CN110615483A - Method for preparing magnetic ferroferric oxide nanoparticles by hydrothermal method - Google Patents
Method for preparing magnetic ferroferric oxide nanoparticles by hydrothermal method Download PDFInfo
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- CN110615483A CN110615483A CN201810635979.8A CN201810635979A CN110615483A CN 110615483 A CN110615483 A CN 110615483A CN 201810635979 A CN201810635979 A CN 201810635979A CN 110615483 A CN110615483 A CN 110615483A
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- CN
- China
- Prior art keywords
- oxide nanoparticles
- ferroferric oxide
- trisodium citrate
- ethylene glycol
- ferric trichloride
- Prior art date
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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 27
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 26
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 68
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 25
- 239000001509 sodium citrate Substances 0.000 claims abstract description 25
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 25
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 25
- 238000005303 weighing Methods 0.000 claims abstract description 20
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 13
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 13
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- DGPIGKCOQYBCJH-UHFFFAOYSA-M sodium;acetic acid;hydroxide Chemical compound O.[Na+].CC([O-])=O DGPIGKCOQYBCJH-UHFFFAOYSA-M 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 11
- 239000004005 microsphere Substances 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 6
- 238000003756 stirring Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 206010028980 Neoplasm Diseases 0.000 abstract 1
- 238000003759 clinical diagnosis Methods 0.000 abstract 1
- 239000011521 glass Substances 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 239000002122 magnetic nanoparticle Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 239000000126 substance Substances 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
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention provides a method for preparing magnetic ferroferric oxide nanoparticles by a hydrothermal method in the neighborhood of tumor clinical diagnosis technology, which comprises the steps of firstly weighing ferric trichloride hexahydrate, trisodium citrate, sodium acetate hydrate and ethylene glycol in a certain amount, then respectively adding the ferric trichloride hexahydrate and the trisodium citrate into the ethylene glycol, stirring and fully dissolving, then adding ethylene glycol solution in which the ferric trichloride hexahydrate and the trisodium citrate are dissolved into polytetrafluoroethylene, naturally cooling to room temperature after a high-pressure high-temperature sealing reaction is carried out for a certain time, washing for a plurality of times by deionized water to obtain the ferroferric oxide nanoparticles serving as a liquid to be detected, and finally observing microspheres by an electron microscope to obtain the morphology of the microspheres; compared with the prior art, the invention has the beneficial effects that: the preparation method is simple, the time consumption is short, the particle size distribution of the prepared particles is narrow, and the shape of the microsphere particles is ideal.
Description
Technology neighborhood
The invention relates to a preparation method, in particular to a method for preparing magnetic ferroferric oxide nanoparticles by a hydrothermal method.
Background
Ferroferric oxide (Fe)304) The magnetic nanoparticles have the characteristics of simple preparation, high stability, low cost, good biocompatibility, good magnetic responsiveness, easy surface modification and the like, and become one of the most widely applied magnetic nanoparticles at present. In recent years, Fe was synthesized304Magnetic nanoparticles are prepared more and more by common physical methods, but the physical methods are simple to operate but time-consuming, the particle size distribution of the prepared particles is wide, the shapes of the microspheres are not ideal, and Fe synthesized by a chemical method304The magnetic nanoparticles have obvious advantages in activity, size and form control.
Disclosure of Invention
Aiming at overcoming the defects in the prior art, the invention provides a method for preparing magnetic ferroferric oxide nanoparticles by a hydrothermal method, which has the advantages of simple preparation method, short time consumption, narrow particle size distribution of the prepared particles and ideal shape and appearance of the microsphere particles.
The purpose of the invention is realized by the following technical scheme: a method for preparing magnetic ferroferric oxide nanoparticles by a hydrothermal method comprises the following steps:
(A1) weighing: quantitatively weighing ferric trichloride hexahydrate, trisodium citrate and sodium acetate hydrate, and quantitatively weighing ethylene glycol;
(A2) dissolving: respectively adding ferric trichloride hexahydrate and trisodium citrate into ethylene glycol, and fully dissolving;
(A3) reaction: adding ethylene glycol solution dissolved with ferric trichloride hexahydrate and trisodium citrate into polytetrafluoroethylene, performing high-pressure high-temperature sealing reaction for a certain time, naturally cooling to room temperature, and washing with deionized water for several times to obtain ferroferric oxide nanoparticles as a liquid to be detected;
(A4) and (3) detection: and observing the morphology of the ferroferric oxide nanoparticles by using an electron microscope.
