CN108190967A - A kind of ferroferric oxide nano-piece and preparation method thereof - Google Patents
A kind of ferroferric oxide nano-piece and preparation method thereof Download PDFInfo
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- CN108190967A CN108190967A CN201810067947.2A CN201810067947A CN108190967A CN 108190967 A CN108190967 A CN 108190967A CN 201810067947 A CN201810067947 A CN 201810067947A CN 108190967 A CN108190967 A CN 108190967A
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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 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 27
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 18
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000012153 distilled water Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 7
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000003599 detergent Substances 0.000 claims abstract description 6
- 235000019441 ethanol Nutrition 0.000 claims abstract description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims description 14
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 12
- 229940056319 ferrosoferric oxide Drugs 0.000 claims description 9
- 229920002538 Polyethylene Glycol 20000 Polymers 0.000 claims description 5
- 229920002594 Polyethylene Glycol 8000 Polymers 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 5
- 239000003814 drug Substances 0.000 abstract description 4
- 229940079593 drug Drugs 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 3
- 230000008685 targeting Effects 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- KEAYESYHFKHZAL-OUBTZVSYSA-N sodium-24 Chemical group [24Na] KEAYESYHFKHZAL-OUBTZVSYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 15
- 239000000047 product Substances 0.000 description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 229910001447 ferric ion Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 244000131522 Citrus pyriformis Species 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000006399 behavior Effects 0.000 description 2
- 229910001448 ferrous ion Inorganic materials 0.000 description 2
- 150000002505 iron Chemical class 0.000 description 2
- 239000006249 magnetic particle Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- -1 iron ion Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000002595 magnetic resonance imaging Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000000015 thermotherapy Methods 0.000 description 1
- 238000012795 verification Methods 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
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention belongs to field of nano material preparation and disclose a kind of ferroferric oxide nano-piece and preparation method thereof；The thickness of the ferroferric oxide nano-piece is between 50 120nm ranges, and diameter is between 300 650nm ranges；Preparation method includes：First, 8 12 parts of ferric trichloride, 46 parts of frerrous chloride, 8 12 parts of sodium bicarbonate and 24 parts of citric acid is taken to be added in 100 200 parts of distilled water；2nd, the 59 parts of surfactants stirring continuously added；3rd, solution is put into reaction kettle, hydro-thermal keeps the temperature 8 12h, and temperature is controlled under the conditions of 100 140 DEG C；4th, by the use of ethyl alcohol and/or distilled water as detergent, 7 10min are washed；5th, product is dried to get to the ferroferric oxide nano-piece.The method of the present invention is simple and practicable, and obtained product purity is high, crystal habit is stablized, and has superior magnetic behavior and biological safety, has important application prospect in terms of magnetic storage, drug targeting guiding, magnetic multifunctional composite and bioengineering.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, and in particular to a kind of ferroferric oxide nano-piece and its preparation side
Method.
Background technology
Ferroso-ferric oxide belongs to cubic system, inverse spinel structure, and ferroferric oxide nano-piece material is with excellent
Magnetism characteristic makes it in magnetic memory materials, microwave absorption, sapecial coating, drug targeting guiding, magnetic multifunctional composite, urges
Agent and bioengineering etc. have important application.Especially the storage density of magnetic memory materials improves rapidly in recent years, magnetic
The superparamagnetic response of property material receives the especially concern of people.Meanwhile ferroso-ferric oxide of the synthesis with biological safety
Nanometer sheet material is because it is in the wide application of the biomedical sectors such as cell separation, targeted drug, magnetic resonance imaging and magnetic thermotherapy
Prospect and one of as research hotspot.Influence nanoscale ferroso-ferric oxide performance principal element include superparamagnetism, coercivity,
Magnetic saturation amount, crystallinity and grain size and pattern etc., known today is that preparation method has its performance and suitable application area
Very tremendous influence.
Method currently used for preparing ferroferric oxide nano-piece mainly has physical method and chemical method, using physics side
Method prepare nanometer sheet common product purity is low, nanometer sheet is unevenly distributed, especially high, Er Qiesheng is required to Preparation equipment sometimes
The ferroferric oxide nano-piece of production is easily oxidized, and pattern is also inhomogenous；People are also using various chemical methodes, such as liquid at present
Phase sedimentation, hydro-thermal method, solvent-thermal method, microemulsion method, sol-gal process, metal-organic precursors thermal decomposition method, electrostatic spinning
Method etc..Wherein liquid-phase precipitation method when prepare a kind of most commonly used method of ferriferrous oxide nanometer material at present, typically with
Divalent iron salt and trivalent iron salt carry out precipitation system according to 1: 2 ratio wiring solution-forming using sodium hydroxide, potassium hydroxide, ammonium hydroxide etc.
