CN105800695A - Carbon-based magnetic composite material and preparation method thereof - Google Patents
Carbon-based magnetic composite material and preparation method thereof Download PDFInfo
- Publication number
- CN105800695A CN105800695A CN201610133264.3A CN201610133264A CN105800695A CN 105800695 A CN105800695 A CN 105800695A CN 201610133264 A CN201610133264 A CN 201610133264A CN 105800695 A CN105800695 A CN 105800695A
- Authority
- CN
- China
- Prior art keywords
- iron salt
- magnetic composite
- carbon back
- back magnetic
- cellulose
- 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
- 239000002131 composite material Substances 0.000 title claims abstract description 56
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 49
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000000243 solution Substances 0.000 claims abstract description 37
- 150000002505 iron Chemical class 0.000 claims abstract description 36
- 229920002678 cellulose Polymers 0.000 claims abstract description 32
- 239000001913 cellulose Substances 0.000 claims abstract description 32
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000012266 salt solution Substances 0.000 claims abstract description 15
- 239000004094 surface-active agent Substances 0.000 claims abstract description 12
- 239000012298 atmosphere Substances 0.000 claims abstract description 11
- 230000005415 magnetization Effects 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 235000010980 cellulose Nutrition 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- JHJUUEHSAZXEEO-UHFFFAOYSA-M sodium;4-dodecylbenzenesulfonate Chemical group [Na+].CCCCCCCCCCCCC1=CC=C(S([O-])(=O)=O)C=C1 JHJUUEHSAZXEEO-UHFFFAOYSA-M 0.000 claims description 4
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000000839 emulsion Substances 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 2
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 2
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 2
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims 2
- 230000003213 activating effect Effects 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 239000003575 carbonaceous material Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 17
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 6
- 229940056319 ferrosoferric oxide Drugs 0.000 description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 6
- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 description 6
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 6
- 239000000696 magnetic material Substances 0.000 description 6
- 150000001721 carbon Chemical class 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005307 ferromagnetism Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- SNRUBQQJIBEYMU-NJFSPNSNSA-N dodecane Chemical group CCCCCCCCCCC[14CH3] SNRUBQQJIBEYMU-NJFSPNSNSA-N 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910000859 α-Fe Inorganic materials 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
- C01G49/06—Ferric oxide [Fe2O3]
-
- 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]
-
- 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
-
- 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
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a carbon-based magnetic composite material and a preparation method thereof. The composite material is prepared from an iron salt solution and a cellulose solution through a microwave hydrothermal method, wherein the mass ratio of the iron salt in the iron salt solution to the cellulose in the cellulose solution is (0.1-1.0):1; the iron salt solution comprises an iron salt, a surfactant and ethylene glycol; the mass ratio of the surfactant to the iron salt is 1:(0.2-0.9); and 15-40ml of ethylene glycol is added into each millimole of iron salt. In the method disclosed by the invention, the magnetic carbon composite material can be directionally synthesized according to atmosphere difference in preparation, and the prepared carbon material has relatively high saturation magnetization intensity of 8.3-17.6emu/g.
Description
Technical field
The present invention relates to a kind of composite, particularly relate to a kind of carbon back magnetic composite and system thereof
Preparation Method.
Background technology
Ferrum oxide includes the multiple thing phases such as ferroso-ferric oxide, λ-iron sesquioxide, α-iron sesquioxide.
Wherein ferroso-ferric oxide and λ-iron sesquioxide have magnetic.Fe 3 O 4 magnetic material is that one is many
Functional magnetic material, the treatment of tumor, microwave absorbing material, catalyst carrier, cell separation,
Magnetic recording material, magnetic fluid, medicine and other fields are widely used the most.Carbon back magnetic material combines
The advantage of carbon and magnetic material, the Adsorption of organic dyestuff and heavy metal ion, medicine in water
Thing loads and release, and the field such as bio-medical all has important function.
