CN101619135A - Magnetic hollow compound microstructure preparation method - Google Patents
Magnetic hollow compound microstructure preparation method Download PDFInfo
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- CN101619135A CN101619135A CN 200810132935 CN200810132935A CN101619135A CN 101619135 A CN101619135 A CN 101619135A CN 200810132935 CN200810132935 CN 200810132935 CN 200810132935 A CN200810132935 A CN 200810132935A CN 101619135 A CN101619135 A CN 101619135A
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Abstract
The invention provides a magnetic hollow compound microstructure preparation method, comprising the following steps: adopting spherical, apple-shaped and jar-shaped polysaccharide microspheres as templates, and coating series magnetic materials such as ferroferric oxide, ferrite and the like on the hollow polysaccharide microstructure compactly under 160-250 DEG C of hydrothermal condition to obtain spherical, apple-shaped and jar-shaped magnetic hollow compound microstructure. By observing under electron microscopy, the particle size of the magnetic materials coated on the surface of the polysaccharide microspheres is uniform and is about 50nm. The magnetic force test shows that the microstructure has good superparamagetism. The method has simple process and low cost.
Description
Technical field
The present invention relates to the preparation of magnetic hollow material, be specially the preparation method of the magnetic hollow composite microstructure of a kind of different-shape (sphere, apple shape, jar shape).
Background technology
The magnetic hollow structure transports at numerous areas such as medicine orientation because it can add big internal capacity by outfield control, medical diagnosis, and biological chemistry is separated, transmitter, catalytic field, environment remediation etc. have huge potential application, thereby receive much concern.Traditional template synthesis strategy needed to add a large amount of modification reagent so that template surface is modified before the coated magnetic particle usually---functionalization, thus but make its surface have the group of bond ion.This just makes complicated process of preparationization and cost higher.Emerging in recent years no template technology (self-assembly method) is though improve traditional method, but because self assembling process is difficult to control, and the adding of a large amount of tensio-active agents is still inevitable, thereby the method that development simply prepares the magnetic hollow structure seems particularly important.
Summary of the invention
The object of the present invention is to provide the method for the magnetic hollow composite microstructure of a kind of simple, with low cost preparation different-shape, the present invention has used hydrothermal synthesis method, and the magnetic composite microsphere that obtains has good homogeneous and magnetic.
The polysaccharide microsphere that method provided by the invention obtains after with the yeast carbonization is a template, water is solvent, ethylene glycol is as reductive agent, and sodium-acetate is a dispersion agent, iron, cobalt, manganese, the inorganic salt of zinc etc. are as the magnetic substance precursor, and the back that stirs moves in the reactor, put into the thermostat container thermostatically heating, the throw out that obtains gets final product with the washed with de-ionized water after drying.
The invention provides the method for the above-mentioned magnetic hollow composite microstructure of preparation, its key step is as follows:
A) preparation saccharan hollow microsphere suspension, concentration is controlled at 10～50g/L;
B) in the suspension that step a obtains, add the iron(ic) chloride of 0.01～0.1mol/L or cobalt chloride, Manganous chloride tetrahydrate, magnetic material precursors such as zinc sulfate, the sodium-acetate that adds 10-50g/L again is as dispersion agent, and ethylene glycol is as reductive agent;
C) suspension that step b is obtained stirred 20-200 minute, transferred to reactor after mixing, and it was transferred to thermostat container, at 160～250 ℃ of following thermostatically heating 6～24h;
D) the product deionized water wash that step c is obtained promptly obtains corresponding magnetic hollow composite microstructure behind 20-50 ℃ of down dry 5～24h.
