CN105883934A - Method for preparing water-soluble superparamagnetic Fe3O4 hollow spheres - Google Patents
Method for preparing water-soluble superparamagnetic Fe3O4 hollow spheres Download PDFInfo
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- CN105883934A CN105883934A CN201610242802.2A CN201610242802A CN105883934A CN 105883934 A CN105883934 A CN 105883934A CN 201610242802 A CN201610242802 A CN 201610242802A CN 105883934 A CN105883934 A CN 105883934A
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- hollow ball
- fe3o4
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- hollow spheres
- spio
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title abstract description 24
- 238000000034 method Methods 0.000 title abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 10
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 10
- 150000002505 iron Chemical class 0.000 claims description 10
- 235000017281 sodium acetate Nutrition 0.000 claims description 10
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 10
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 8
- 241000399119 Spio Species 0.000 claims description 8
- 239000001632 sodium acetate Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- BDKLKNJTMLIAFE-UHFFFAOYSA-N 2-(3-fluorophenyl)-1,3-oxazole-4-carbaldehyde Chemical group FC1=CC=CC(C=2OC=C(C=O)N=2)=C1 BDKLKNJTMLIAFE-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical group O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 2
- 229940087562 sodium acetate trihydrate Drugs 0.000 claims description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 238000004729 solvothermal method Methods 0.000 abstract 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000008204 material by function Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000013019 agitation Methods 0.000 description 6
- 239000002243 precursor Substances 0.000 description 6
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 3
- 229950000845 politef Drugs 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- KVIPHDKUOLVVQN-UHFFFAOYSA-N ethene;hydrate Chemical compound O.C=C KVIPHDKUOLVVQN-UHFFFAOYSA-N 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000001228 spectrum 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]
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- 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
- C01P2006/32—Thermal properties
- C01P2006/33—Phase transition temperatures
- C01P2006/34—Melting temperatures
-
- 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
- C01P2006/42—Magnetic properties
Abstract
The invention discloses a method for preparing water-soluble superparamagnetic Fe3O4 hollow spheres, belongs to the field of nano functional materials and solves the problem of poor water solubility caused during preparation of Fe3O4 hollow spheres with a solvothermal method. A small amount of lauryl sodium sulfate is added on the basis of an existing solvothermal method for synthesis of Fe3O4, so that the prepared Fe3O4 hollow spheres have very good water solubility; the method is simple to operate and low in cost and facilitates large-scale production; the synthesized Fe3O4 hollow spheres show superparamagnetism, and accordingly, the value of the water-soluble superparamagnetic Fe3O4 hollow spheres in the aspect of biological application is also increased.
Description
Technical field
The invention belongs to nano-functional material technical field.
Background technology
Fe3O4Magnetic Nano material, due to structure and the performance of its uniqueness, is all with a wide range of applications in many fields,
Especially at biology, medical treatment etc. field attract wide attention especially.Fe at numerous different-shapes3O4In nano material, Fe3O4
It is low that hollow ball has density, and specific surface is big, and the magnetic performance that stability is high and outstanding, it is special to have at drug delivery art
Application prospect.Fe3O4The preparation method of hollow ball is more, wherein uses solvent-thermal method to prepare Fe3O4Hollow ball is rather extensive, but
Introducing due to organic solvent, it will usually cause Fe3O4Hollow ball water solublity is poor, limits its application at biological field, and
And it is longer to prepare required time, cost is high, is unfavorable for large-scale production.
Summary of the invention
Fe is prepared in order to solve solvent-thermal method3O4The problem of the poorly water-soluble that hollow ball causes, the invention provides a kind of water solublity
The preparation method of SPIO hollow ball, concrete grammar is as follows:
1) trivalent iron salt is added stirring and dissolving in ethylene glycol solution；
2) add sodium acetate, be uniformly mixed；
3) add sodium lauryl sulphate (SDS), be uniformly mixed；
4) by step 3) in gained mixed solution be transferred in reactor, under the conditions of 180～200 DEG C react 5～14 hours；
5) cooled, washing, Fe is obtained after drying3O4Hollow ball.
Wherein, the mol ratio of sodium lauryl sulphate, trivalent iron salt and sodium acetate is 3～9:30:100；The addition of ethylene glycol is
Be enough to dissolve the amount of trivalent iron salt and sodium acetate, the amount of being preferably added to is to make the trivalent iron salt be with the molal volume ratio of ethylene glycol
0.1mol/L；The compactedness of reactor is 50～90%.
The preferred Iron(III) chloride hexahydrate of described trivalent iron salt；
The preferred sodium acetate trihydrate of described sodium acetate.
In step 4) solvent-thermal process time temperature preferably 200 DEG C, preferably 10 hours response time.
Beneficial effects of the present invention:
And by improving solvent-thermal method, add sodium lauryl sulphate (SDS), not only can shorten Fe3O4The preparation of hollow ball
Time, and Fe can be improved3O4The water solublity of hollow ball, the method operational approach is simple, low cost, beneficially large-scale production,
The Fe prepared due to the inventive method again3O4Hollow ball also shows superparamagnetism, therefore its valency in terms of biologic applications
Value have also been obtained raising.