The preparation side of a kind of magnetic nanometer ferroferric oxide-graphene composite catalyst that prior art proposes
Method, this magnetic material uses chemical coprecipitation, bivalence, trivalent iron salt is mixed with graphene oxide,
Stir at a certain temperature, synthesize Fe3O by ammonia water titration afterwards4-graphene composite material.This system
Preparation Method technological requirement is high, and step is relatively complicated, and product impurity content is many, and reduces graphite oxide
The hydrazine hydrate that alkene is conventional has certain toxicity, and the magnetic material that the method prepares exists potential safety hazard.
Summary of the invention
Present invention is primarily targeted at, it is provided that a kind of novel carbon back magnetic composite and preparation side thereof
Method, to be solved technical problem is that makes that its preparation technology is simple, preparation process condition is gentle, and tool
There is higher saturation magnetization, thus more suitable for practicality.
The object of the invention to solve the technical problems realizes by the following technical solutions.Foundation
The carbon back magnetic composite that the present invention proposes is reacted by iron salt solutions and cellulose solution and prepares, wherein,
In iron salt solutions, the quality of iron salt is 0.1-1.0:1 with the mass ratio of cellulose in cellulose solution；
Described iron salt solutions includes: iron salt, surfactant, ethylene glycol, wherein, surfactant and
The mass ratio of iron salt is 1:0.2-0.9, and every mM of iron salt adds 15-40ml ethylene glycol.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Preferably, aforesaid carbon back magnetic composite, wherein said iron salt is selected from ferric nitrate, chlorine
Change one or more in ferrum, iron acetate.
Preferably, aforesaid carbon back magnetic composite, wherein said cellulose is microcrystalline Cellulose.
Preferably, aforesaid carbon back magnetic composite, wherein said surfactant is dodecane
Base benzene sulfonic acid sodium salt.
The object of the invention to solve the technical problems also uses following technical scheme to realize.Foundation
The preparation method of the carbon back magnetic composite that the present invention proposes, comprises the following steps:
1) 1:0.2-0.9 in mass ratio weighs surfactant and iron salt, joins in ethylene glycol,
Mix homogeneously, forms iron salt solutions, and every mM of iron salt adds 15-40ml ethylene glycol；In mass ratio 1:
0.2-0.9 weighing sodium hydroxide and cellulose, join in ethylene glycol, mix homogeneously, forms cellulose
Solution, every gram of cellulose adds 5-20ml ethylene glycol；In iron salt solutions, the quality of iron salt is molten with cellulose
In liquid, the mass ratio of cellulose is 0.1-1.0:1；
2) iron salt solutions and cellulose solution are mixed, stirring, obtain suspended emulsion, suspension is carried out
Microwave-hydrothermal method processes 5-60min, and the temperature of microwave-hydrothermal method processing procedure is 120-220 DEG C, microwave
Hydro-thermal method carries out cooling down after processing, ultrasonic Separation, wash, be dried to obtain product；
3) under inert atmosphere or air atmosphere, product is calcined 1-6h at 300-800 DEG C, cold
But, carbon back magnetic composite is obtained；Described inert atmosphere is in nitrogen, argon, helium
Kind.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Preferably, the preparation method of aforesaid carbon back magnetic composite, wherein said step 2) in
The treatment temperature of microwave-hydrothermal method is 180 DEG C, and the process time is 10-40min.
Preferably, the preparation method of aforesaid carbon back magnetic composite, wherein said step 3) in
Calcining heat is 300-500 DEG C, and calcination time is 3-6h.
Preferably, the preparation method of aforesaid carbon back magnetic composite, wherein said step 3) in
Inert atmosphere is argon.
By technique scheme, carbon back magnetic composite of the present invention and preparation method thereof at least has
Following advantages:
1, the carbon back magnetic composite that prepared by the present invention, raw material is simple, for cellulose and iron salt, nothing
Need extra reducing agent and organic solvent, save the energy, environmental protection.
2, the carbon back magnetic composite of the present invention has higher saturation magnetization, its saturated magnetization
Intensity is 8.3emu/g～17.6emu/g.