Description of drawings
Fig. 1 is field emission scanning electron microscope (FESEM) the pattern photo of embodiment 1;
Fig. 2 is field emission scanning electron microscope (FESEM) the pattern photo of embodiment 2;
Fig. 3 is field emission scanning electron microscope (FESEM) the pattern photo of embodiment 3;
Fig. 4 is X-ray diffraction (XRD) collection of illustrative plates of final magnetic product: a curve is Fe
3O
4The b curve is CoFe
2O
4The c curve is MnFe
2O
4The d curve is ZnFe
2O
4
Embodiment
Embodiment 1: take by weighing spherical polysaccharide microsphere 3.0g, be scattered in the 50ml deionized water, add iron(ic) chloride, make its concentration remain on 0.01～0.1mol/L, sodium-acetate, make its concentration remain on 10-50g/L, ethylene glycol 50ml stirs to transfer to after 60 minutes to be put in the reactor in the thermostat container and heats 12h down at 190 ℃, with the throw out that obtains deionized water wash, dry 24h under 20 ℃ can obtain spheric Fe 3 O 4 magnetic composite microstructure finished product.
Embodiment 2: difference from Example 1 is that take by weighing is apple shape polysaccharide microsphere 3.0g, and all the other steps can obtain apple shape Fe 3 O 4 magnetic composite microstructure finished product with embodiment 1.
Embodiment 3: difference from Example 1 is that take by weighing is the polysaccharide microsphere 3.0g of jar shape, and all the other steps can obtain jar shape Fe 3 O 4 magnetic composite microstructure finished product with embodiment 1.
Embodiment 4: difference from Example 1 is, adds iron(ic) chloride, makes its concentration remain on 0.01～0.1mol/L, add Manganous chloride tetrahydrate again, make its concentration remain on 0.005-0.05mol/L, all the other steps can obtain spheric ferrous acid manganese magnetic composite microstructure finished product with embodiment 1.
Embodiment 5: difference from Example 1 is, adds iron(ic) chloride, makes its concentration remain on 0.01～0.1mol/L, add cobalt chloride again, make its concentration remain on 0.005-0.05mol/L, all the other steps can obtain spheric cobalt ferrite magnetic composite microstructure finished product with embodiment 1.
Embodiment 6: difference from Example 4 is, does not add Manganous chloride tetrahydrate, adds zinc sulfate, makes its concentration remain on 0.005-0.05mol/L, and all the other steps can obtain spheric zinc ferrite magnetic composite microstructure finished product with embodiment 4.
From the test result of the field emission scanning electron microscope (FE-SEM) of sample, the magnetic hollow microstructure that the present invention makes (spherical, apple shape, jar shape) homogeneity is fine, and magnetic-particle is even, the fine and close surface that is coated on the saccharan hollow ball.XRD result shows the magneticsubstance (MFe of series
2O
4, M=Fe, Co, Mn Zn) is successfully coated.
Claims (8)
1. the preparation method of a magnetic hollow composite microstructure is characterized in that:
Getting the polysaccharide microsphere that obtains after the yeast carbonization is template, the precursor that adds magnetic substance, disperse the back to add certain reductive agent and dispersion agent with deionized water, transfer to thermostat container 6～24h in the reactor after stirring, temperature range is 160 ℃～250 ℃, the throw out that obtains with washed with de-ionized water after convection drying promptly obtain corresponding magnetic hollow microstructure.
2. preparation method according to claim 1 is characterized in that, is template with the polysaccharide microsphere that obtains after the yeast carbonization, and the shape of polysaccharide microsphere has sphere, apple shape, jar shape.
3. preparation method according to claim 1 is characterized in that, the precursor of magnetic substance is an iron, cobalt, manganese, the inorganic salt of zinc etc.
4. preparation method according to claim 1 is characterized in that, the concentration of the precursor of magnetic substance is 0.01-0.1mol/L.
5. preparation method according to claim 1 is characterized in that, reductive agent is an ethylene glycol, and dispersion agent is a sodium-acetate.
6. preparation method according to claim 1 is characterized in that, the hydro-thermal Heating temperature of optimization is 160-250 ℃.
7. preparation method according to claim 1 is characterized in that, the hydro-thermal reaction time of optimization is 6-24h.
