CN103833087B - The microwave synthesis method of a kind of water-soluble ferroferric oxide nano particle - Google Patents
The microwave synthesis method of a kind of water-soluble ferroferric oxide nano particle Download PDFInfo
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- CN103833087B CN103833087B CN201410090607.3A CN201410090607A CN103833087B CN 103833087 B CN103833087 B CN 103833087B CN 201410090607 A CN201410090607 A CN 201410090607A CN 103833087 B CN103833087 B CN 103833087B
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Abstract
The microwave synthesis method of a kind of water-soluble ferroferric oxide nano particle, it relates to ferriferrous oxide nano-particle. 1) ferric chloride hexahydrate is added in glycol ether, it is stirred to after it dissolves completely, then adds anhydrous sodium acetate, make it dissolve completely after fully stirring, obtain solution A; 2) step 1) gained solution A is transferred in single port flask, and it is placed in single mold microwave synthesis system, after adopting uncovered pattern to react completely, naturally cool to room temperature, obtain reaction product; 3) by step 2) reaction product that obtains is by magnetic resolution, and after washing, lyophilize preserves, and obtains water-soluble ferroferric oxide nano particle. Prepared nanoparticle has good water-soluble, monodispersity and superparamagnetism, can have good T simultaneously2Contrasting effects, has potential using value at biomedical sector.
Description
Technical field
The present invention relates to ferriferrous oxide nano-particle, especially relate to the microwave synthesis method of a kind of water-soluble ferroferric oxide nano particle.
Background technology
Ferriferrous oxide nano-particle has unique quantum size effect, surface effects, small-size effect and macroscopic quantum effect tunnel effect etc. due to it, make it that there is optical, electrical, hot, sound, magnetic, the sensitivity characteristic that are different from conventional material, there is good biocompatibility simultaneously, thus have broad application prospects in bioseparation, magnetic thermotherapy, tissue repair, drug targeting transmission, nuclear magnetic resonance, immunodetection etc., also more and more receive the concern of biomedical worker.
The method of current synthesis of nano ferriferrous oxide nano-particle mainly contains mechanical attrition method, chemical coprecipitation, pyrolysis method, settlement-oxidation method, sol method, microemulsion method etc.
Chinese patent CN102887546A discloses the preparation method of a kind of water-soluble ferroferric oxide nano particle and the water-soluble ferroferric oxide nano particle prepared by the method and application, the method comprises the following steps: (1) is under the existence of phenylcarbinol, the organic precursor of iron is carried out thermolysis, and carry out solid-liquid separation, obtain ferriferrous oxide nano-particle; (2) ferriferrous oxide nano-particle obtained by the ethanol wash step (1) of low carbon chain, to remove phenylcarbinol wherein; (3) water soluble ligand solution is mixed with the ferriferrous oxide nano-particle washed through step (2), obtain water-soluble ferroferric oxide nano particle.
The applicant discloses the preparation method of a kind of water-soluble ferroferric oxide nano particle in Chinese patent CN103274478A, and 1) Anhydrous Ferric Chloride and trisodium citrate are dissolved in glycol ether, it is heated to dissolve completely; 2) to step 1) gained mixing solutions adds sodium acetate, anhydrous, treat that it dissolves completely; 3) by step 2) mixed solution that obtains is placed in reactor, and capping still, after reaction, naturally cools to room temperature; 4) with magnet by ferriferrous oxide nano-particle from step 3) reaction solution that obtains is separated, dry after washing, obtain monodisperse water soluble ferriferrous oxide nano-particle.
But aforesaid method respectively has its defect, such as long reaction time, the required control condition of reaction are too much, to be difficult to modification, cost more high, the ferriferrous oxide nano-particle simultaneously synthesized often is having particle diameter inequality one in varying degrees, bad dispersibility, it is insoluble in a series of problems such as water, thus it is difficult to put in practical application. Microwave heating method, as a kind of novel reaction synthesis process, has that the reaction times is short, an advantage such as assimilated efficiency height, side reaction are few, energy-conserving and environment-protective, has huge advantage in rapidly and efficiently nano materials. But applied to Fast back-projection algorithm have good aqueous solubility and dispersion property small-particle ferriferrous oxide nano-particle be not reported so far.
