CN104987731B - 1-dimention nano chain Fe3O4/ silk-fibroin compound and preparation method thereof - Google Patents
1-dimention nano chain Fe3O4/ silk-fibroin compound and preparation method thereof Download PDFInfo
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- CN104987731B CN104987731B CN201510382554.7A CN201510382554A CN104987731B CN 104987731 B CN104987731 B CN 104987731B CN 201510382554 A CN201510382554 A CN 201510382554A CN 104987731 B CN104987731 B CN 104987731B
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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 38
- 108010022355 Fibroins Proteins 0.000 title claims abstract description 37
- 150000001875 compounds Chemical class 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002105 nanoparticle Substances 0.000 claims abstract description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 10
- 239000012460 protein solution Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 7
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 2
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 claims 1
- 102000002322 Egg Proteins Human genes 0.000 claims 1
- 108010000912 Egg Proteins Proteins 0.000 claims 1
- 235000014103 egg white Nutrition 0.000 claims 1
- 210000000969 egg white Anatomy 0.000 claims 1
- 230000005291 magnetic effect Effects 0.000 abstract description 19
- 239000000463 material Substances 0.000 abstract description 7
- 238000010189 synthetic method Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 description 11
- 239000002086 nanomaterial Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012456 homogeneous solution Substances 0.000 description 3
- ZWKKPKNPCSTXGA-UHFFFAOYSA-N iron neodymium Chemical compound [Fe].[Fe].[Nd] ZWKKPKNPCSTXGA-UHFFFAOYSA-N 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000005381 magnetic domain Effects 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 210000005252 bulbus oculi Anatomy 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000009329 sexual behaviour Effects 0.000 description 1
- 238000013456 study Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L89/00—Compositions of proteins; Compositions of derivatives thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/10—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Peptides Or Proteins (AREA)
- Cosmetics (AREA)
Abstract
The invention belongs to material chemistry technical field, more particularly to a kind of 1-dimention nano chain Fe3O4/ silk-fibroin compound and preparation method thereof, above-mentioned compound includes Fe3O4Nano-particle and silk-fibroin, the Fe3O4Nano-particle is coated on the silk-fibroin and forms globular complex, and several described globular complex connect into chain under the influence of a magnetic field, and the wide material sources of raw material in the synthetic method, synthetic method craft is simple.
Description
Technical field
The invention belongs to material chemistry technical field, more particularly to a kind of 1-dimention nano chain Fe3O4/ silk-fibroin compound
And preparation method thereof.
Background technology
It is well known that nano material is due to its excellent characteristic, every field is had been applied to, specific morphology and structure
Progress of the preparation of nano material to new material is significant.The nano material of one-dimensional self assembly, can because widely used
For each side such as nanoelectronic, photoelectron, nanomagnets and biosensing apparatus, especially attract the eyeball of researcher.
In recent years, one-dimensional magnetic nano material is of great interest, its electro transfer, magnetic conversion, DNA separation and
Other biological medical domain has notable contribution.One-dimensional magnetic nano material is generally existed by ferromagnetism and superparamagnetic nanoparticle
Formed in holder or solution, the influence factor that scientists are formed to its one-dimentional structure is explored.First, block magnetic
Material anisotropy is very small, is easy to disappear in the presence of crystalline field, but under nanoscale, nanocrystal surface is relative
More atoms can be such that its track is restored on relatively low collaboration face, so as to form bigger magnetic anisotropy energy, be conducive to
The formation of one-dimensional catenary structure.Secondly, the dimensional effect caused by the change of electric field structure is also important factor in order, when organic
Caused electric field structure change can make the ferromagnetic sexual behaviour of material change during molecule cladding nano magnetic material, so as to cause
The formation of special construction.In addition, electrostatic interaction that the formation of 1-dimention nano chain may also be due between nano-particle and its
Caused by the effect of his power.Although having there is many pilot studys to attempt efficiency and water that raising prepares one-dimensional magnetic nanochain
Flat, the effective ways that exploration exploitation prepares one-dimensional magnetic nano material are still key issue urgently to be resolved hurrily.