Accompanying drawing explanation
Fig. 1 is the Fe of embodiment 1 preparation3O4The X ray diffracting spectrum of hollow ball, abscissa is 2 θ (units for °), vertical
Coordinate is relative diffracted intensity.
Fig. 2 is the Fe of embodiment 1 preparation3O4The stereoscan photograph of hollow ball.
Fig. 3 is the Fe of embodiment 1 preparation3O4The transmission electron microscope photo of hollow ball.
Fig. 4 is the Fe of embodiment 1 preparation3O4The magnetic hysteresis regression curve of hollow ball, abscissa is magnetic field intensity (unit is Oe),
Vertical coordinate is the intensity of magnetization (unit is emu/g).
Fig. 5 is the Fe of embodiment 1 preparation3O4The water solublity photo of hollow ball, being layered solution upper strata in figure is hexamethylene
(cyclohexane), lower floor is water (water).
Detailed description of the invention
With the form of embodiment technical solution of the present invention it is further explained below and illustrates.
Embodiment 1
By 1.62g FeCl3·6H2O joins in 60mL ethylene glycol solution, mechanical agitation 30 minutes so that it is be completely dissolved shape
Yellowly solution, then by 2.7g NaAc 3H2O joins in yellow solution, and continued mechanical stirs 1 hour, forms mixing
Solution.0.1839g sodium lauryl sulphate is joined in above-mentioned mixed solution, continue mechanical agitation 1 hour, it is thus achieved that be final
Precursor solution.Then precursor solution is loaded in the stainless steel cauldron that liner is politef that volume is 100mL,
10h is reacted at 200 DEG C.After solvent thermal reaction terminates, being cooled to room temperature, take out product, washing is dried, it is thus achieved that final sample.
Structure and morphology characterization
(220), (311), (222) of the most corresponding standard card (JCPDS 19-0629) of characteristic peak in Fig. 1, (400),
(422), (511), (440), (620), (533) corresponding with (444) crystal face, and do not have miscellaneous peak to occur, it can be seen that
Sample is the Fe that purity is higher3O4Crystal.
As can be seen from Figure 2 sample is made up of the spheroid of many a diameter of about 600nm surfaces versus rough.
From figure 3, it can be seen that Fe3O4Bead is hollow-core construction.
Performance characterization
Fe as can be seen from Figure 43O4The saturation magnetization of hollow ball is of a relatively high, and owing to coercivity and remanent magnetism are zero, sample
Product demonstrate superparamagnetism.
By Fe3O4Hollow ball is dispersed in the mixed solution of water and hexamethylene, stands a little while, lamination occurs, obtain Fig. 5,
Fe in Fig. 53O4Hollow ball is uniformly dispersed in water layer, thus proves prepared Fe3O4Hollow ball has preferable water solublity
Performance.
Embodiment 2
By 1.62g FeCl3·6H2O joins in 60mL ethylene glycol solution, mechanical agitation 30 minutes so that it is be completely dissolved shape
Yellowly solution 1., then by 2.7g NaAc 3H2O joins in yellow solution, and continued mechanical stirs 1 hour, is formed mixed
Close solution 2..0.3677g sodium lauryl sulphate is joined in above-mentioned mixed solution, continues mechanical agitation 1 hour, it is thus achieved that
Final precursor solution.Then precursor solution is loaded the stainless steel reaction that liner is politef that volume is 100mL
In still, at 200 DEG C, react 10h.After solvent thermal reaction terminates, being cooled to room temperature, take out product, washing is dried, it is thus achieved that
Whole sample.
Embodiment 3
By 1.62g FeCl3·6H2O joins in 60mL ethylene glycol solution, mechanical agitation 30 minutes so that it is be completely dissolved shape
Yellowly solution 1., then by 2.7g NaAc 3H2O joins in yellow solution, and continued mechanical stirs 1 hour, is formed mixed
Close solution 2..0.5191g sodium lauryl sulphate is joined in above-mentioned mixed solution, continues mechanical agitation 1 hour, it is thus achieved that
Final precursor solution.Then precursor solution is loaded the stainless steel reaction that liner is politef that volume is 100mL
In still, at 200 DEG C, react 10h.After solvent thermal reaction terminates, being cooled to room temperature, take out product, washing is dried, it is thus achieved that
Whole sample.
Embodiment 4
In addition to above example, the present invention can refer to existing method in the temperature conditions of solvent-thermal process, 180～200 DEG C of conditions
Lower reaction 5～all can realize the effect of the present invention under conditions of 14 hours.
Claims (6)
1. a preparation method for water solublity SPIO hollow ball, concrete grammar is as follows:
1) trivalent iron salt is added stirring and dissolving in ethylene glycol solution；
2) add sodium acetate, be uniformly mixed；
3) add sodium lauryl sulphate, be uniformly mixed；
4) by step 3) in gained mixed solution be transferred in reactor, under the conditions of reaction temperature 180～200 DEG C react 5～
14 hours；
5) cooled, washing, Fe is obtained after drying3O4Hollow ball；
Wherein, the mol ratio of sodium lauryl sulphate, trivalent iron salt and sodium acetate is 3～9:30:100, and the addition of ethylene glycol is
Be enough to dissolve the amount of trivalent iron salt and sodium acetate, the compactedness of reactor is 50～90%.