8. preparation method according to claim 1, it is characterized in that, the shell wall of gained magnetic hollow composite microstructure is made of two-layer material, and the internal layer material is the saccharan that obtains after the yeast carbonization, and outer material is serial magnetic substances such as Z 250, wustite.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817091A (en) * | 2010-04-28 | 2010-09-01 | 燕山大学 | Method for preparing iron nano-magnetic particles by taking T4 phage as template |
| CN102208614A (en) * | 2011-04-26 | 2011-10-05 | 中国矿业大学 | Method for preparing lithium ion battery cathode material coated iron sesquioxide |
| CN102921360A (en) * | 2012-11-15 | 2013-02-13 | 南京工程学院 | Monodisperse magnetic microsphere and preparation method thereof |
| CN103730226A (en) * | 2014-01-06 | 2014-04-16 | 四川大学 | Hollow magnetic polymer composite microsphere, and preparation method and application thereof |
| CN103949193A (en) * | 2014-04-04 | 2014-07-30 | 南京工业大学 | Universal method for preparation of inorganic hollow microspheres |
| CN104511263A (en) * | 2013-09-27 | 2015-04-15 | 中国科学院生态环境研究中心 | Microsphere with multiple magnetic nano cores@gaps@porous shell structures 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 |
| CN108726574A (en) * | 2018-06-15 | 2018-11-02 | 天津大学 | A kind of hollow core structures ferrimanganic oxygen magnetic Nano microsphere and preparation method |
| CN109806876A (en) * | 2018-12-18 | 2019-05-28 | 浙江工业大学 | A kind of magnetism ZnFe2O4/ graphene nano composite photo-catalyst and the preparation method and application thereof |
| CN112296350A (en) * | 2020-09-27 | 2021-02-02 | 浙江师范大学 | Magnetic hollow microsphere and preparation method and application thereof |
-
2008
- 2008-07-02 CN CN 200810132935 patent/CN101619135A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817091A (en) * | 2010-04-28 | 2010-09-01 | 燕山大学 | Method for preparing iron nano-magnetic particles by taking T4 phage as template |
| CN102208614A (en) * | 2011-04-26 | 2011-10-05 | 中国矿业大学 | Method for preparing lithium ion battery cathode material coated iron sesquioxide |
| CN102921360A (en) * | 2012-11-15 | 2013-02-13 | 南京工程学院 | Monodisperse magnetic microsphere and preparation method thereof |
| CN104511263A (en) * | 2013-09-27 | 2015-04-15 | 中国科学院生态环境研究中心 | Microsphere with multiple magnetic nano cores@gaps@porous shell structures and preparation method thereof |
| CN103730226A (en) * | 2014-01-06 | 2014-04-16 | 四川大学 | Hollow magnetic polymer composite microsphere, and preparation method and application thereof |
| CN103730226B (en) * | 2014-01-06 | 2016-10-05 | 四川大学 | A kind of hollow magnetic polymer complex microsphere and preparation method and application |
| CN103949193B (en) * | 2014-04-04 | 2016-02-10 | 南京工业大学 | A kind of general method preparing Inorganic Hollow Microspheres |
| CN103949193A (en) * | 2014-04-04 | 2014-07-30 | 南京工业大学 | Universal method for preparation of inorganic hollow microspheres |
| 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 |
| CN108726574A (en) * | 2018-06-15 | 2018-11-02 | 天津大学 | A kind of hollow core structures ferrimanganic oxygen magnetic Nano microsphere and preparation method |
| CN109806876A (en) * | 2018-12-18 | 2019-05-28 | 浙江工业大学 | A kind of magnetism ZnFe2O4/ graphene nano composite photo-catalyst and the preparation method and application thereof |
| CN109806876B (en) * | 2018-12-18 | 2022-01-25 | 浙江工业大学 | Magnetic ZnFe2O4Graphene nano composite photocatalyst and preparation method and application thereof |
| CN112296350A (en) * | 2020-09-27 | 2021-02-02 | 浙江师范大学 | Magnetic hollow microsphere and preparation method and application thereof |
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