The method comprises the steps of quantitatively weighing ferric trichloride hexahydrate, trisodium citrate and sodium acetate hydrate by using a precision balance, then quantitatively measuring ethylene glycol by using a measuring cylinder, then respectively adding the ferric trichloride hexahydrate and the trisodium citrate into the ethylene glycol, stirring by using a glass rod to fully dissolve the ferric trichloride hexahydrate and the trisodium citrate, then adding a glycol solution in which the ferric trichloride hexahydrate and the trisodium citrate are dissolved into polytetrafluoroethylene, setting pressure and temperature, reacting for a certain time in a high-pressure high-temperature sealed environment, wherein the solubility of hydroxide in water is greater than that of a corresponding oxide in water, so that the hydroxide is dissolved into the water to simultaneously separate out the oxide, finally naturally cooling to room temperature, washing by using deionized water for a plurality of times to obtain ferroferric oxide nanoparticles serving as a liquid to be detected, and finally observing the microspheres by using an electron microscope to obtain the morphology of the microspheres; compared with the prior art, the invention has the beneficial effects that: the preparation method is simple, the time consumption is short, the particle size distribution of the prepared particles is narrow, and the shape of the microsphere particles is ideal.
According to the preparation method, as a further improvement of the invention, the electron microscope method further comprises a scanning electron microscope or a transmission electron microscope.
As a further improvement of the invention, the high pressure is 10MPa to 100 MPa.
As a further improvement of the invention, the high temperature is 100 deg.CoC～200oC。
As a further improvement of the invention, the reaction time is 5 to 12 hours.
Drawings
FIG. 1 is an electron micrograph of microspheres of the present invention.
Detailed Description
Example 1
As shown in fig. 1, a hydrothermal method for preparing magnetic ferroferric oxide nanoparticles comprises the following steps:
(A1) weighing: respectively and quantitatively weighing 0.4g of ferric trichloride hexahydrate, 0.4g of trisodium citrate and 4g of sodium acetate hydrate on weighing paper by using a precision balance, respectively and quantitatively weighing 40mL of ethylene glycol and 100mL of polytetrafluoroethylene by using a measuring cylinder, and placing the ethylene glycol and the polytetrafluoroethylene into two beakers;
(A2) dissolving: adding ferric trichloride hexahydrate and trisodium citrate into a beaker filled with glycol, and stirring by a glass rod to fully dissolve the ferric trichloride hexahydrate and the trisodium citrate;
(A3) reaction: adding ethylene glycol solution dissolved with ferric trichloride hexahydrate and trisodium citrate into a polytetrafluoroethylene beaker at 10MPa and 200%oC, after sealing reaction for 12 hours, naturally cooling to room temperature, and washing for 3 times by using deionized water to obtain ferroferric oxide nanoparticles serving as a liquid to be detected;
(A4) and (3) detection: and observing the morphology of the ferroferric oxide nanoparticles by using an electron microscope.
Example 2
As shown in fig. 1, a hydrothermal method for preparing magnetic ferroferric oxide nanoparticles comprises the following steps:
(A1) weighing: respectively and quantitatively weighing 0.2g of ferric trichloride hexahydrate, 0.2g of trisodium citrate and 2g of sodium acetate hydrate on weighing paper by using a precision balance, respectively and quantitatively weighing 20mL of ethylene glycol and 100mL of polytetrafluoroethylene by using a measuring cylinder, and putting the ethylene glycol and the polytetrafluoroethylene into two beakers;
(A2) dissolving: adding ferric trichloride hexahydrate and trisodium citrate into a beaker filled with glycol, and stirring by a glass rod to fully dissolve the ferric trichloride hexahydrate and the trisodium citrate;
(A3) reaction: adding ethylene glycol solution dissolved with ferric trichloride hexahydrate and trisodium citrate into a polytetrafluoroethylene beaker at 50MPa and 200%oC, after sealing reaction for 10 hours, naturally cooling to room temperature, and washing for 3 times by using deionized water to obtain ferroferric oxide nanoparticles serving as a liquid to be detected;
(A4) and (3) detection: and observing the morphology of the ferroferric oxide nanoparticles by using an electron microscope.