3, preparation technology of the present invention is simple, preparation is quick, process conditions are gentle, and beneficially industrialization pushes away
Extensively.
4, by controlling reaction atmosphere, the oxide of controlled syntheses ferrum is also one of advantage of this method.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the present invention's
Technological means, and can be practiced according to the content of description, below with presently preferred embodiments of the present invention
And after coordinating accompanying drawing to describe in detail such as.
Accompanying drawing explanation
Fig. 1 is the preparation technology flow chart of carbon back magnetic composite of the present invention.
Fig. 2 is the X-ray diffraction spectrogram of the embodiment of the present invention 1 carbon back magnetic composite.
Fig. 3 is the X-ray diffraction spectrogram of the embodiment of the present invention 2 carbon back magnetic composite.
Fig. 4 is the X-ray diffraction spectrogram of the embodiment of the present invention 3 carbon back magnetic composite.
Fig. 5 is the hysteresis curve spectrogram of embodiment of the present invention 1-3 carbon back magnetic composite.
Detailed description of the invention
By further illustrating the technological means and merit that the present invention taked by reaching predetermined goal of the invention
Effect, below in conjunction with accompanying drawing and preferred embodiment, to the carbon back magnetic composite proposed according to the present invention and
Its detailed description of the invention of its preparation method, feature and effect thereof, after describing in detail such as.In the description below
In, what different " embodiments " or " embodiment " referred to is not necessarily same embodiment.Additionally,
Special characteristic or feature in one or more embodiment can be combined by any suitable form.
Embodiment 1
1) 1.6g sodium hydroxide is joined in 10ml ethylene glycol, stirring, obtain sodium hydroxide solution；
0.5g cellulose is joined in above-mentioned sodium hydroxide solution, stirring, obtain homodisperse cellulose
Solution；Being joined by 0.6g dodecylbenzene sodium sulfonate in 20ml ethylene glycol, stirring forms surface and lives
Property agent solution；0.54g iron chloride is joined in above-mentioned surfactant solution, stirring, obtain all
Even scattered ferric chloride solution；
2) above-mentioned cellulose solution and ferric chloride solution mixing, stirring, obtain suspension, to suspension
Carrying out microwave-hydrothermal method and process 45min, the temperature of microwave-hydrothermal method processing procedure is 180 ± 2 DEG C, micro-
Ripple hydro-thermal method carries out cooling down after processing, ultrasonic Separation, wash, be dried to obtain product；
3) under argon shield, product is calcined 3h, cooling at 300 DEG C, obtains carbon back magnetic
Composite.
Fig. 2 is the X-ray diffraction spectrogram of the carbon back magnetic composite obtained by this, X-ray diffraction
Diffraction maximum in spectrogram is identical with the X-ray diffraction spectrogram of the single-phase ferroso-ferric oxide of standard, spectrum
Each diffraction maximum in figure can index be all to have the single-phase ferroso-ferric oxide of inverse spinel structure, with
Standard JCPDS card (No.19-0629) fits like a glove.The X-ray diffraction spectrogram display of product is produced
Thing contains the diffraction maximum of ferroso-ferric oxide, illustrates that product is carbon back Fe 3 O 4 magnetic composite.
The hysteresis curve figure of this carbon back magnetic composite is as it is shown in figure 5,1 be this composite in Fig. 5
The first magnetic hysteresis regression line, its saturation magnetization is 8.3emu/g.
Embodiment 2
1) 1.6g sodium hydroxide is joined in 10ml ethylene glycol, stirring, obtain sodium hydroxide solution；
1.0g cellulose is joined in above-mentioned sodium hydroxide solution, stirring, obtain homodisperse cellulose
Solution；Being joined by 0.6g dodecylbenzene sodium sulfonate in 30ml ethylene glycol, stirring forms surface and lives
Property agent solution；0.4g ferric nitrate is joined in above-mentioned surfactant solution, stirring, obtain uniformly
Scattered ferric chloride solution；
2) above-mentioned cellulose solution and ferric chloride solution mixing, stir, obtain suspension, to outstanding
Supernatant liquid carries out microwave-hydrothermal method and processes 20min, and the temperature of microwave-hydrothermal method processing procedure is 160 ± 2 DEG C,
Microwave-hydrothermal method carries out cooling down after processing, ultrasonic Separation, wash, be dried to obtain product；
3) under argon shield, product is calcined 6h, cooling at 500 DEG C, obtains carbon back magnetic
Composite.
