CN115072785A - Preparation method of manganous-manganic oxide nanoparticles - Google Patents
Preparation method of manganous-manganic oxide nanoparticles Download PDFInfo
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- CN115072785A CN115072785A CN202210926082.7A CN202210926082A CN115072785A CN 115072785 A CN115072785 A CN 115072785A CN 202210926082 A CN202210926082 A CN 202210926082A CN 115072785 A CN115072785 A CN 115072785A
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- trimanganese tetroxide
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 title claims abstract description 5
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 74
- 239000002904 solvent Substances 0.000 claims abstract description 33
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000010415 colloidal nanoparticle Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 150000003904 phospholipids Chemical class 0.000 claims abstract description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 9
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 7
- 239000007810 chemical reaction solvent Substances 0.000 claims abstract description 7
- CNFDGXZLMLFIJV-UHFFFAOYSA-L manganese(II) chloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Mn+2] CNFDGXZLMLFIJV-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002798 polar solvent Substances 0.000 abstract description 8
- 239000006185 dispersion Substances 0.000 abstract description 3
- 230000003993 interaction Effects 0.000 abstract description 3
- 239000012046 mixed solvent Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of manganous-manganic oxide nano particles, which comprises the following steps: the method comprises the following steps: adding manganese chloride tetrahydrate into the reaction solvent ethanolamine, and uniformly stirring to ensure that the solvent fully reacts; step two: emitting ultrasonic waves to the solvent obtained by mixing in the step one to prepare trimanganese tetroxide colloidal nanoparticles; step three: adding a polyethyleneimine solvent and poly (ethylene glycol) phospholipid into the trimanganese tetroxide colloidal nanoparticles prepared in the second step; step four: and D, adding ethanol into the solvent prepared in the step three, and stirring the solvent. According to the technical scheme, the polymine solvent with good water solubility and the poly (ethylene glycol) phospholipid are added into the trimanganese tetroxide colloidal nanoparticles, so that the interaction force among the nanoparticles can be reduced, the dispersion solubility of the nanoparticles in polar solvent water is improved, and the applicability of the trimanganese tetroxide nanoparticles after being prepared is improved.
Description
Technical Field
The invention is applicable to the technical field of auxiliary preparation of manganomanganic oxide, and particularly relates to a preparation method of manganomanganic oxide nanoparticles.
Background
At present, the application of the trimanganese tetroxide nanoparticles to the biomedical field must endow the nanoparticles with higher colloidal stability, good biocompatibility and longer blood circulation time.
However, there are still some disadvantages to the trimanganese tetroxide nanoparticles today: at present, when the trimanganese tetroxide nanoparticles are prepared, the trimanganese tetroxide nanoparticles are prepared under the action of manganese salt and ultrasonic waves, although the preparation requirement is simpler, the particle diameter of the prepared trimanganese tetroxide nanoparticles is overlarge and uneven in distribution, and the trimanganese tetroxide nanoparticles are not easy to disperse and dissolve in polar solvent water, so that the applicability of the prepared trimanganese tetroxide nanoparticles is influenced, and the subsequent biomedical use is influenced. Therefore, we propose a preparation method of trimanganese tetroxide nanoparticles.
Disclosure of Invention
The invention mainly aims to provide a preparation method of manganous-manganic oxide nano particles, which can effectively solve the problems in the background technology.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of manganomanganic oxide nanoparticles comprises the following steps:
the method comprises the following steps: adding manganese chloride tetrahydrate into the reaction solvent ethanolamine, and uniformly stirring to ensure that the solvent fully reacts;
step two: emitting ultrasonic waves to the solvent obtained by mixing in the step one to prepare trimanganese tetroxide colloidal nanoparticles;
step three: adding a polyethyleneimine solvent and poly (ethylene glycol) phospholipid into the trimanganese tetroxide colloidal nanoparticles prepared in the second step, and continuously stirring and mixing to increase the water solubility of colloidal particles;
step four: adding ethanol into the solvent prepared in the third step, and stirring the solvent;
step five: and 4, heating, filtering, washing and drying the solvent prepared in the step four to prepare the trimanganese tetroxide nano-particles.
As a preferred embodiment of the present invention, the particle diameter of the trimanganese tetroxide colloidal particles prepared in the fifth step is less than 12 nm.
In a preferred embodiment of the present invention, the heating reaction temperature in the fifth step is between 70 ℃ and 140 ℃.
