CN111517370A - Preparation method of magnetic ferroferric oxide nanoparticles - Google Patents
Preparation method of magnetic ferroferric oxide nanoparticles Download PDFInfo
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- CN111517370A CN111517370A CN201910102723.5A CN201910102723A CN111517370A CN 111517370 A CN111517370 A CN 111517370A CN 201910102723 A CN201910102723 A CN 201910102723A CN 111517370 A CN111517370 A CN 111517370A
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- ferroferric oxide
- magnetic ferroferric
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- ferric trichloride
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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 34
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000009835 boiling Methods 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000003599 detergent Substances 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 238000010992 reflux Methods 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 239000000725 suspension Substances 0.000 claims abstract description 3
- 239000007966 viscous suspension Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 239000002245 particle Substances 0.000 abstract description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 6
- 230000007062 hydrolysis Effects 0.000 abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000004094 surface-active agent Substances 0.000 abstract description 4
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 27
- 238000003760 magnetic stirring Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 239000012295 chemical reaction liquid Substances 0.000 description 4
- 230000005415 magnetization Effects 0.000 description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 3
- 229940032296 ferric chloride Drugs 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229940031182 nanoparticles iron oxide Drugs 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000004038 photonic crystal Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
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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
- C01G49/06—Ferric oxide [Fe2O3]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a preparation method of magnetic ferroferric oxide nanoparticles. The preparation method comprises the following steps: 1) adding ferric trichloride, sodium hydroxide and deionized water into ethylene glycol, and fully stirring to obtain a brown yellow viscous suspension; 2) heating the suspension obtained in the step 1) to boiling, keeping boiling and refluxing for 4-12 hours, stopping heating, cooling to room temperature, performing centrifugal separation to remove liquid, washing with a detergent, and drying to obtain magnetic ferroferric oxide nano particle powder. The method adopts ferric trichloride as an iron source, ethylene glycol as a solvent and a reducing agent and sodium hydroxide as a hydrolysis promoter, and the reaction is carried out in a normal-pressure open container, a high-pressure closed container is not required, and any surfactant is not used, so that the magnetic ferroferric oxide nano particles with the particle size of 30-100nm, uniform size, high crystallinity and good dispersibility can be prepared. The preparation method has simple process and low cost of raw materials, and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a preparation method of magnetic ferroferric oxide nano particles.
Background
The magnetic ferroferric oxide nano particle has unique magnetic property and good biocompatibility, has wide application prospect in the fields of information storage, biomedicine, industrial catalysis, water treatment and the like, and is a functional nano material with great development potential. At present, the methods for preparing the ferroferric oxide nano particles mainly comprise a coprecipitation method, an organic phase thermal decomposition method, a microemulsion method, a solvothermal method and the like. These methods have advantages and disadvantages, and are difficult to meet the requirements of different applications. A solvothermal method (Angew. chem. int. Ed.,2005,44: 2782-. However, the method needs to be carried out in a high-pressure closed container, the preparation process is complex, the cost of the used raw materials such as carboxylate, polyethylene glycol and the like is high, and the method is not beneficial to large-scale industrial production. Meanwhile, the size of the particles prepared by the method is large, and the ferroferric oxide nano particles with uniform size below 100nm are difficult to prepare.
Disclosure of Invention
Aiming at the problems of the existing method, the invention provides the preparation method of the magnetic ferroferric oxide nano particles, which has simple process and low raw material cost and is suitable for large-scale production. The method adopts ferric trichloride as an iron source, ethylene glycol as a solvent and a reducing agent, sodium hydroxide as a hydrolysis promoter, and does not use any surfactant, the reaction is carried out in a normal-pressure open container, a high-pressure closed reaction container is not needed, and the magnetic ferroferric oxide nano particles with the particle size of 30-100nm, uniform size, high crystallinity and good dispersibility can be prepared.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of magnetic ferroferric oxide nanoparticles comprises the following steps:
1) adding ferric trichloride, sodium hydroxide and deionized water into ethylene glycol, and fully stirring to obtain a brown yellow viscous suspension;
2) heating the suspension obtained in the step 1) to boiling, keeping boiling and refluxing for 4-12 hours, stopping heating, cooling to room temperature, performing centrifugal separation to remove liquid, washing with a detergent, and drying to obtain magnetic ferroferric oxide nano particle powder.
In the preparation method, the whole reaction process is carried out in a normal-pressure open container without a high-pressure closed container, the reaction device is simple, the cheap and easily obtained sodium hydroxide is used as the hydrolysis promoter in the reaction, any surfactant is not used, the reaction cost is low, and the large-scale industrial production is facilitated.
Preferably, the ferric trichloride in the step 1) is ferric trichloride hexahydrate or anhydrous ferric trichloride.
Preferably, the adding amount of the ferric trichloride in the step 1) is 0.05-0.5 mol/L.
Preferably, the sodium hydroxide is added in the step 1) in an amount of 0.1-2.0 mol/L.