Fig. 3 is the X-ray diffraction spectrogram of the carbon back magnetic composite obtained by this, and the X-of product penetrates
Line diffraction spectrogram display product contains the diffraction maximum of ferroso-ferric oxide, illustrates that product is that carbon back four aoxidizes three
Ferromagnetism composite.The hysteresis curve figure of this carbon back magnetic composite is as it is shown in figure 5, in Fig. 52
For the first magnetic hysteresis regression line of this composite, its saturation magnetization is 17.2emu/g.
Embodiment 3
1) 1.6g sodium hydroxide is joined in 10ml ethylene glycol, stirring, obtain sodium hydroxide solution；
2.0g cellulose is joined in above-mentioned sodium hydroxide solution, stirring, obtain homodisperse cellulose
Solution；Being joined by 0.6g dodecylbenzene sodium sulfonate in 30ml ethylene glycol, stirring forms surface and lives
Property agent solution；0.17g Schweinfurt green is joined in above-mentioned surfactant solution, stirring, obtain all
Even scattered ferric chloride solution；
2) above-mentioned cellulose solution and ferric chloride solution mixing, stir, obtain suspension, to outstanding
Supernatant liquid carries out microwave-hydrothermal method and processes 60min, and the temperature of microwave-hydrothermal method processing procedure is 140 ± 2 DEG C,
Microwave-hydrothermal method carries out cooling down after processing, ultrasonic Separation, wash, be dried to obtain product；
3) in air atmosphere, product is calcined 1h, cooling at 300 DEG C, obtains carbon back magnetic
Composite.
Fig. 4 is the X-ray diffraction spectrogram of the carbon back magnetic composite obtained by this, and the X-of product penetrates
Line diffraction spectrogram display product contains the diffraction maximum of λ-iron sesquioxide, illustrates that product is carbon back λ-three
Aoxidize two ferromagnetism composites.The hysteresis curve figure of this carbon back magnetic composite as it is shown in figure 5,
In Fig. 5,3 is the first magnetic hysteresis regression line of this composite, and its saturation magnetization is 17.6emu/g.
The above, be only presently preferred embodiments of the present invention, and the present invention not makees any form
On restriction, any simple modification above example made according to the technical spirit of the present invention, etc.
With change and modification, all still fall within the range of technical solution of the present invention.
Claims (10)
1. a carbon back magnetic composite, it is characterised in that: this composite is by iron salt solutions and fibre
Dimension cellulose solution reaction prepares, wherein, and the quality of iron salt and cellulose in cellulose solution in iron salt solutions
Mass ratio be 0.1-1.0:1；Described iron salt solutions includes: iron salt, surfactant, second
Glycol, wherein, the mass ratio of surfactant and iron salt is 1:0.2-0.9, and every mM of iron salt adds
Enter 15-40ml ethylene glycol.
Carbon back magnetic composite the most according to claim 1, it is characterised in that described ferrum
One or more in ferric nitrate, iron chloride, iron acetate of salt.
Carbon back magnetic composite the most according to claim 1, it is characterised in that described fibre
Dimension element is microcrystalline Cellulose.
Carbon back magnetic composite the most according to claim 1, it is characterised in that described table
Face activating agent is dodecylbenzene sodium sulfonate.
5. according to the carbon back magnetic composite described in any one of claim 1-4, it is characterised in that
Its saturation magnetization is 8.3emu/g～17.6emu/g.
