CN107601576B - Ferroferric oxide hollow magnetic nano-particles and preparation method thereof - Google Patents
Ferroferric oxide hollow magnetic nano-particles and preparation method thereof Download PDFInfo
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Abstract
The invention relates to ferroferric oxide hollow magnetic nanoparticles and a preparation method thereof, and the method comprises the following steps of mixing a ferric iron source and organic alcohol, adding 1-10 parts of sodium bicarbonate or ammonium acetate by mass to obtain an emulsion, reacting the emulsion at 150-220 ℃ for 6-96 hours to obtain a reaction solution, and obtaining magnetic particles in the reaction solution to obtain the ferroferric oxide hollow magnetic nanoparticles, wherein the mass volume ratio of the ferric iron source to the organic alcohol is 1-10 g: 100-400 ml, and the preparation method of the ferroferric oxide hollow magnetic nanoparticles can be used for preparing the ferroferric oxide hollow magnetic nanoparticles with a hollow structure and higher surface roughness and can be applied more .
Description
Technical Field
The invention relates to the field of magnetic nanoparticles, in particular to ferroferric oxide hollow magnetic nanoparticles and a preparation method thereof.
Background
The magnetic nanoparticles have magnetic guidance, can be concentrated in a magnetic field due to magnetic attraction, and can be dispersed away from the magnetic field. A commonly used magnetic nanoparticle is Fe3O4And gamma-Fe2O3Iron oxide substances, in which Fe3O4The magnetic nano-particles are magnetic nano-particles which are most applied to organisms and can be prepared by a chemical coprecipitation method, a thermal decomposition method, a microemulsion method and the like. Fe3O4The magnetic nanoparticles have the advantages of easy modification and the like, can realize separation and enrichment steps at the same time, improves the separation speed and the enrichment efficiency, and also obviously improves the sensitivity of analysis and detection, and is widely applied to the biochemical fields of nucleic acid extraction, cell sorting, protein purification, nuclear magnetic resonance imaging, drug targeting, magnetic thermal therapy and the like.
Fe of hollow structure3O4The magnetic nanoparticles are more easily influenced by an external magnetic field, the hollow structure can also contain a large amount of guest molecules or drugs, and many scholars prepare Fe by adopting a hard template method and a soft template method3O4Hollow magnetic nanoparticles are used to better meet the application requirements of biochemistry. Huang et al, which uses hydrophilic polystyrene microspheres as hard templates, prepares Fe by depositing magnetic nanoparticles on the interface and then calcining at high temperature to remove the templates3O4Hollow magnetic nanoparticles, however, the method requires high-temperature control, and the process is too complicated, which is not suitable for industrialization. Wang et al prepared Fe using 1, 6-hexanediamine as a surfactant as a soft template and micelles formed during the reaction as a template directing agent3O4Hollow magnetic nanoparticles, but this method requires the use of large amounts of organic solvents as raw materials, causing severe environmental pollution and also causing severe injury to operators.
The hollow structure Fe prepared at present3O4The magnetic nanoparticles have low surface roughness and low specific surface area, and are difficult to obtain good effects when applied to the fields of biochemistry such as nucleic acid, cells and the like, so that the application range is greatly limited.
Disclosure of Invention
Therefore, preparation methods capable of preparing ferroferric oxide hollow magnetic nanoparticles with high surface roughness are needed.
The preparation method of ferroferric oxide hollow magnetic nanoparticles comprises the following steps:
mixing a ferric iron source and organic alcohol, then adding sodium bicarbonate or ammonium acetate to obtain emulsion, wherein the ferric iron source accounts for 1-10 parts by mass, the sodium bicarbonate or ammonium acetate accounts for 5-20 parts by mass, and the mass volume ratio of the ferric iron source to the organic alcohol is 1-10 g: 100-400 ml;
reacting the emulsion at 150-220 ℃ for 6-96 hours to obtain a reaction solution;
and obtaining the magnetic particles in the reaction liquid to obtain the ferroferric oxide hollow magnetic nanoparticles.
In examples, the weight parts of the ferric iron source are 5-8 parts, the weight parts of sodium bicarbonate or ammonium acetate are 15-20 parts, and the weight volume ratio of the ferric iron source to the organic alcohol is 5-8 g: 250-350 ml.