At the same time, silk-fibroin has good biocompatibility, can effectively control preparation and the pattern of nano material,
And successfully prepare different nano materials, but 1-dimention nano chain Fe3O4The synthesis of/silk-fibroin compound not yet has been reported that.
In view of above-mentioned defect, the design people is actively subject to research and innovation, to found a kind of wiener rice chain
Fe3O4/ silk-fibroin compound and preparation method thereof, makes it with more the value in industry.
The content of the invention
In order to solve the above technical problems, it is an object of the invention to provide a kind of 1-dimention nano chain Fe3O4/ silk-fibroin is combined
Thing and preparation method thereof, its preparation method is simple.
A kind of 1-dimention nano chain Fe proposed by the present invention3O4/ silk-fibroin compound, including Fe3O4Nano-particle and silk egg
In vain, the Fe3O4Nano-particle is coated on the silk-fibroin and forms globular complex, several described globular complex connections
Into chain.
The invention also provides 1-dimention nano chain Fe3O4The preparation method of/silk-fibroin compound, comprises the following steps：
(1) silk-fibroin and source of iron are dissolved in solvent, stir and disperse；
(2) solution in the step (1) is poured into reactor, one block of magnet is placed in reactor bottom, in 160-
1-36h is reacted at 200 DEG C；
(3) after the completion of reacting, product is by washing, centrifugation and dries.
Further, the source of iron is FeCl3·6H2O, the weight/mass percentage composition of the silk protein solution intermediate filment is
7%.
Further, the solvent is ethylene glycol, and the step (1) is first by CH3COONa·3H2O and source of iron are dissolved in second two
After alcohol, silk-fibroin is added, stirs and disperses.
Further, the FeCl3·6H2O、CH3COONa·3H2O, ethylene glycol and silk protein solution mass ratio is：
(1-1.5)∶(5-6)∶(55.5-77.7)∶(8-12)。
Further, the magnet is Fe-Nd-B magnet.
By such scheme, the present invention at least has advantages below：The present invention loads Fe using silk-fibroin as carrier3O4Receive
Rice corpuscles, the compound is in chain, and its preparation method is simple, and magnet is used during preparation as externally-applied magnetic field and induces Fe3O4Nanoparticle
The magnetic domain orientation of son is consistent, the compound is had stronger saturation magnetic field, and synthesis material wide material sources, synthetic method work
Skill is simple.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, below with presently preferred embodiments of the present invention and coordinate accompanying drawing describe in detail as after.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of sample in the embodiment of the present invention one；
Fig. 2 is the transmission electron microscope picture of sample in the embodiment of the present invention one；
Fig. 3 is the X-ray powder diffraction figure of sample in the embodiment of the present invention one；
Fig. 4 is the scanning electron microscope (SEM) photograph of sample in the embodiment of the present invention two；
Fig. 5 is the scanning electron microscope (SEM) photograph of sample in the embodiment of the present invention three；
Fig. 6 is the scanning electron microscope (SEM) photograph of sample in the embodiment of the present invention four；
Fig. 7 is the scanning electron microscope (SEM) photograph of sample in the embodiment of the present invention five；
Fig. 8 is the magnetic hysteresis tropic comparison diagram of sample in the embodiment of the present invention one, four, five.
Embodiment
With reference to the accompanying drawings and examples, the embodiment to the present invention is described in further detail.Implement below
Example is used to illustrate the present invention, but is not limited to the scope of the present invention.
Embodiment one：
1-dimention nano chain Fe3O4The preparation method of/silk-fibroin compound comprises the following steps：
(1) by 1.35g FeCl3·6H2O, 5.97g CH3COONa·3H2O is added in 60mL ethylene glycol solutions, stirring
Until it is completely dissolved；
(2) silk protein solution of 10mL weight/mass percentage compositions 7% is added, is continued to stir to forming homogeneous solution；
(3) this mixed liquor is poured into reactor, 36h is reacted in 160 DEG C, while placing one piece of iron neodymium in reactor bottom
Boron magnets；
(4) reaction naturally cools to room temperature, and the centrifuge washing (deionized water under 8000rpm/min rotating speed after terminating
Respectively washed with ethanol 3 times), finally by product in 60 DEG C of vacuum drying.