6. the preparation method of a carbon back magnetic composite, it is characterised in that: comprise the following steps:
1) 1:0.2-0.9 in mass ratio weighs surfactant and iron salt, joins in ethylene glycol,
Mix homogeneously, forms iron salt solutions, and every mM of iron salt adds 15-40ml ethylene glycol；In mass ratio 1:
0.2-0.9 weighing sodium hydroxide and cellulose, join in ethylene glycol, mix homogeneously, forms cellulose
Solution, every gram of cellulose adds 5-20ml ethylene glycol；In iron salt solutions, the quality of iron salt is molten with cellulose
In liquid, the mass ratio of cellulose is 0.1-1.0:1；
2) iron salt solutions and cellulose solution are mixed, stirring, obtain suspended emulsion, suspension is carried out
Microwave-hydrothermal method processes 5-60min, and the temperature of microwave-hydrothermal method processing procedure is 120-220 DEG C, microwave
Hydro-thermal method carries out cooling down after processing, ultrasonic Separation, wash, be dried to obtain product；
3) under inert atmosphere or air atmosphere, product is calcined 1-6h at 300-800 DEG C, cold
But, carbon back magnetic composite is obtained；Described inert atmosphere is in nitrogen, argon, helium
Kind.
The preparation method of carbon back magnetic composite the most according to claim 6, it is characterised in that
Step 2) in the treatment temperature of microwave-hydrothermal method be 180 DEG C, the process time is 10-40min.
The preparation method of carbon back magnetic composite the most according to claim 6, it is characterised in that
Step 3) in calcining heat be 300-500 DEG C, calcination time is 3-6h.
The preparation method of carbon back magnetic composite the most according to claim 6, it is characterised in that
Step 3) described in inert atmosphere be argon.
10. according to the preparation method of the carbon back magnetic composite described in any one of claim 6-9,
It is characterized in that, the saturation magnetization of the composite of preparation is 8.3emu/g～17.6emu/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610133264.3A CN105800695A (en) | 2016-03-09 | 2016-03-09 | Carbon-based magnetic composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610133264.3A CN105800695A (en) | 2016-03-09 | 2016-03-09 | Carbon-based magnetic composite material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105800695A true CN105800695A (en) | 2016-07-27 |
Family
ID=56467870
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610133264.3A Pending CN105800695A (en) | 2016-03-09 | 2016-03-09 | Carbon-based magnetic composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105800695A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107308937A (en) * | 2017-06-30 | 2017-11-03 | 青岛科技大学 | A kind of hydrothermal preparing process of carbon base catalyst for paranitrophenol catalytic hydrogenation |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337695A (en) * | 2008-08-07 | 2009-01-07 | 上海交通大学 | Method for preparing nanometer ferroferric oxide microballoons with particle diameter adjustable by microwave |
| CN102976416A (en) * | 2012-12-04 | 2013-03-20 | 东华大学 | Preparation method of hollow superparamagnetic nanospheres |
| CN103599737A (en) * | 2013-11-20 | 2014-02-26 | 北京化工大学 | Magnetic nano material with carbon shell layer and preparation method thereof |
| CN104028214A (en) * | 2014-04-02 | 2014-09-10 | 安徽农业大学 | Preparation method for agriculture biomass carbon-based magnetic adsorption material |
| CN104117329A (en) * | 2014-07-21 | 2014-10-29 | 太原理工大学 | Preparation method of carbon-coated ferroferric oxide magnetic microspheres |
-
2016
- 2016-03-09 CN CN201610133264.3A patent/CN105800695A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337695A (en) * | 2008-08-07 | 2009-01-07 | 上海交通大学 | Method for preparing nanometer ferroferric oxide microballoons with particle diameter adjustable by microwave |
| CN102976416A (en) * | 2012-12-04 | 2013-03-20 | 东华大学 | Preparation method of hollow superparamagnetic nanospheres |