In of these embodiments, the organic alcohols include diethylene glycol and ethylene glycol.
In of these embodiments, the source of ferric iron comprises FeCl3、FeCl3·6H2 one or more of O, ammonium ferric sulfate, ferric sulfate and ferric nitrate.
In embodiments, the method further comprises adding sodium acetate, sodium hydroxide, or potassium hydroxide to the emulsion.
In embodiments, the mass ratio of sodium acetate, sodium hydroxide or potassium hydroxide to sodium bicarbonate or ammonium acetate is 1-5: 5-20.
In embodiments, the step of obtaining the magnetic particles in the reaction solution comprises attracting the reaction solution to a supernatant with a magnet to obtain colorless supernatant, and discarding the supernatant to obtain the magnetic particles.
In embodiments, the method further comprises washing the magnetic particles times or more with a mixture of water and ethanol after obtaining the magnetic particles in the reaction solution.
In embodiments, the washing step is followed by the step of drying the magnetic particles at 65-75 ℃ for 18-28 hours.
The application also provides ferroferric oxide hollow magnetic nanoparticles prepared by the preparation method.
The method takes a ferric iron source, organic alcohol and ammonium acetate or sodium bicarbonate as raw materials to react for 6-96 h at the temperature of 150-220 ℃, so that Fe is prepared3O4Hollow magnetic nanoparticles. The ammonium acetate or the sodium bicarbonate can be used as alkalies to promote the hydrolysis of the ferric iron source, and can be easily decomposed at high temperature to generate gas so as to generate holes in the magnetic nanoparticles, and the more important point is that the addition of the ammonium acetate or the sodium bicarbonate can enable the prepared Fe to be3O4The hollow magnetic nanoparticles have high surface roughness, thereby obtaining high specific surface area, and the Fe3O4The hollow magnetic nano-particle has good suspension property and permeability, low density, unique shape rule and uniform particle size, has very excellent effect when being applied to the fields of biochemistry such as nucleic acid extraction, cell sorting and the like, and is more universal.
the diethylene glycol can delay the reaction, the growth rate and the particle size of the magnetic nanoparticles can be regulated and controlled as required by adding the diethylene glycol and the ethylene glycol and adjusting the proportion of the diethylene glycol to the ethylene glycol, the higher the proportion of the diethylene glycol, the smaller the particle size of the magnetic nanoparticles, the lower the proportion of the diethylene glycol, and the larger the particle size of the magnetic nanoparticles.
Drawings
FIG. 1 is a transmission electron microscope image of ferroferric oxide hollow magnetic nanoparticles prepared in example 1;
FIG. 2 is a particle size distribution diagram of the ferroferric oxide hollow magnetic nanoparticles prepared in example 1;
FIG. 3 is a transmission electron microscope image of the ferroferric oxide hollow magnetic nanoparticles prepared in example 2;
fig. 4 is a particle size distribution diagram of the ferroferric oxide hollow magnetic nanoparticles prepared in example 2.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention, the term "and/or" as used herein includes any and all combinations of or more of the associated listed items.
The preparation method of the ferroferric oxide hollow magnetic nanoparticles according to the embodiment of the invention comprises the following steps of S1-S3:
s1, mixing a ferric iron source and organic alcohol, and then adding sodium bicarbonate or ammonium acetate to obtain emulsion, wherein the ferric iron source accounts for 1-10 parts by mass, the sodium bicarbonate or ammonium acetate accounts for 5-20 parts by mass, and the mass volume ratio of the ferric iron source to the organic alcohol is 1-10 g: 100-400 ml.
Optionally, the source of ferric iron comprises FeCl3、FeCl3·6H2O, ammonium ferric sulfate, ferric sulfate and or more of ferric nitrate.
Specifically, the weight parts of the ferric iron source are 5-8 parts, the weight parts of sodium bicarbonate or ammonium acetate are 15-20 parts, and the weight volume ratio of the ferric iron source to the organic alcohol is 5-8 g: 250-350 ml.
In examples, the organic alcohols include diethylene glycol and ethylene glycol.