.However in preparation process, make the ratio of reaction since ferrous ion is easily oxidized to ferric ion in air
It changes.Meanwhile strong base solution (such as sodium hydroxide) adds in the hydrolysate that part iron ion is had in mixing salt solution
Generation, is unfavorable for the preparation of magnetic-particle.And be easy to reunite by magnetic particles of ferroferric oxide prepared by the above method, it is brilliant
Volume morphing is bad, and technical process is difficult to control.Therefore it is restricted, can not be widely applied in actually mass producing.
Given this how to provide that a kind of crystal habit is good, the simple easily controllable, nano particle of technical process is not easy to reunite and performance is stablized
Ferroferric oxide nano-piece and preparation method thereof be those skilled in the art's technical issues that need to address.
Invention content
The present invention is bad for preparation process complexity, crystal habit in existent technique, is unfavorable for large-scale production
Problem, and a kind of ferroferric oxide nano-piece and preparation method thereof is provided.
The present invention using following technical scheme in order to solve the above technical problems, realized：
Design a kind of ferroferric oxide nano-piece, the thickness of the ferroferric oxide nano-piece 50-120nm ranges it
Between, diameter is between 300-650nm ranges.
A kind of preparation method of ferroferric oxide nano-piece is designed, this method comprises the following steps：
Step 1：Take the ferric trichloride, 4-6 parts of frerrous chloride, 8-12 parts of sodium bicarbonate that mass fraction is 8-12 parts
Citric acid with 2-4 parts is added in 100-200 parts of distilled water；
Step 2：5-9 part surfactants of mass fraction are continuously added in 200- in the solution of step 1 configuration
Stir 4-10 minutes under 400rpm rotating speeds, for use；
Step 3：Solution obtained by step 2 is put into reaction kettle, hydro-thermal heat preservation 8-12h, solution in reaction process
Temperature control under the conditions of 100-140 DEG C；
Step 4：Using the ethyl alcohol of the product obtained by step 3 and/or distilled water as detergent, existed by centrifuge
Centrifuge washing 7-10min under 4000-8000rpm rotating speeds；
Step 5：By the product obtained by step 4, dry 2-5h aoxidizes three to get to described four at a temperature of 30-50 DEG C
Iron nanometer sheet.
Preferably, the surfactant includes polyethylene glycol and cetyl trimethylammonium bromide, the poly- second
The mass fraction of glycol is 4-6 parts, and the mass fraction of the cetyl trimethylammonium bromide is 1-3 parts.
Preferably, the polyethylene glycol includes PEG8000, PFG10000 and PEG20000.
Preferably, the mass fraction of the step tetraethoxide is 75%-90%.
A kind of ferroferric oxide nano-piece proposed by the present invention and preparation method thereof, advantageous effect is：
(1) the ferroferric oxide nano-piece purity that the method for the present invention obtains is high, and size is uniform, distribution is concentrated, pattern
Similarity is high, convenient for industrialized production；
(2) the method for the present invention is simple for process, preparation time is no more than 18 hours, when shortening preparation compared with prior art
Between, and substitute strong base solution in the prior art with sodium bicarbonate and add citric acid and inhibit ferric ion as reducing agent
Hydrolysis so that ferrous ion and ferric ion keep optimal ratio, prepared ferriferrous oxide nano
The magnetic behavior of piece has significant improvement compared with the prior art；
(3) polyethylene glycol and cetyl trimethylammonium bromide are used in the method for the present invention as surfactant, a side
Face polyethylene glycol and cetyl trimethylammonium bromide effectively reduce product agglomeration, enhancing dispersibility, on the other hand by
As polymer there is stable cross-linked structure in polyethylene glycol, form micro- reative cell coated ferroferric oxide nano material, obtain
The ferroferric oxide nano-piece form stable arrived, size is uniform, distribution is concentrated；
(4) the obtained ferroferric oxide nano-piece crystal habit of the method for the present invention is stablized, and has superior magnetic behavior
And biological safety, there is important answer in terms of magnetic storage, drug targeting guiding, magnetic multifunctional composite and bioengineering
Use prospect.
Description of the drawings
The present invention is described in further detail for embodiment in below in conjunction with the accompanying drawings, but does not form to the present invention's
Any restrictions.
Fig. 1 is the X-ray diffraction spectrogram of ferroferric oxide nano-piece that embodiment 2 obtains；
Fig. 2 and Fig. 3 is scanning electron microscope under the ferroferric oxide nano-piece different amplification that embodiment 2 obtains
(SEM) picture.
