CN104984693A - Preparation method of nanometer magnetism capsule - Google Patents
Preparation method of nanometer magnetism capsule Download PDFInfo
- Publication number
- CN104984693A CN104984693A CN201510438783.6A CN201510438783A CN104984693A CN 104984693 A CN104984693 A CN 104984693A CN 201510438783 A CN201510438783 A CN 201510438783A CN 104984693 A CN104984693 A CN 104984693A
- Authority
- CN
- China
- Prior art keywords
- preparation
- shuttle
- reaction
- described step
- capsule
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention relates to a preparation method of a nanometer magnetism capsule, and belongs to the technical field of nanometer material production. The preparation method comprises the following steps: firstly performing a hybrid reaction on ferric chloride hexahydrate and deionized water to obtain fusiform iron hydroxide oxide particles; then uniformly dispersing the fusiform iron hydroxide oxide particles into a trometamol buffer solution, then blending in dopamine hydrochloride for reaction to obtain fusiform iron hydroxide oxide alpha polydopamine nano-particles; and finally calcining the fusiform iron hydroxide oxide alpha polydopamine nano-particles to obtain the nanometer magnetism capsule. The preparation method is low in preparation cost and simple and convenient in operation process, materials required in the reaction process are low in toxicity and harmless, the stoichiometric ratio of the multi-component material can be effectively controlled, the obtained high-purity nanometer magnetism capsule is of a hollow structure at two ends, the shape is relatively uniform, and the specific surface area is large.
Description
Technical field
The invention belongs to nano material production technical field, be specifically related to the preparation method of nuclear shell structure nano magnetic capsule.
Background technology
Magnetic Nano material and composite thereof all obtain extensive and important application in conventional art and new and high technology, and the scope relating to its application comprises Magnetic resonance imaging, the field such as fixing, targeted drug delivery, immunoassays, cell separation of enzyme shows huge application prospect.It is single that magnetic nanometer composite material not only overcomes common monocomponent nanocomposite material composi, and the several functions that different material has organically can be combined, and demonstrates the unrivaled superior physicochemical property of common monocomponent nanocomposite particle.
Magnetic composite nano material not only has general nano material total surface and interface effect, small-size effect, quantum size effect and macro quanta tunnel effect, also show special magnetic property, this makes magnetic composite nano material be utilized widely, becomes one of important new material.The magnetic composite nano material of nucleocapsid structure is the novel magnetic composite nano materials just grown up in recent years, is made up of central particles and clad material.
Magnetic adhesive cryptomere core-shell structure copolymer composite nano materials as a kind of new material, novelty by magnetic ferroferric oxide core and capsule shape carbon shell phase compound, make it have unique capsule shape hollow-core construction and magnetic property, be with a wide range of applications.
Therefore how preparation property is stablized, the magnetic core-shell structure copolymer composite Nano functional material of excellent performance is still a problem being worth inquiring into.
Summary of the invention
The object of the invention is to the preparation method proposing a kind of nano magnetic capsule.
The present invention includes following steps:
1) ferric chloride (FeCl36H2O) and deionized water are mixed to reaction to terminate, after washing, obtain solid phase drying, obtain shuttle-type FeOOH particle;
2) under ultrasound condition, shuttle-type FeOOH is dispersed in TRIS buffer, and then be mixed into Dopamine hydrochloride and react, reaction terminates rear washing, obtains solid phase drying, obtains shuttle-type FeOOH@and gather dopamine nano particle;
3) shuttle-type FeOOH@is gathered dopamine nano particle to calcine under argon shield, obtain nano magnetic capsule.
The advantage of the above processing step of the present invention is: the equipment of employing is simple; preparation cost is low; operating process is easy; course of reaction material requested low toxicity, harmless; effectively can control the stoichiometric proportion of multi-component material; calcine under argon shield; prevent tri-iron tetroxide to be oxidized to di-iron trioxide, thus lose magnetism, obtaining highly purified nano magnetic capsule diameter is 50 ~ 80nm; length is 200 ~ 300nm; wall thickness is 5 ~ 10nm, and two ends are hollow structure, and pattern is more homogeneous; there is great specific area, can produce in large quantity.
In addition, in step 1) of the present invention, the temperature conditions of reaction is 60 ~ 80 DEG C, the temperature conditions of described drying is 60 DEG C, the FeOOH process made in this way is easy, and productive rate is higher, and pattern is homogeneous, favorable dispersibility, gathers dopamine provide advantage for preparing shuttle-type FeOOH@further.