Fig. 1 and Fig. 2 are the ESEM and transmission electron microscope picture of sample, it can be seen that Fe3O4Nano-particle and silk
Albumen composition is in spherical, and arranges chaining, and Fig. 3 is the X-ray powder diffraction figure of sample, shows the one-dimensional chain production of synthesis
Thing is Fe3O4。
Embodiment two：
1-dimention nano chain Fe3O4The preparation method of/silk-fibroin compound comprises the following steps：
(1) by 1.0g FeCl3·6H2O, 5.3g CH3COONa·3H2O is added in 50mL ethylene glycol solutions, and stirring is straight
It is completely dissolved to it；
(2) silk protein solution of 8mL weight/mass percentage compositions 7% is added, is continued to stir to forming homogeneous solution；
(3) this mixed liquor is poured into reactor, 24h is reacted in 180 DEG C, while placing one piece of iron neodymium in reactor bottom
Boron magnets；
(4) reaction naturally cools to room temperature, and the centrifuge washing (deionized water under 8000rpm/min rotating speed after terminating
Respectively washed with ethanol 3 times), finally by product in 60 DEG C of vacuum drying.
Fig. 4 is the scanning electron microscope (SEM) photograph of the sample, it can be seen that Fe3O4Nano-particle and silk-fibroin compound are in ball
Shape, and chaining is arranged, partly there is reunion.
Embodiment three：
1-dimention nano chain Fe3O4The preparation method of/silk-fibroin compound comprises the following steps：
(1) by 1.5g FeCl3·6H2O, 5.0g CH3COONa·3H2O is added in 70mL ethylene glycol solutions, and stirring is straight
It is completely dissolved to it；
(2) silk protein solution of 12mL weight/mass percentage compositions 7% is added, is continued to stir to forming homogeneous solution；
(3) this mixed liquor is poured into reactor, 12h is reacted in 200 DEG C, while placing one piece of iron neodymium in reactor bottom
Boron magnets；
(4) reaction naturally cools to room temperature, and the centrifuge washing (deionized water under 8000rpm/min rotating speed after terminating
Respectively washed with ethanol 3 times), finally by product in 60 DEG C of vacuum drying.
Fig. 5 is the scanning electron microscope (SEM) photograph of the sample, it can be seen that Fe3O4Nano-particle and silk-fibroin compound are in ball
Shape, and arrange chaining.
Example IV：
Fe3O4The preparation of nano-particle：
Its synthesis step is identical with embodiment one, only removes the step of adding silk-fibroin.
Fig. 6 is the scanning electron microscope (SEM) photograph of the sample, it can be seen that Fe3O4The pattern of nano-particle is irregular, and it is tight to reunite
Weight, can not be presented chain, and the presence for being indicated above silk-fibroin is the key factor of 1-dimention nano chain formation, while being also to be formed
Spherical Fe3O4The important template of/silk-fibroin nano-complex.
Embodiment five：
Fe3O4The preparation of/silk-fibroin compound：
Its synthesis step is identical with embodiment one, only removes the step of reactor bottom places magnet.
Fig. 7 is the scanning electron microscope (SEM) photograph of the sample, it can be seen that compound is in spherical, but it is serious to reunite, it is impossible in chain, by
This shows that externally-applied magnetic field is one of factor of 1-dimention nano chain formation.
Fig. 8 be in the magnetic hysteresis tropic of three kinds of different samples, Fig. 8 a, b, c curve be respectively embodiment one, example IV and
The magnetic hysteresis tropic of sample in embodiment five, it can be seen that 1-dimention nano chain Fe3O4The saturation of/silk-fibroin compound
Magnetic field highest, and it is not added with the Fe of silk-fibroin3O4Nano-particle takes second place, and that minimum is the Fe for being not added with magnetic field3O4/ silk-fibroin compound,
Illustrate in building-up process, externally-applied magnetic field plays vital effect to the magnetic of compound.
In summary, the present invention proposes one kind and prepares 1-dimention nano chain Fe3O4The method of/silk-fibroin compound, the party
Extensively, with low cost, synthesis technique is simple for the raw material sources of method；Wherein, the template of use is native protein, silk-fibroin, its
Bc is good, environmental sound；In reaction, Fe is induced using magnet as externally-applied magnetic field3O4The magnetic domain orientation of nano-particle
Unanimously, make compound that there is stronger saturation magnetic field, enhance its performance, make its application wider.