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.
Embodiment one
A kind of ferroferric oxide nano-piece of the present invention, the thickness of the ferroferric oxide nano-piece are 50nm, diameter
For 300nm.
A kind of preparation method of ferroferric oxide nano-piece of the present invention, this method comprises the following steps：
Step 1：Take ferric trichloride, 4 parts of frerrous chloride, 8 parts of sodium bicarbonate and 2 parts of the lemon that mass fraction is 8 parts
Lemon acid is added in 100 parts of distilled water；
Step 2：5 parts of surfactants that mass fraction is continuously added in the solution of step 1 configuration turn in 200rpm
The lower stirring of speed 10 minutes, for use；The surfactant includes polyethylene glycol and cetyl trimethylammonium bromide, described
The mass fraction of polyethylene glycol is 4 parts, and the mass fraction of the cetyl trimethylammonium bromide is 1 part；The poly- second
Glycol includes PEG8000, PFG10000 and PEG20000.
Step 3：Solution obtained by step 2 is put into reaction kettle, hydro-thermal heat preservation 8h, the temperature of solution in reaction process
Degree control is under the conditions of 140 DEG C；
Step 4：Using the ethyl alcohol of the product obtained by step 3 and/or distilled water as detergent, existed by centrifuge
Centrifuge washing 10min under 4000rpm rotating speeds, the mass fraction of the step tetraethoxide is 75%；
Step 5：By the product obtained by step 4, dry 5h receives to get to the ferroso-ferric oxide at a temperature of 30 DEG C
Rice piece.
Embodiment two
A kind of ferroferric oxide nano-piece of the present invention, the thickness of the ferroferric oxide nano-piece are 85nm, diameter
For 475nm.
A kind of preparation method of ferroferric oxide nano-piece of the present invention, this method comprises the following steps：
Step 1：Take ferric trichloride, 5 parts of frerrous chloride that mass fraction is 10 parts, 10 parts of sodium bicarbonate and 3 parts
Citric acid is added in 150 parts of distilled water；
Step 2：7 parts of surfactants that mass fraction is continuously added in the solution of step 1 configuration turn in 300rpm
The lower stirring of speed 7 minutes, for use；The surfactant includes polyethylene glycol and cetyl trimethylammonium bromide, described
The mass fraction of polyethylene glycol is 5 parts, and the mass fraction of the cetyl trimethylammonium bromide is 2 parts；The poly- second
Glycol includes PEG8000, PFG10000 and PEG20000.
Step 3：Solution obtained by step 2 is put into reaction kettle, hydro-thermal heat preservation 10h, solution in reaction process
Temperature is controlled under the conditions of 120 DEG C；
Step 4：Using the ethyl alcohol of the product obtained by step 3 and/or distilled water as detergent, existed by centrifuge
Centrifuge washing 9min under 6000rpm rotating speeds, the mass fraction of the step tetraethoxide is 85%；
Step 5：By the product obtained by step 4 at a temperature of 40 DEG C dry 3.5h to get to the ferroso-ferric oxide
Nanometer sheet.
Embodiment three
A kind of ferroferric oxide nano-piece of the present invention, the thickness of the ferroferric oxide nano-piece are 120nm, diameter
For 650nm.
A kind of preparation method of ferroferric oxide nano-piece of the present invention, this method comprises the following steps：
Step 1：Take ferric trichloride, 6 parts of frerrous chloride that mass fraction is 12 parts, 12 parts of sodium bicarbonate and 4 parts
Citric acid is added in 200 parts of distilled water；
Step 2：9 parts of surfactants that mass fraction is continuously added in the solution of step 1 configuration turn in 400rpm
The lower stirring of speed 4 minutes, for use；The surfactant includes polyethylene glycol and cetyl trimethylammonium bromide, described
The mass fraction of polyethylene glycol is 6 parts, and the mass fraction of the cetyl trimethylammonium bromide is 3 parts；The poly- second
Glycol includes PEG8000, PFG10000 and PEG20000.
Step 3：Solution obtained by step 2 is put into reaction kettle, hydro-thermal heat preservation 12h, solution in reaction process
Temperature is controlled under the conditions of 100 DEG C；
Step 4：Using the ethyl alcohol of the product obtained by step 3 and/or distilled water as detergent, existed by centrifuge
Centrifuge washing 7min under 8000rpm rotating speeds, the mass fraction of the step tetraethoxide is 90%；
Step 5：By the product obtained by step 4, dry 2h receives to get to the ferroso-ferric oxide at a temperature of 50 DEG C
Rice piece.