Described step 2) in, described shuttle-type FeOOH is 1: 0.2 ~ 2 with the mixing quality ratio of Dopamine hydrochloride, can obtain poly-dopamine coating thickness homogeneous under this ratio, dispersed nano particle preferably.
Preferred described shuttle-type FeOOH is 1: 0.4 ~ 1 with the mixing quality ratio of Dopamine hydrochloride.
Described step 2) in, the temperature conditions of described reaction is 20 ~ 80 DEG C, reaction time 1 ~ 24h.Dopamine hydrochloride generation auto polymerization forms poly-dopamine at this point in the reaction, and can be coated on shuttle-type hydroxyl oxidize iron surface uniformly.
Preferred, step 2) in, the temperature conditions of described reaction is 30 ~ 50 DEG C, reaction time 12h.
Described step 2) in, the temperature conditions of described drying is 60 DEG C.Under this baking temperature, not only can remove residual moisture and solvent and can not have an impact to product clad and pattern.
In described step 3), described calcining heat condition is 500 ~ 600 DEG C, and calcination time is 1 ~ 24h.Within the scope of this calcining heat and calcination time, the dehydration of shuttle-type FeOOH can be made, cause volume contraction, form magnetic ferroferric oxide core, make poly-DOPA amine layer carbonization form carbon shell, final formation nano magnetic capsule.
In described step 3), be warming up to calcining heat with the heating rate of 5 DEG C/min.Carrying out intensification with this speed can make shuttle-type FeOOH good dehydration and volume when calcining shrink, and can not damage exterior carbon shell.
Accompanying drawing explanation
Fig. 1,2 is respectively the transmission electron microscope picture of the shuttle-type FeOOH prepared in the process of the present invention.
Fig. 3,4 is respectively the transmission electron microscope picture that the shuttle-type FeOOH@prepared in the process of the present invention gathers dopamine.
Fig. 5,6 is respectively the transmission electron microscope picture of the nano magnetic capsule prepared in the process of the present invention.
Detailed description of the invention
One, in order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1:
1, shuttle-type FeOOH is prepared:
Take 2.5g ferric chloride (FeCl36H2O) and 125mL deionized water, stir 30min after mixing, then this solution is placed in 80 DEG C of stirred in water bath 12h, respectively wash three times and centrifuging and taking with water, ethanol after question response terminates and obtain solid phase, then by solid phase in 60 DEG C of dry 12h, obtain shuttle-type FeOOH particle.
2, prepare shuttle-type FeOOH@and gather dopamine nano particle:
Take 0.045g shuttle-type FeOOH, be dispersed in 50mL TRIS buffer (pH ≈ 8.5) under ultrasound condition, and then add 0.02g Dopamine hydrochloride, after stirring 10min, this reaction system is placed in 30 DEG C of stirred in water bath 12h, respectively wash three times and centrifuging and taking with water, ethanol after question response terminates and obtain solid phase, then by solid phase in 60 DEG C of dry 12h, obtain shuttle-type FeOOH@and gather dopamine nano particle.
3, nano magnetic capsule is prepared:
Above-mentioned shuttle-type FeOOH@is gathered dopamine nano particle and is placed in tube furnace, under argon shield, be warming up to 500 DEG C (heating rate 5 DEG C/min) calcine 5h, obtain nano magnetic capsule.
Embodiment 2:
1, shuttle-type FeOOH is prepared:
Take 2.5g ferric chloride (FeCl36H2O) and 125mL deionized water, after mixing, stir 30min, then this solution is placed in 60 DEG C of stirred in water bath 12h, respectively 3 to 4 times are washed with water, ethanol after question response terminates, centrifugal, obtain 60 DEG C of dry 12h after solid phase, obtain shuttle-type FeOOH particle.
2, prepare shuttle-type FeOOH@and gather dopamine nano particle:
Take 0.045g shuttle-type FeOOH, be dispersed in 50mL TRIS buffer (pH ≈ 8.5) under ultrasound condition, and then add 0.03 g Dopamine hydrochloride, after stirring 10min, this reaction system is placed in 40 DEG C of stirred in water bath 12h, respectively 3 to 4 times are washed with water, ethanol after question response terminates, centrifugal, obtain 60 DEG C of dry 12h after solid phase, obtain shuttle-type FeOOH@and gather dopamine nano particle.