In a preferred embodiment of the present invention, the ultrasonic wave is applied for 1 to 2 hours in the second step.
In a preferred embodiment of the present invention, the concentration of the ethanolamine solution used in the first step is 0.1 to 1 mol/L.
In a preferred embodiment of the present invention, the reaction temperature in the first step is 20 to 30 ℃.
In a preferred embodiment of the present invention, the heating reaction time in the fifth step is 6 to 12 hours.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, by adding the polyethyleneimine solvent with good water solubility and the poly (ethylene glycol) phospholipid into the trimanganese tetroxide colloidal nanoparticles, the interaction force between the nanoparticles can be reduced, and the dispersion solubility of the nanoparticles in polar solvent water is improved, so that the trimanganese tetroxide colloidal particles which are originally prepared and are insoluble in the polar solvent water can be dissolved in the polar solvent water, and further the trimanganese tetroxide nanoparticles prepared have good water solubility and biocompatibility, and the particle diameter of the nanoparticles prepared can be changed and controlled by adding the ethanol solvent and controlling the reaction temperature, and further the applicability of the trimanganese tetroxide nanoparticles after being prepared is improved.
Detailed Description
The invention provides a technical scheme that: a preparation method of manganomanganic oxide nanoparticles comprises the following steps: the method comprises the following steps: adding manganese chloride tetrahydrate into the reaction solvent ethanolamine, and uniformly stirring to ensure that the solvent fully reacts; step two: emitting ultrasonic waves to the solvent obtained by mixing in the step one to prepare trimanganese tetroxide colloidal nanoparticles; step three: adding a polyethyleneimine solvent and poly (ethylene glycol) phospholipid into the trimanganese tetroxide colloidal nanoparticles prepared in the second step, and continuously stirring and mixing to increase the water solubility of colloidal particles; step four: adding ethanol into the solvent prepared in the third step, and stirring the solvent; step five: and 4, heating, filtering, washing and drying the solvent prepared in the step four to prepare the trimanganese tetroxide nano-particles.
Example one
Adding manganese chloride tetrahydrate into ethanolamine with the concentration of a reaction solvent of 0.1-1 mol/L, stirring uniformly in a reaction environment with the reaction temperature of 20-30 ℃ to enable the solvent to react fully, then adding a polyethyleneimine solvent and poly (ethylene glycol) phospholipid, continuously stirring and mixing, simultaneously emitting ultrasonic waves to the mixed solvent to enable the action time of the ultrasonic waves to be 1-2 h, then adding ethanol into the mixed solvent, heating the mixed solvent to 70-140 ℃, continuously stirring and mixing, keeping the heating time to be 6-12 h, after the full reaction is completed, carrying out suction filtration, washing and drying treatment on the mixed solvent to prepare the trimanganese tetroxide nanoparticles with the particle diameter smaller than 12 nm and easy to dissolve in polar solvent water.
Comparison example 1
Adding manganese chloride tetrahydrate into ethanolamine with the concentration of a reaction solvent of 0.1-1 mol/L, stirring uniformly in a reaction environment with the reaction temperature of 20-30 ℃ to enable the solvent to react fully, then adding polyethyleneimine solvent and poly (ethylene glycol) phospholipid, continuously stirring and mixing, emitting ultrasonic waves to the mixed solvent to enable the action time of the ultrasonic waves to be 1-2 h, standing for full reaction, and carrying out suction filtration, washing and drying treatment on the mixed solvent to prepare the trimanganese tetroxide nanoparticles.
Comparative example two
Adding manganese chloride tetrahydrate into ethanolamine with the concentration of a reaction solvent of 0.1-1 mol/L, stirring uniformly in a reaction environment with the reaction temperature of 20-30 ℃ to enable the solvent to react fully, then adding ethanol into the mixed solvent, heating the mixed solvent to 70-140 ℃, continuously stirring and mixing the mixed solvent, keeping the heating time at 6-12 h, after the full reaction is completed, carrying out suction filtration, washing and drying treatment on the mixed solvent, and preparing the trimanganese tetroxide nanoparticles with the particle diameter of less than 12 nanometers and easy solubility in polar solvent water.