The preparation method of water solublity SPIO hollow ball the most according to claim 1, it is characterised in that
Described trivalent iron salt is Iron(III) chloride hexahydrate.
The preparation method of water solublity SPIO hollow ball the most according to claim 1, it is characterised in that
Described sodium acetate is sodium acetate trihydrate.
The preparation method of water solublity SPIO hollow ball the most according to claim 1, it is characterised in that
In step 4) in reaction temperature be 200 DEG C.
The preparation method of water solublity SPIO hollow ball the most according to claim 1, it is characterised in that
In step 4) in the response time be 10 hours.
The preparation method of water solublity SPIO hollow ball the most according to claim 1, it is characterised in that
The molal volume of trivalent iron salt and ethylene glycol is than for 0.1mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610242802.2A CN105883934A (en) | 2016-04-18 | 2016-04-18 | Method for preparing water-soluble superparamagnetic Fe3O4 hollow spheres |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610242802.2A CN105883934A (en) | 2016-04-18 | 2016-04-18 | Method for preparing water-soluble superparamagnetic Fe3O4 hollow spheres |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105883934A true CN105883934A (en) | 2016-08-24 |
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| CN201610242802.2A Pending CN105883934A (en) | 2016-04-18 | 2016-04-18 | Method for preparing water-soluble superparamagnetic Fe3O4 hollow spheres |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365208A (en) * | 2016-09-12 | 2017-02-01 | 安徽省特种设备检测院 | Method for preparing spherical Fe3O4 magnetic powder nano-particles |
| CN106475104A (en) * | 2016-11-20 | 2017-03-08 | 吉林师范大学 | A kind of recyclable Corallium Japonicum Kishinouye type photocatalyst and preparation method thereof |
| CN106495232A (en) * | 2016-11-20 | 2017-03-15 | 吉林师范大学 | Nano combined medicine-carried system of a kind of hollow sea urchin type magneto-optic and preparation method thereof |
| CN107311238A (en) * | 2017-08-02 | 2017-11-03 | 浙江理工大学 | A kind of preparation method of the hollow ferroso-ferric oxide microballoon of superparamagnetic |
| CN111463440A (en) * | 2020-04-13 | 2020-07-28 | 山东建筑大学 | Aminated Fe3O4@ MCM-41 nano-particles and application thereof in graphite felt anode of microbial fuel cell |
| CN113136106A (en) * | 2021-05-18 | 2021-07-20 | 湖南飞鸿达新材料有限公司 | Thin-sheet type heat-conducting wave-absorbing composite material |
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| CN103274478A (en) * | 2013-06-15 | 2013-09-04 | 厦门大学 | Method for preparing water-soluble ferroferric oxide nano particle |
| CN103480323A (en) * | 2013-09-03 | 2014-01-01 | 安徽师范大学 | Method for realizing one-step synthesis of ferroferric oxide microspheres having hierarchical structure and application method of product thereof |
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2016
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| CN103274478A (en) * | 2013-06-15 | 2013-09-04 | 厦门大学 | Method for preparing water-soluble ferroferric oxide nano particle |
| CN103480323A (en) * | 2013-09-03 | 2014-01-01 | 安徽师范大学 | Method for realizing one-step synthesis of ferroferric oxide microspheres having hierarchical structure and application method of product thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365208A (en) * | 2016-09-12 | 2017-02-01 | 安徽省特种设备检测院 | Method for preparing spherical Fe3O4 magnetic powder nano-particles |
| CN106365208B (en) * | 2016-09-12 | 2018-04-03 | 安徽省特种设备检测院 | One kind prepares spherical Fe3O4The method of nano-magnetic powder particle |
| CN106475104A (en) * | 2016-11-20 | 2017-03-08 | 吉林师范大学 | A kind of recyclable Corallium Japonicum Kishinouye type photocatalyst and preparation method thereof |
| CN106495232A (en) * | 2016-11-20 | 2017-03-15 | 吉林师范大学 | Nano combined medicine-carried system of a kind of hollow sea urchin type magneto-optic and preparation method thereof |
| CN107311238A (en) * | 2017-08-02 | 2017-11-03 | 浙江理工大学 | A kind of preparation method of the hollow ferroso-ferric oxide microballoon of superparamagnetic |
| CN111463440A (en) * | 2020-04-13 | 2020-07-28 | 山东建筑大学 | Aminated Fe3O4@ MCM-41 nano-particles and application thereof in graphite felt anode of microbial fuel cell |
| CN111463440B (en) * | 2020-04-13 | 2022-02-18 | 山东建筑大学 | Aminated Fe3O4@ MCM-41 nano-particles and application thereof in graphite felt anode of microbial fuel cell |
| CN113136106A (en) * | 2021-05-18 | 2021-07-20 | 湖南飞鸿达新材料有限公司 | Thin-sheet type heat-conducting wave-absorbing composite material |
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