3, nano magnetic capsule is prepared:
Above-mentioned shuttle-type FeOOH@is gathered dopamine nano particle and is placed in tube furnace, under argon shield, be warming up to 600 DEG C (heating rate 5 DEG C/min) calcine 4h, obtain nano magnetic capsule.
Embodiment 3:
1, shuttle-type FeOOH is prepared:
Take 2.5g ferric chloride (FeCl36H2O) and 125mL deionized water, after mixing, stir 30min, then this solution is placed in 80 DEG C of stirred in water bath 12h, respectively 3 to 4 times are washed with water, ethanol after question response terminates, centrifugal, obtain 60 DEG C of dry 12h after solid phase, obtain shuttle-type FeOOH particle.
2, prepare shuttle-type FeOOH@and gather dopamine nano particle:
Take 0.045g shuttle-type FeOOH, be dispersed in 50mL TRIS buffer (pH ≈ 8.5) under ultrasound condition, then 0.045g Dopamine hydrochloride is added, after stirring 10min, this reaction system is placed in 50 DEG C of stirred in water bath 12h, respectively 3 to 4 times are washed with water, ethanol after question response terminates, centrifugal, obtain 60 DEG C of dry 12h after solid phase, obtain shuttle-type FeOOH@and gather dopamine nano particle.
3, nano magnetic capsule is prepared:
Above-mentioned shuttle-type FeOOH@is gathered dopamine nano particle and is placed in tube furnace, under argon shield, be warming up to 700 DEG C (heating rate 5 DEG C/min) calcine 2h, obtain nano magnetic capsule.
Two, product checking:
As shown in Figure 1, 2, for adopt the inventive method to prepare the different amplification of shuttle-type FeOOH under transmission electron microscope picture.From Fig. 1,2: prepared product is shuttle-type nano particle, and length is at 200 ~ 300nm, and diameter is at about 50nm.
As shown in Figure 3,4, the shuttle-type FeOOH@for adopting the inventive method to prepare gathers the transmission electron microscope picture under the different amplification of dopamine.From Fig. 3,4: prepared product keeps shuttle-type pattern, and surface has clad, coating thickness 5 ~ 10nm.
As shown in Figure 5,6, for adopt the inventive method to prepare the different amplification of nano magnetic capsule under transmission electron microscope picture.From Fig. 5,6: prepared product presents capsule shape, tri-iron tetroxide is core, and carbon coating layer is the capsule-like structure of shell, two ends hollow.
Claims (10)
1. a preparation method for nano magnetic capsule, is characterized in that comprising the following steps:
1) ferric chloride (FeCl36H2O) and deionized water are mixed to reaction to terminate, after washing, obtain solid phase drying, obtain shuttle-type FeOOH particle;
2) under ultrasound condition, shuttle-type FeOOH is dispersed in TRIS buffer, and then be mixed into Dopamine hydrochloride and react, reaction terminates rear washing, obtains solid phase drying, obtains shuttle-type FeOOH@and gather dopamine nano particle;
3) shuttle-type FeOOH@is gathered dopamine nano particle to calcine under argon shield, obtain nano magnetic capsule.
2. preparation method according to claim 1, it is characterized in that in described step 1), the temperature conditions of described reaction is 60 ~ 80 DEG C.
3. preparation method according to claim 1, it is characterized in that in described step 1), the temperature conditions of described drying is 60 DEG C.
4. preparation method according to claim 1, is characterized in that described step 2) in, described shuttle-type FeOOH is 1: 0.2 ~ 2 with the mixing quality ratio of Dopamine hydrochloride.
5. preparation method according to claim 4, is characterized in that described step 2) in, described shuttle-type FeOOH is 1: 0.4 ~ 1 with the mixing quality ratio of Dopamine hydrochloride.
6. preparation method according to claim 1, is characterized in that described step 2) in, the temperature conditions of described reaction is 20 ~ 80 DEG C, reaction time 1 ~ 24h.
7. preparation method according to claim 6, is characterized in that described step 2) in, the temperature conditions of described reaction is 30 ~ 50 DEG C, reaction time 12h.
8. preparation method according to claim 1, is characterized in that described step 2) in, the temperature conditions of described drying is 60 DEG C.
9. preparation method according to claim 1, it is characterized in that in described step 3), described calcining heat condition is 500 ~ 600 DEG C, and calcination time is 1 ~ 24h.