The data of the first comprehensive example, the first comparative example and the second comparative example are as follows:
according to the invention, the polymine solvent and the poly (ethylene glycol) phospholipid with good water solubility are added into the trimanganese tetroxide colloidal nanoparticles, so that the interaction force among the nanoparticles can be reduced, the dispersion solubility of the nanoparticles in polar solvent water is improved, and the particle diameter of the prepared nanoparticles can be changed and controlled by adding the ethanol solvent and controlling the reaction temperature, thereby improving the applicability of the trimanganese tetroxide nanoparticles after being prepared.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. A preparation method of manganous-manganic oxide nano particles is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: adding manganese chloride tetrahydrate into the reaction solvent ethanolamine, and uniformly stirring to ensure that the solvent fully reacts;
step two: emitting ultrasonic waves to the solvent obtained by mixing in the step one to prepare trimanganese tetroxide colloidal nanoparticles;
step three: adding a polyethyleneimine solvent and poly (ethylene glycol) phospholipid into the trimanganese tetroxide colloidal nanoparticles prepared in the second step, and continuously stirring and mixing to increase the water solubility of colloidal particles;
step four: adding ethanol into the solvent prepared in the third step, and stirring the solvent;
step five: and 4, heating, filtering, washing and drying the solvent prepared in the step four to prepare the trimanganese tetroxide nano-particles.
2. The method for preparing manganomanganic oxide nanoparticles as claimed in claim 1, wherein the method comprises the following steps: the particle diameter of the trimanganese tetroxide colloidal particles prepared in the fifth step is less than 12 nanometers.
3. The method for preparing manganomanganic oxide nanoparticles as claimed in claim 1, wherein the method comprises the following steps: and the heating reaction temperature in the fifth step is between 70 and 140 ℃.
4. The method for preparing manganomanganic oxide nanoparticles as claimed in claim 1, wherein the method comprises the following steps: and the action time of the ultrasonic wave in the second step is 1-2 h.
5. The method for preparing manganomanganic oxide nanoparticles as claimed in claim 1, wherein the method comprises the following steps: the concentration of the ethanolamine solution used in the first step is 0.1-1 mol/L.
6. The method for preparing manganomanganic oxide nanoparticles as claimed in claim 1, wherein the method comprises the following steps: the reaction temperature in the first step is 20-30 ℃.
7. The method for preparing manganomanganic oxide nanoparticles as claimed in claim 1, wherein the method comprises the following steps: and the heating reaction time in the fifth step is 6-12 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210926082.7A CN115072785A (en) | 2022-08-03 | 2022-08-03 | Preparation method of manganous-manganic oxide nanoparticles |
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| CN202210926082.7A CN115072785A (en) | 2022-08-03 | 2022-08-03 | Preparation method of manganous-manganic oxide nanoparticles |
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| CN115072785A true CN115072785A (en) | 2022-09-20 |
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| CN202210926082.7A Pending CN115072785A (en) | 2022-08-03 | 2022-08-03 | Preparation method of manganous-manganic oxide nanoparticles |
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Citations (8)
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|---|---|---|---|---|
| KR20090129935A (en) * | 2008-06-13 | 2009-12-17 | 성균관대학교산학협력단 | Hollow nanoparticles containing paramagnetic material as mri contrast agent and drug delivery system using the same |
| US20120114564A1 (en) * | 2007-01-30 | 2012-05-10 | Seoul National University Industry Foundation | Mri t1 contrasting agent comprising manganese oxide nanoparticle |
| CN104056284A (en) * | 2013-10-17 | 2014-09-24 | 华东师范大学 | MPEG-DA-MnO nano contrast agent with different surface modification density and preparation method and use thereof |
| CN104274842A (en) * | 2014-10-13 | 2015-01-14 | 东华大学 | Method for preparing multifunctional manganous manganic oxide nano-particle nuclear magnetic resonance contrast agent mediated by polyethyleneimine |
| CN105770922A (en) * | 2016-03-08 | 2016-07-20 | 东华大学 | Method for preparing 64 Cu marked and folic acid targeted functional trimanganese tetroxide nano-particles with stable polyethyleneimine |
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-
2022
- 2022-08-03 CN CN202210926082.7A patent/CN115072785A/en active Pending
Patent Citations (8)
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| US20120114564A1 (en) * | 2007-01-30 | 2012-05-10 | Seoul National University Industry Foundation | Mri t1 contrasting agent comprising manganese oxide nanoparticle |
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Application publication date: 20220920 |