| CN103599737A (en) * | 2013-11-20 | 2014-02-26 | 北京化工大学 | Magnetic nano material with carbon shell layer and preparation method thereof |
| CN104028214A (en) * | 2014-04-02 | 2014-09-10 | 安徽农业大学 | Preparation method for agriculture biomass carbon-based magnetic adsorption material |
| CN104117329A (en) * | 2014-07-21 | 2014-10-29 | 太原理工大学 | Preparation method of carbon-coated ferroferric oxide magnetic microspheres |
Non-Patent Citations (2)
| Title |
|---|
| XIANLUO HU ET AL.: ""Microwave-assisted synthesis of a superparamagnetic surface functionalized porous Fe3O4/Cnanocomposite"", 《CHEM.ASIAN J.》 * |
| 田禾等: "《精细化工产品手册 信息用化学品》", 30 November 2002, 化学工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107308937A (en) * | 2017-06-30 | 2017-11-03 | 青岛科技大学 | A kind of hydrothermal preparing process of carbon base catalyst for paranitrophenol catalytic hydrogenation |
| CN107308937B (en) * | 2017-06-30 | 2020-10-23 | 青岛科技大学 | Application of carbon-based catalyst in catalytic hydrogenation reaction of p-nitrophenol |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Deraz | Glycine-assisted fabrication of nanocrystalline cobalt ferrite system | |
| Kurmoo et al. | Formation of nanoparticles of ε-Fe2O3 from yttrium iron garnet in a silica matrix: An unusually hard magnet with a Morin-like transition below 150 K | |
| CN101332515B (en) | Preparation method of fibrous iron-nickel alloy powder | |
| Zhang et al. | Synthesis and characterization of SrFe12O19/CoFe2O4 nanocomposites with core-shell structure | |
| CN104437372B (en) | A kind of original position prepares the method for ferroso-ferric oxide/charcoal/graphite nanosheets nano composite material | |
| Paramasivan et al. | A novel approach: hydrothermal method of fine stabilized superparamagnetics of cobalt ferrite (CoFe 2 O 4) nanoparticles | |
| CN104045336B (en) | The preparation method of nickel ferrite magnetic nano-fiber material | |
| Dai et al. | Entropy-driven phase regulation of high-entropy transition metal oxide and its enhanced high-temperature microwave absorption by in-situ dual phases | |
| CN105948085A (en) | Preparation method of magnetic hydrotalcite | |
| Bohlender et al. | Phase formation, magnetic properties, and phase stability in reducing atmosphere of M-type strontium hexaferrite nanoparticles synthesized via a modified citrate process | |
| Saemian et al. | Synthesis of CoFe2O4@ Cu3 (BTC) 2 nanocomposite as a magnetic metal–organic framework | |
| CN105800695A (en) | Carbon-based magnetic composite material and preparation method thereof | |
| CN105081338B (en) | Method for preparing mono-dispersed NdFeB nano particles | |
| KR101328195B1 (en) | Nickel ferrite nano composite and method for manufacturing thereof | |
| CN106277075A (en) | A kind of lanthanum, nickel are co-doped with BaFe12o19nano-powder and preparation method thereof | |
| Paramasivan et al. | Comparative investigation of NiFe2O4 nano and microstructures for structural, optical, magnetic and catalytic properties | |
| Yan et al. | Preparation and morphology of nano-size ceria by a stripping precipitation using oxalic acid as a precipitating agent | |
| CN102744419A (en) | Morphology control method of magnetic nanometer particles | |
| Zhao et al. | Fabrication and characterization of uniform Fe3O4 octahedral micro-crystals | |
| CN105436510A (en) | Method for preparing chemical and magnetic ordered-phase nanoparticles | |
| Trofimova et al. | Anion-exchange synthesis of copper ferrite powders | |
| CN107021520B (en) | A kind of yttrium oxide powder and preparation method thereof | |
| CN106890644B (en) | A kind of ferrocobalt microstructure catalyst material, preparation method and application | |
| CN109678118A (en) | A kind of preparation method of metal oxide nanoparticles and metal nanoparticle | |
| Hamedoun et al. | Physical properties of Co (Mn) Fe2O4 nanomaterials |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160727 |
|
| RJ01 | Rejection of invention patent application after publication |