Preferably, the deionized water is added in the step 1) in an amount of 0.5-20 mol/L.
Preferably, the temperature is increased to boiling in step 2) at a rate of 1-10 deg.C/min. More preferably 3 deg.C/min.
Preferably, the detergent is absolute ethanol.
Preferably, the drying is vacuum drying; it will be readily understood by those skilled in the art that the drying herein may also be other conventional drying means such as blower drying, low temperature drying, etc.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention can carry out reaction in a normal-pressure open container without a high-pressure closed container, has simple reaction device and is easy to realize large-scale production.
(2) Cheap and easily available ferric trichloride is used as an iron source, sodium hydroxide is used as a hydrolysis promoter, any surfactant is not used, and the raw material cost is low.
(3) The invention can prepare magnetic iron oxide nano particles with the particle size of 30-100nm, and enlarges the application range of preparing a ferroferric oxide nano reaction system in the ethylene glycol solution. The obtained magnetic ferroferric oxide nano particles have good crystallinity, high saturation magnetization, uniform size and easy dispersion in aqueous solution, and have wide application prospect in the fields of oilfield sewage treatment, drug delivery, photonic crystals, industrial catalysis and the like.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of the magnetic ferroferric oxide nanoparticles obtained in example 1.
FIG. 2 is an X-ray diffraction (XRD) spectrum of the magnetic ferroferric oxide nanoparticles obtained in example 1.
FIG. 3 is a room temperature magnetization curve of the magnetic ferroferric oxide nanoparticles obtained in example 1.
Fig. 4 is a Scanning Electron Microscope (SEM) image of the magnetic ferroferric oxide nanoparticles obtained in example 2.
FIG. 5 is a Scanning Electron Microscope (SEM) image of the magnetic ferroferric oxide nanoparticles obtained in example 3.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Example 1
Weighing 0.004mol of anhydrous ferric chloride and 0.012mol of sodium hydroxide, adding into 40mL of glycol, and then adding 0.12mol of deionized water; stirring at room temperature to dissolve to form a brown yellow viscous solution; transferring the solution into a 250mL three-neck flask, heating the solution to boiling at the speed of 3 ℃/min under the condition of magnetic stirring, keeping the solution in the boiling state, and gradually changing the solution from brown red to black in the process; and after 8 hours, stopping heating, cooling the reaction liquid to room temperature, separating the product by a centrifugal method, washing the product for 3 times by using absolute ethyl alcohol, and performing vacuum drying at 60 ℃ for 12 hours to obtain black magnetic ferroferric oxide powder.
Fig. 1 is a Scanning Electron Microscope (SEM) image of the magnetic ferroferric oxide nanoparticles obtained in this example, which shows that the average particle size of the obtained ferroferric oxide nanoparticles is about 100nm, and the nanoparticles are spherical, have good dispersibility, and do not agglomerate.
Fig. 2 is an X-ray diffraction (XRD) pattern of the magnetic iron oxide nanoparticles obtained in this example, from which it can be seen that the product has good crystallinity, and the positions and intensities of the diffraction peaks are consistent with the standard pattern of ferroferric oxide.
FIG. 3 is the room temperature magnetization curve of the ferroferric oxide nanoparticles obtained in this example, from which it can be seen that the product is superparamagnetic and the saturation magnetization at room temperature is 65.8 emu/g.
Example 2
Weighing 0.004mol of anhydrous ferric chloride and 0.012mol of sodium hydroxide, adding into 40mL of glycol, and then adding 0.18mol of deionized water; stirring at room temperature to dissolve to form a brown yellow viscous solution; transferring the solution into a 250mL three-neck flask, heating the solution to boiling at the speed of 3 ℃/min under the condition of magnetic stirring, keeping the solution in the boiling state, and gradually changing the solution from brown red to black in the process; and after 8 hours, stopping heating, cooling the reaction liquid to room temperature, separating the product by a centrifugal method, washing the product for 3 times by using absolute ethyl alcohol, and performing vacuum drying at 60 ℃ for 12 hours to obtain black magnetic ferroferric oxide powder.
Fig. 4 is a Scanning Electron Microscope (SEM) image of the magnetic ferriferrous oxide nanoparticles obtained in this example, which shows that the average particle size of the obtained ferriferrous oxide nanoparticles is about 70 nm.
Example 3
Weighing 0.004mol of anhydrous ferric chloride and 0.012mol of sodium hydroxide, adding into 40mL of glycol, and then adding 0.24mol of deionized water; stirring at room temperature to dissolve to form a brown yellow viscous solution; transferring the solution into a 250mL three-neck flask, heating the solution to boiling at the speed of 3 ℃/min under the condition of magnetic stirring, keeping the solution in the boiling state, and gradually changing the solution from brown red to black in the process; and after 8 hours, stopping heating, cooling the reaction liquid to room temperature, separating the product by a centrifugal method, washing the product for 3 times by using absolute ethyl alcohol, and performing vacuum drying at 60 ℃ for 12 hours to obtain black magnetic ferroferric oxide powder.