Summary of the invention
It is an object of the invention to provide the microwave synthesis method of a kind of water-soluble ferroferric oxide nano particle.
The present invention comprises the following steps:
1) ferric chloride hexahydrate is added in glycol ether, it is stirred to after it dissolves completely, then adds anhydrous sodium acetate, make it dissolve completely after fully stirring, obtain solution A;
2) by step 1) gained solution A is transferred in single port flask, and is placed in single mold microwave synthesis system, after adopting uncovered pattern to react completely, naturally cool to room temperature, obtain reaction product;
3) by step 2) reaction product that obtains is by magnetic resolution, and after washing, lyophilize preserves, and obtains water-soluble ferroferric oxide nano particle.
In step 1) in, the proportioning of described ferric chloride hexahydrate, glycol ether, anhydrous sodium acetate can be 0.54g: 20mL: 0.5g, wherein, ferric chloride hexahydrate, anhydrous sodium acetate are calculated in mass, glycol ether is calculated by volume, the volumetric molar concentration of described ferric chloride hexahydrate can be 0.5��4mmol, and the volumetric molar concentration of anhydrous sodium acetate can be 4��8mmol.
In step 2) in, the temperature of described reaction can be 140��220 DEG C, and the time of reaction can be 1��30min; The work power of described single mold microwave synthesis system can be 40��200W.
In step 3) in, described washing can use ethanol, ultrapure water respectively to wash 3 times respectively; The particle diameter of obtained water-soluble ferroferric oxide nano particle is 8.0��10nm.
The present invention provide a kind of particle diameter be 8.0��10nm, single dispersing and there is the microwave synthesis method of water-soluble ferriferrous oxide nano-particle. Adopting glycol ether as solvent and reductive agent, ferric chloride hexahydrate, as raw material, completes reaction in single mold microwave synthesis system. Prepared nanoparticle has good water-soluble, monodispersity and superparamagnetism, can have good T simultaneously2Contrasting effects, has potential using value at biomedical sector.
The present invention adopts microwave heating method to prepare ferriferrous oxide nano-particle and has the following advantages:
1) of the present invention to prepare ferriferrous oxide nano-particle method simple to operate, and reactant is cheap, and cost is low; Reaction completes rapidly, and required time is short; Side reaction is few, generates produce rate height; To capacity usage ratio height, reaction process does not produce objectionable impurities, energy-conserving and environment-protective.
2) ferriferrous oxide nano-particle prepared by the present invention has good superparamagnetism, and saturation magnetization is 62emug-1, coercive force is 10e.
3) ferriferrous oxide nano-particle prepared by the present invention has good T2Contrasting effects, r2Value is 167mM-1s-1��
4) ferriferrous oxide nano-particle uniform particle diameter prepared by the present invention, has good water dispersible and stability, can preserve for a long time after lyophilize.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo (TEM) of ferriferrous oxide nano-particle prepared by embodiment 1.
Fig. 2 is the X-ray diffraction spectrum of ferriferrous oxide nano-particle prepared by embodiment 1.
Fig. 3 is the magnetic hysteresis loop figure of ferriferrous oxide nano-particle prepared by embodiment 1.
Fig. 4 is the T of ferriferrous oxide nano-particle prepared by embodiment 12Imaging photo.
Fig. 5 is the T of ferriferrous oxide nano-particle prepared by embodiment 12The relaxation time linear relationship chart with Fe concentration reciprocal.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described further.
Embodiment 1:
The microwave synthesis method of water-soluble ferroferric oxide nano particle, step is as follows:
1) ferric chloride hexahydrate 0.54g (2mmol) is added in 20mL glycol ether, it is stirred to after it dissolves completely, adds 0.5g (6mmol) anhydrous sodium acetate, after fully stirring, make it dissolve completely.
2) by step 1) gained solution is transferred in single port flask, and is placed in single mold microwave synthesis system, adopts uncovered pattern to react, and temperature of reaction is 200 DEG C, and the reaction times is 5min, and power is 150W, after question response, naturally cools to room temperature.