10. preparation method according to claim 9, is characterized in that, in described step 3), being warming up to calcining heat with the heating rate of 5 DEG C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510438783.6A CN104984693A (en) | 2015-07-24 | 2015-07-24 | Preparation method of nanometer magnetism capsule |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510438783.6A CN104984693A (en) | 2015-07-24 | 2015-07-24 | Preparation method of nanometer magnetism capsule |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104984693A true CN104984693A (en) | 2015-10-21 |
Family
ID=54296659
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510438783.6A Pending CN104984693A (en) | 2015-07-24 | 2015-07-24 | Preparation method of nanometer magnetism capsule |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104984693A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107561137A (en) * | 2016-07-01 | 2018-01-09 | 南京理工大学 | Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene nano composite material and preparation method thereof |
| CN107561130A (en) * | 2016-07-01 | 2018-01-09 | 南京理工大学 | The Fe of diallyl dimethyl ammoniumchloride cladding1.833(OH)0.5O2.5Load nano combined sensing material of nitrogen-doped graphene and preparation method thereof |
| CN107574510A (en) * | 2017-09-18 | 2018-01-12 | 扬州大学 | A kind of preparation method of the composite nano fiber of the ferroso-ferric oxide for carrying space and carbon |
| CN108424617A (en) * | 2018-03-15 | 2018-08-21 | 厦门大学 | A kind of preparation method and applications of iron oxide hydroxide load graphene oxide fire retardant |
| CN109825252A (en) * | 2019-03-04 | 2019-05-31 | 安徽理工大学 | Core-shell structure Fe3O4@C@MoS2The preparation and its application of composite material |
| CN109953021A (en) * | 2017-12-26 | 2019-07-02 | 华东理工大学 | Pyrethroids microcapsules, preparation method and insect prevention preparation |
| CN107561137B (en) * | 2016-07-01 | 2019-07-16 | 南京理工大学 | Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene nanocomposite and preparation method thereof |
| CN111117564A (en) * | 2019-12-03 | 2020-05-08 | 安徽理工大学 | Yolk-eggshell type magnetic carbon composite material, preparation method and application |
| CN115636443A (en) * | 2022-10-27 | 2023-01-24 | 郑州航空工业管理学院 | Preparation method of magnetic nanoparticle coated microcapsule-shaped carbon-based composite material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101259399A (en) * | 2007-12-18 | 2008-09-10 | 浙江大学 | Method for preparing inorganic nano microcapsule by one-step method |
| CN102623693A (en) * | 2012-04-13 | 2012-08-01 | 山东大学 | High specific capacity spindle-shaped ferroferric oxide/carbon nano composite material for negative electrode of lithium ion battery |
| CN103618061A (en) * | 2013-11-04 | 2014-03-05 | 中国科学院化学研究所 | Method for carbon layer controllable coating to polyanion-type lithium ion batteries cathode materials |
| CN103894161A (en) * | 2014-04-09 | 2014-07-02 | 复旦大学 | Synthesis method of magnetic metal organic framework composite material and application of material |
| CN104549159A (en) * | 2015-01-30 | 2015-04-29 | 上海工程技术大学 | Functional magnetic silver nano wire composite material as well as preparation method and application thereof |
-
2015
- 2015-07-24 CN CN201510438783.6A patent/CN104984693A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101259399A (en) * | 2007-12-18 | 2008-09-10 | 浙江大学 | Method for preparing inorganic nano microcapsule by one-step method |
| CN102623693A (en) * | 2012-04-13 | 2012-08-01 | 山东大学 | High specific capacity spindle-shaped ferroferric oxide/carbon nano composite material for negative electrode of lithium ion battery |
| CN103618061A (en) * | 2013-11-04 | 2014-03-05 | 中国科学院化学研究所 | Method for carbon layer controllable coating to polyanion-type lithium ion batteries cathode materials |
| CN103894161A (en) * | 2014-04-09 | 2014-07-02 | 复旦大学 | Synthesis method of magnetic metal organic framework composite material and application of material |
| CN104549159A (en) * | 2015-01-30 | 2015-04-29 | 上海工程技术大学 | Functional magnetic silver nano wire composite material as well as preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| YA MAO ET AL.: "Rod-like β-FeOOH＠poly(dopamine)-Au-poly(dopamine) nanocatalysts with improved recyclable activities", 《DALTON TRANSACTIONS》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107561137A (en) * | 2016-07-01 | 2018-01-09 | 南京理工大学 | Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene nano composite material and preparation method thereof |
