5%；It is described The mass concentration of silicon fluoride alcoholic solution is 1~3%；The mass concentration of the ammoniacal liquor is 25~28%.
- 2. the preparation method of hydrophobic ferroferric oxide magnetic nano-particles according to claim 1, it is characterised in that：The fluorine Silane be tridecafluoro-n-octyltriethoxysilane, ten trifluoro octyl group trimethoxy silanes, 17 fluorine decyl triethoxysilanes or The fluorine decyl trimethoxy silane of person 17；The esters of silicon acis is tetraethyl orthosilicate.
- 3. the preparation method of hydrophobic ferroferric oxide magnetic nano-particles according to claim 1, it is characterised in that：Stirring Under, will be poly-（4- styrene sulfonic acids-common maleic acid）Sodium salt is added in ethylene glycol；Add FeCl3·6H2O and CH3CH2Na, Obtain rufous liquid；Then rufous liquid is transferred in autoclave, in 180~220 DEG C, reacts 8~24 h, so After be cooled to room temperature；Reactant clean with ethanol and deionized water after by the isolated average grain diameter of strong magnet for 147 nm's Nano ferriferrous oxide；It is described poly-（4- styrene sulfonic acids-common maleic acid）Sodium salt, FeCl3·6H2O and CH3CH2Na mass ratio For 1: 1.08: 3.
- 4. prepared by the preparation method of any one hydrophobic ferroferric oxide magnetic nano-particles according to claims 1 to 3 Hydrophobic ferroferric oxide magnetic nano-particles.
- 5. hydrophobic ferroferric oxide magnetic nano-particles according to claim 4, it is characterised in that：Hydrophobic four oxidation three Ferromagnetism nanometer particle is by nano ferriferrous oxide Surface coating SiO2Formed with long alkyl chain.
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