Fig. 5 is a Scanning Electron Microscope (SEM) image of the magnetic ferriferrous oxide nanoparticles obtained in this example, which shows that the average particle size of the obtained ferriferrous oxide nanoparticles is about 50 nm.
Example 4
Weighing 0.005mol of ferric chloride hexahydrate, 0.01425mol of sodium hydroxide and 0.13mol of deionized water, adding into 50mL of ethylene glycol, and fully stirring to form a brown yellow viscous solution; transferring the solution into a 250mL three-neck flask, heating the solution to boiling at the speed of 5 ℃/min under the condition of magnetic stirring, keeping the solution in the boiling state, and gradually changing the solution from brown red to black in the process; stopping heating after 12h, cooling the reaction liquid to room temperature, separating the product by a centrifugal method, washing the product for 3 times by absolute ethyl alcohol, and performing vacuum drying at 60 ℃ for 12h to obtain black magnetic ferroferric oxide powder.
Example 5
Weighing 0.005mol of ferric chloride hexahydrate, 0.01475mol of sodium hydroxide and 0.15mol of deionized water, adding into 50mL of ethylene glycol, and fully stirring to form a brown yellow viscous solution; transferring the solution into a 250mL three-neck flask, heating the solution to boiling at the speed of 5 ℃/min under the condition of magnetic stirring, keeping the solution in the boiling state, and gradually changing the solution from brown red to black in the process; and stopping heating after 6h, cooling the reaction solution to room temperature, separating the product by a centrifugal method, washing the product for 3 times by absolute ethyl alcohol, and performing vacuum drying at 60 ℃ for 12h to obtain black magnetic ferroferric oxide powder.
Other examples are as follows:
the black magnetic ferroferric oxide powder is obtained smoothly in the above embodiments, the particle size of the black magnetic ferroferric oxide powder is about 30-100nm, the nano particles are spherical, the dispersibility is good, and the black magnetic ferroferric oxide powder is not agglomerated.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (8)
1. A preparation method of magnetic ferroferric oxide nanoparticles is characterized by comprising the following steps:
1) adding ferric trichloride, sodium hydroxide and deionized water into ethylene glycol, and fully stirring to obtain a brown yellow viscous suspension;
2) heating the suspension obtained in the step 1) to boiling, keeping boiling and refluxing for 4-12 hours, stopping heating, cooling to room temperature, performing centrifugal separation to remove liquid, washing with a detergent, and drying to obtain magnetic ferroferric oxide nano particle powder.
2. The method according to claim 1, wherein the ferric trichloride in the step 1) is ferric trichloride hexahydrate or anhydrous ferric trichloride.
3. The method according to claim 1, wherein the ferric trichloride is added in an amount of 0.05 to 0.5mol/L in the step 1).
4. The method according to claim 1, wherein the sodium hydroxide is added in the amount of 0.1 to 2.0mol/L in the step 1).
5. The method according to claim 1, wherein the deionized water is added in the step 1) in an amount of 0.5 to 20 mol/L.
6. The method according to claim 1, wherein the heating is carried out at a rate of 1-10 ℃/min until boiling in step 2).
7. The method of claim 1, wherein the detergent is absolute ethanol.
8. The method of claim 1, wherein the drying is vacuum drying.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661195A (en) * | 2020-12-23 | 2021-04-16 | 青岛科技大学 | Preparation method of subminiature magnetic ferroferric oxide nanoparticles |
| CN113247959A (en) * | 2021-06-09 | 2021-08-13 | 东北大学 | Method for preparing functional iron oxide nanoparticles by using machine head ash as raw material |
| CN116119796A (en) * | 2023-03-03 | 2023-05-16 | 斯坦德技术工程(青岛)有限公司 | Ferroferric oxide nano-composite adsorption flocculant and preparation method thereof |
-
2019
- 2019-02-01 CN CN201910102723.5A patent/CN111517370A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| SABA JAMIL等: ""Microwave Assisted Reflux Synthesis and Characterization of Magnetic Fe3O4 MicroBubbles Embedin Nano particles"", 《ADVANCED MATERIALS RESEARCH》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661195A (en) * | 2020-12-23 | 2021-04-16 | 青岛科技大学 | Preparation method of subminiature magnetic ferroferric oxide nanoparticles |
| CN113247959A (en) * | 2021-06-09 | 2021-08-13 | 东北大学 | Method for preparing functional iron oxide nanoparticles by using machine head ash as raw material |
| CN116119796A (en) * | 2023-03-03 | 2023-05-16 | 斯坦德技术工程(青岛)有限公司 | Ferroferric oxide nano-composite adsorption flocculant and preparation method thereof |
| CN116119796B (en) * | 2023-03-03 | 2023-07-14 | 斯坦德技术工程(青岛)有限公司 | Ferroferric oxide nano-composite adsorption flocculant and preparation method thereof |
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