3) by reaction product by magnetic resolution, and after using ethanol, ultrapure water respectively to wash three times respectively, lyophilize preserves.
Fig. 1 is transmission electron microscope (TEM) photo of the ferriferrous oxide nano-particle of preparation in embodiment 1, and as can be seen from Figure 1, prepared ferriferrous oxide nano-particle median size is about about 9nm.
Fig. 2 is the X-ray diffraction spectrum of the ferriferrous oxide nano-particle of preparation in embodiment 1. The diffraction peak of Z 250 sample can be seen, it does not have two-phase detected from collection of illustrative plates.
Fig. 3 is the magnetic hysteresis loop figure of the ferriferrous oxide nano-particle of preparation in embodiment 1. Can see that prepared ferriferrous oxide nano-particle has good superparamagnetism and higher saturation magnetization (62emug-1)��
Fig. 4 and 5 is the T of the ferriferrous oxide nano-particle of preparation in embodiment 12Imaging photo and T2The relaxation time linear relationship chart with Fe concentration reciprocal. Can see that prepared ferriferrous oxide nano-particle has higher relaxation rate (167mM-1s-1), thus in MRI molecular image is diagnosed, can be used as good T2Contrast medium.
Embodiment 2:
The microwave synthesis method of water-soluble ferroferric oxide nano particle, step is with embodiment 1, and difference is, temperature of reaction is 140 DEG C.
Embodiment 3:
The microwave synthesis method of water-soluble ferroferric oxide nano particle, step is with embodiment 1, and difference is, temperature of reaction is 220 DEG C.
Embodiment 4:
The microwave synthesis method of water-soluble ferroferric oxide nano particle, step is with embodiment 1, and difference is, the reaction times is 1min.
Embodiment 5:
The microwave synthesis method of water-soluble ferroferric oxide nano particle, step is with embodiment 1, and difference is, the reaction times is 30min.
Embodiment 6:
The microwave synthesis method of water-soluble ferroferric oxide nano particle, step is with embodiment 1, and difference is, reaction power is 50W.
Embodiment 7:
The microwave synthesis method of water-soluble ferroferric oxide nano particle, step is with embodiment 1, and difference is, ferric chloride hexahydrate content used is 0.27g (1mmol).
Embodiment 8:
The microwave synthesis method of water-soluble ferroferric oxide nano particle, step is with embodiment 1, and difference is, anhydrous acetic acid sodium content used is 1.0g (12mmol).
Claims (3)
1. the microwave synthesis method of a water-soluble ferroferric oxide nano particle, it is characterised in that comprise the following steps:
1) ferric chloride hexahydrate is added in glycol ether, it is stirred to after it dissolves completely, then adds anhydrous sodium acetate, make it dissolve completely after fully stirring, obtain solution A; The proportioning of described ferric chloride hexahydrate, glycol ether, anhydrous sodium acetate is 0.54g: 20mL: 0.5g, and wherein, ferric chloride hexahydrate, anhydrous sodium acetate are calculated in mass, and glycol ether is calculated by volume;
2) by step 1) gained solution A is transferred in single port flask, and is placed in single mold microwave synthesis system, after adopting uncovered pattern to react completely, naturally cool to room temperature, obtain reaction product; The temperature of described reaction is 140��220 DEG C, and the time of reaction is 1��30min;
3) by step 2) reaction product that obtains is by magnetic resolution, and after washing, lyophilize preserves, and obtains water-soluble ferroferric oxide nano particle.
2. the microwave synthesis method of a kind of water-soluble ferroferric oxide nano particle as claimed in claim 1, it is characterised in that in step 2) in, the work power of described single mold microwave synthesis system is 40��200W.
3. the microwave synthesis method of a kind of water-soluble ferroferric oxide nano particle as claimed in claim 1, it is characterised in that in step 3) in, described washing uses ethanol, ultrapure water respectively to wash 3 times respectively.
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| CN102153149B (en) * | 2010-12-29 | 2012-10-24 | 济南大学 | Method for preparing nano quantum dot level Fe3O4 superparamagnetic particles |
| CN103274478A (en) * | 2013-06-15 | 2013-09-04 | 厦门大学 | Method for preparing water-soluble ferroferric oxide nano particle |
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