Experimental verification：
Refering to shown in attached drawing 1, sample is made in 2 obtained ferroferric oxide nano-piece of embodiment and passes through X-ray diffraction
Instrument measures its X ray diffracting spectrum, the characteristic peak in diffracting spectrum and standard diffraction collection of illustrative plates (Fe3O4PDF76-1849 peak value)
It coincide, the main component for illustrating product is ferroso-ferric oxide.
Refering to shown in attached drawing 2 and attached drawing 3, sample is made by sweeping in 3 obtained ferroferric oxide nano-piece of embodiment
Electron microscope scanning is retouched, obtains the SEM figures under 48000 times and 96000 times.From scanning result：First, four oxidation in sample
Three-iron nanometer sheet purity is close to 100%, and size is uniform, and well-tended appearance rate is high, crystal habit is stablized；2nd, ferroso-ferric oxide
The thickness of nanometer sheet is concentrated in 120nm or so, diameter in 650nm or so, Size Distribution, and pattern is laminated structure.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of ferroferric oxide nano-piece, which is characterized in that the thickness of the ferroferric oxide nano-piece is in 50-120nm
Between range, diameter is between 300-650nm ranges.
2. a kind of preparation method of ferroferric oxide nano-piece as described in claim 1, which is characterized in that this method is included such as
Lower step：
Step 1：Take the ferric trichloride, 4-6 parts of frerrous chloride, 8-12 parts of sodium bicarbonate and 2-4 that mass fraction is 8-12 parts
The citric acid of part is added in 100-200 parts of distilled water；
Step 2：5-9 part surfactants of mass fraction are continuously added in 200-400rpm in the solution of step 1 configuration
Stir 4-10 minutes under rotating speed, for use；
Step 3：Solution obtained by step 2 is put into reaction kettle, hydro-thermal heat preservation 8-12h, the temperature of solution in reaction process
Degree control is under the conditions of 100-140 DEG C；
Step 4：Using the ethyl alcohol of the product obtained by step 3 and/or distilled water as detergent, by centrifuge in 4000-
Centrifuge washing 7-10min under 8000rpm rotating speeds；
Step 5：By the product obtained by step 4, dry 2-5h receives to get to the ferroso-ferric oxide at a temperature of 30-50 DEG C
Rice piece.
A kind of 3. preparation method of ferroferric oxide nano-piece according to claim 2, which is characterized in that the surface
Activating agent includes polyethylene glycol and cetyl trimethylammonium bromide, and the mass fraction of the polyethylene glycol is 4-6 parts, described
Cetyl trimethylammonium bromide mass fraction be 1-3 parts.
4. the preparation method of a kind of ferroferric oxide nano-piece according to Claims 2 or 3, which is characterized in that described
Polyethylene glycol includes PEG8000, PFG10000 and PEG20000.
5. the preparation method of a kind of ferroferric oxide nano-piece according to Claims 2 or 3, which is characterized in that described
The mass fraction of step tetraethoxide is 75%-90%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113866136A (en) * | 2021-06-16 | 2021-12-31 | 江苏科技大学 | Method for detecting antibiotics through solvent-free single-drop magnetic enrichment-dispersion solid phase extraction method |
| CN114524463A (en) * | 2022-03-18 | 2022-05-24 | 中南大学 | Super-large-size high-length-diameter-ratio ferroferric oxide two-dimensional nanosheet and preparation method thereof |
| CN115028206A (en) * | 2022-06-21 | 2022-09-09 | 中海石油(中国)有限公司 | Janus two-dimensional magnetic nanoparticle and preparation method and application thereof |
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| CN102992408A (en) * | 2013-01-07 | 2013-03-27 | 江苏大学 | Preparation method of ferroferric oxide magnetic nanocrystal |
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| CN113866136A (en) * | 2021-06-16 | 2021-12-31 | 江苏科技大学 | Method for detecting antibiotics through solvent-free single-drop magnetic enrichment-dispersion solid phase extraction method |
| CN114524463A (en) * | 2022-03-18 | 2022-05-24 | 中南大学 | Super-large-size high-length-diameter-ratio ferroferric oxide two-dimensional nanosheet and preparation method thereof |
| CN114524463B (en) * | 2022-03-18 | 2023-05-26 | 中南大学 | Super-large-size high-length-diameter-ratio ferroferric oxide two-dimensional nano sheet and preparation method thereof |
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| CN115028206B (en) * | 2022-06-21 | 2023-10-31 | 中海石油(中国)有限公司 | Janus two-dimensional magnetic nanoparticle and preparation method and application thereof |
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