Example 3
As shown in fig. 1, a hydrothermal method for preparing magnetic ferroferric oxide nanoparticles comprises the following steps:
(A1) weighing: respectively and quantitatively weighing 0.3g of ferric trichloride hexahydrate, 0.3g of trisodium citrate and 3g of sodium acetate hydrate on weighing paper by using a precision balance, respectively and quantitatively weighing 30mL of ethylene glycol and 100mL of polytetrafluoroethylene by using a measuring cylinder, and placing the ethylene glycol and the polytetrafluoroethylene into two beakers;
(A2) dissolving: adding ferric trichloride hexahydrate and trisodium citrate into a beaker filled with glycol, and stirring by a glass rod to fully dissolve the ferric trichloride hexahydrate and the trisodium citrate;
(A3) reaction: adding ethylene glycol solution dissolved with ferric trichloride hexahydrate and trisodium citrate into a polytetrafluoroethylene beaker at 100MPa and 100 DEG CoC, after sealing reaction for 5 hours, naturally cooling to room temperature, and washing for 3 times by using deionized water to obtain ferroferric oxide nanoparticles serving as a liquid to be detected;
(A4) and (3) detection: and observing the morphology of the ferroferric oxide nanoparticles by using an electron microscope.
The present invention is not limited to the above embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make various substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (5)
1. A method for preparing magnetic ferroferric oxide nanoparticles by a hydrothermal method is characterized by comprising the following steps:
(A1) weighing: quantitatively weighing ferric trichloride hexahydrate, trisodium citrate and sodium acetate hydrate, and quantitatively weighing ethylene glycol;
(A2) dissolving: respectively adding ferric trichloride hexahydrate and trisodium citrate into ethylene glycol, and fully dissolving;
(A3) reaction: adding ethylene glycol solution dissolved with ferric trichloride hexahydrate and trisodium citrate into polytetrafluoroethylene, performing high-pressure high-temperature sealing reaction for a certain time, naturally cooling to room temperature, and washing with deionized water for several times to obtain ferroferric oxide nanoparticles as a liquid to be detected;
(A4) and (3) detection: and observing the morphology of the ferroferric oxide nanoparticles by using an electron microscope.
2. The hydrothermal method for preparing magnetic ferroferric oxide nanoparticles according to claim 1, wherein in the step (A4), the electron microscope comprises a scanning electron microscope or a transmission electron microscope.
3. The hydrothermal method for preparing magnetic ferroferric oxide nanoparticles according to claim 1, wherein the high pressure is 10MPa to 100 MPa.
4. The hydrothermal method for preparing magnetic ferroferric oxide nanoparticles according to claim 1, wherein the high temperature is 100 ℃oC～200oC。
5. The hydrothermal method for preparing magnetic ferroferric oxide nanoparticles according to claim 1, wherein the reaction time is 5-12 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810635979.8A CN110615483A (en) | 2018-06-20 | 2018-06-20 | Method for preparing magnetic ferroferric oxide nanoparticles by hydrothermal method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810635979.8A CN110615483A (en) | 2018-06-20 | 2018-06-20 | Method for preparing magnetic ferroferric oxide nanoparticles by hydrothermal method |
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| Publication Number | Publication Date |
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| CN110615483A true CN110615483A (en) | 2019-12-27 |
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| CN201810635979.8A Pending CN110615483A (en) | 2018-06-20 | 2018-06-20 | Method for preparing magnetic ferroferric oxide nanoparticles by hydrothermal method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108840371A (en) * | 2018-06-29 | 2018-11-20 | 复旦大学 | A kind of preparation method of ferroso-ferric oxide/manganese dioxide complex microsphere |
| CN112591802A (en) * | 2020-12-04 | 2021-04-02 | 暨南大学 | Preparation method of hollow ferroferric oxide drug-loaded nanoparticles |
| CN112607785A (en) * | 2020-12-23 | 2021-04-06 | 浙江理工大学 | MnFe2O4/C nano composite microsphere and preparation method thereof |
-
2018
- 2018-06-20 CN CN201810635979.8A patent/CN110615483A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108840371A (en) * | 2018-06-29 | 2018-11-20 | 复旦大学 | A kind of preparation method of ferroso-ferric oxide/manganese dioxide complex microsphere |
| CN112591802A (en) * | 2020-12-04 | 2021-04-02 | 暨南大学 | Preparation method of hollow ferroferric oxide drug-loaded nanoparticles |
| CN112607785A (en) * | 2020-12-23 | 2021-04-06 | 浙江理工大学 | MnFe2O4/C nano composite microsphere and preparation method thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20191227 |
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| WD01 | Invention patent application deemed withdrawn after publication |