Described above is only the preferred embodiment of the present invention, is not intended to limit the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is some improvement and
Modification, these improvement and modification also should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of 1-dimention nano chain Fe3O4The preparation method of/silk-fibroin compound, it is characterised in that：The 1-dimention nano chain
Fe3O4/ silk-fibroin compound includes Fe3O4Nano-particle and silk-fibroin, the Fe3O4Nano-particle is coated on the silk-fibroin
Globular complex is formed, several described globular complex connect into chain, and its preparation method comprises the following steps：
(1) silk protein solution and source of iron are dissolved in solvent, stir and disperse；
(2) solution in the step (1) is poured into reactor, one block of magnet is placed in reactor bottom, at 160-200 DEG C
Lower reaction 1-36h；
(3) after the completion of reacting, product is by washing, centrifugation and dries.
2. 1-dimention nano chain Fe according to claim 13O4The preparation method of/silk-fibroin compound, it is characterised in that：
The source of iron is FeCl3·6H2O, the weight/mass percentage composition of the silk protein solution intermediate filment is 7%.
3. 1-dimention nano chain Fe according to claim 23O4The preparation method of/silk-fibroin compound, it is characterised in that：
The solvent is ethylene glycol, and the step (1) is first by CH3COONa·3H2O and source of iron are dissolved in after ethylene glycol, add an egg
White solution, stirs and disperses.
4. 1-dimention nano chain Fe according to claim 33O4The preparation method of/silk-fibroin compound, it is characterised in that：
The FeCl3·6H2O、CH3COONa·3H2O, ethylene glycol and silk protein solution mass ratio is：(1-1.5)∶(5-6)∶
(55.5-77.7)∶(8-12)。
5. 1-dimention nano chain Fe according to claim 13O4The preparation method of/silk-fibroin compound, it is characterised in that：
The magnet is Fe-Nd-B magnet.
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| CN201510382554.7A CN104987731B (en) | 2015-07-03 | 2015-07-03 | 1-dimention nano chain Fe3O4/ silk-fibroin compound and preparation method thereof |
| PCT/CN2015/089493 WO2017004893A1 (en) | 2015-07-03 | 2015-09-14 | One-dimensional fe3o4/fibroin composite nanochain and preparation method thereof |
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| CN105801878B (en) * | 2016-04-11 | 2017-12-29 | 武汉纺织大学 | A kind of fibroin albumen base nanometer MOFs preparation method |
| CN107552095A (en) * | 2017-09-17 | 2018-01-09 | 钱景 | The silk three-dimensional porous material and preparation method of carried titanium dioxide Nano Silver |
| CN112537797B (en) * | 2020-12-07 | 2023-04-18 | 安徽师范大学 | Ferroferric oxide/carbon nano tube/sulfur-loaded composite material with one-dimensional chain-like core-shell structure, preparation method and application |
| CN112980203B (en) * | 2021-02-18 | 2023-02-03 | 重庆大学 | Flexible ultrasonic attenuation film and application thereof |
| CN113004555A (en) * | 2021-02-18 | 2021-06-22 | 重庆大学 | Preparation method of flexible ultrasonic attenuation membrane |
| CN112980012A (en) * | 2021-02-22 | 2021-06-18 | 苏州大学 | Oriented material based on magnetic nanofiber and preparation method and application thereof |
| CN114209845B (en) * | 2021-12-18 | 2023-11-07 | 苏州健雄职业技术学院 | Preparation method of magnetic nano particles |
| CN115998946B (en) * | 2022-12-15 | 2024-08-09 | 四川大学 | Magneto-electric response bionic oriented fiber hydrogel and preparation method and application thereof |
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| CN101885513A (en) * | 2010-07-15 | 2010-11-17 | 上海交通大学 | One-dimensional ferroferric oxide magnetic nano chain and preparation method thereof |
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| CN102502873B (en) * | 2011-09-22 | 2013-10-16 | 西北工业大学 | Preparation method for one-dimensional magnetic nanochain |
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