| CN107561130A (en) * | 2016-07-01 | 2018-01-09 | 南京理工大学 | The Fe of diallyl dimethyl ammoniumchloride cladding1.833(OH)0.5O2.5Load nano combined sensing material of nitrogen-doped graphene and preparation method thereof |
| CN107561137B (en) * | 2016-07-01 | 2019-07-16 | 南京理工大学 | Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene nanocomposite and preparation method thereof |
| CN107561130B (en) * | 2016-07-01 | 2019-07-16 | 南京理工大学 | The Fe of diallyl dimethyl ammoniumchloride cladding1.833(OH)0.5O2.5Load nano combined sensing material of nitrogen-doped graphene and preparation method thereof |
| CN107574510A (en) * | 2017-09-18 | 2018-01-12 | 扬州大学 | A kind of preparation method of the composite nano fiber of the ferroso-ferric oxide for carrying space and carbon |
| CN109953021A (en) * | 2017-12-26 | 2019-07-02 | 华东理工大学 | Pyrethroids microcapsules, preparation method and insect prevention preparation |
| CN108424617A (en) * | 2018-03-15 | 2018-08-21 | 厦门大学 | A kind of preparation method and applications of iron oxide hydroxide load graphene oxide fire retardant |
| CN109825252A (en) * | 2019-03-04 | 2019-05-31 | 安徽理工大学 | Core-shell structure Fe3O4@C@MoS2The preparation and its application of composite material |
| CN109825252B (en) * | 2019-03-04 | 2021-09-10 | 安徽理工大学 | Core-shell structure Fe3O4@C@MoS2Preparation of composite material and application thereof |
| CN111117564A (en) * | 2019-12-03 | 2020-05-08 | 安徽理工大学 | Yolk-eggshell type magnetic carbon composite material, preparation method and application |
| CN115636443A (en) * | 2022-10-27 | 2023-01-24 | 郑州航空工业管理学院 | Preparation method of magnetic nanoparticle coated microcapsule-shaped carbon-based composite material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104984693A (en) | Preparation method of nanometer magnetism capsule | |
| CN104810509B (en) | Ferroso-ferric oxide/graphene three dimensional composite structure and its preparation method and application | |
| CN105502342A (en) | Method for preparing nanometer hollow carbon spheres with dopamine serving as carbon source | |
| CN103633295B (en) | A kind of Si-C composite material, lithium ion battery and its preparation method and application | |
| CN105565265B (en) | A kind of preparation method of the complex microsphere lithium ion battery negative material with yolk structure | |
| CN106966443B (en) | A kind of preparation method of transition metal oxide/sulfide nanocomposite | |
| CN106025231B (en) | A kind of preparation method of hollow graphite alkene ball/sulphur composite material | |
| CN107384326B (en) | Preparation method of gelatin chitosan-nano silicon dioxide multi-core phase change energy storage microcapsule | |
| CN103936987B (en) | Carbon nanotube composite material and preparation method thereof | |
| CN103880020B (en) | Chirality mesoporous organic silica nanotube or core-shell type nanometer rod and preparation method thereof | |
| CN104403275B (en) | A kind of modified graphene/thermoset ting resin composite and preparation method thereof | |
| CN103360616A (en) | Method for preparing hybrid film through graphene/nano crystalline cellulose dispersion liquid | |
| CN102391831A (en) | Carbon nanotube composite material modified by magnetic nanoparticles, its preparation method and application | |
| CN105664936A (en) | Method for preparing nano composite material having core-shell structure with dopamine as carbon source | |
| CN108039287B (en) | A kind of Fe of bivalve layer core-shell structure3O4@C@MnO2Composite material and preparation method | |
| CN105036178B (en) | A kind of preparation method of modified nano zinc oxide | |
| CN104192820A (en) | Mesoporous carbon sphere/manganese dioxide composite nano material and preparation method thereof | |
| CN108217733A (en) | A kind of preparation method of carbon-manganese dioxide composite material | |
| CN102674379B (en) | Hollow mesoporous silicon dioxide nano particles and method for preparing same | |
| CN104439276B (en) | A kind of quick method and product preparing hollow porous silica/argentum nano composite material | |
| CN102641701A (en) | Method for preparing carbon-coated ferroferric oxide double-shell hollow colloidal spheres | |
| CN107507686A (en) | A kind of preparation method of magnetic nano cages | |
| CN104857945A (en) | Preparation method of zinc oxide/carbon micro-sphere composite material | |
| CN105110343A (en) | Method for rapid preparation of monodisperse ordered mesoporous silicon oxide hollow sphere | |
| CN105000589A (en) | Citric acid-modified nanometer zinc oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20151021 |