In embodiments, the method further comprises the step of adding sodium acetate, sodium hydroxide or potassium hydroxide to the emulsion, specifically, the mass ratio of sodium acetate, sodium hydroxide or potassium hydroxide to sodium bicarbonate or ammonium acetate is 1-5: 5-20.
S2, reacting the emulsion at 150-220 ℃ for 6-96 hours to obtain a reaction solution.
S3, obtaining the magnetic particles in the reaction liquid to obtain the ferroferric oxide hollow magnetic nanoparticles.
Specifically, the specific steps of obtaining the magnetic particles in the reaction solution include: and (3) attracting the reaction solution by a magnet until the supernatant is colorless, and removing the supernatant to obtain the magnetic particles.
In embodiments, the method further comprises washing the magnetic particles times or more with a mixture of water and ethanol after obtaining the magnetic particles in the reaction solution.
In embodiments, the washing step is followed by a step of drying the magnetic particles at 65-75 ℃ for 18-28 hours.
The invention also provides ferroferric oxide hollow magnetic nanoparticles prepared by the preparation method.
The method takes a ferric iron source, organic alcohol and ammonium acetate or sodium bicarbonate as raw materials to react for 6-96 h at the temperature of 150-220 ℃, so that Fe is prepared3O4Hollow magnetic nanoparticles. The ammonium acetate or the sodium bicarbonate can be used as alkalies to promote the hydrolysis of the ferric iron source, and can be easily decomposed at high temperature to generate gas so as to generate holes in the magnetic nanoparticles, and the more important point is that the addition of the ammonium acetate or the sodium bicarbonate can enable the prepared Fe to be3O4The hollow magnetic nanoparticles have a high surface roughness to obtainHigher specific surface area of the Fe3O4The hollow magnetic nano-particle has good suspension property and permeability, low density, unique shape rule and uniform particle size, has very excellent effect when being applied to the fields of biochemistry such as nucleic acid extraction, cell sorting and the like, and is more universal.
the diethylene glycol can delay the reaction, the growth rate and the particle size of the magnetic nanoparticles can be regulated and controlled as required by adding the diethylene glycol and the ethylene glycol and adjusting the proportion of the diethylene glycol to the ethylene glycol, the higher the proportion of the diethylene glycol, the smaller the particle size of the magnetic nanoparticles, the lower the proportion of the diethylene glycol, and the larger the particle size of the magnetic nanoparticles.
The following are specific examples.
Example 1
First, 6.75g of FeCl was weighed3·6H2Putting O and 18g of sodium bicarbonate into a 500ml polytetrafluoroethylene lining, weighing 300ml of diethylene glycol, adding into the lining, mechanically stirring uniformly to obtain yellow emulsion, then putting into a stainless steel reaction kettle, and screwing down the stainless steel reaction kettle. And (3) putting the reaction kettle into a constant-temperature oven to react for 20 hours at 200 ℃, cooling to room temperature after the reaction is finished, and taking out the reaction kettle to obtain brown or black reaction liquid. And (3) attracting the reaction solution by using a strong magnet until the supernatant is colorless, discarding the supernatant to obtain black precipitates, namely magnetic particles, repeatedly cleaning the black precipitates by using a mixed solution of water and ethanol, and then drying the magnetic particles in a drying oven at 70 ℃ for 24 hours to obtain the ferroferric oxide hollow magnetic nanoparticles.
For Fe prepared in this example3O4Performing transmission electron microscope test on the hollow magnetic nanoparticles, and observing Fe through the transmission electron microscope test3O4The chemical structure, surface morphology and particle size distribution of the hollow magnetic nanoparticles are shown in FIG. 1, and the result is that Fe is present3O4The hollow magnetic nano-particles have unique morphological characteristics and are composed of a plurality of small magnetic beads, the large magnetic beads formed by the small magnetic beads are internally provided with hollow parts, and the small magnetic beads are accompanied with a plurality of small cavities, gaps and other structures, so that the Fe content can be remarkably increased3O4Surface roughness, pore volume, pore diameter, specific surface area, and the like of the hollow magnetic nanoparticles. The particle size statistics of the transmission electron microscope pictures are carried out to obtain a figure 2, most of Fe3O4The particle size of the hollow magnetic nanoparticles is between 150 nm and 250nm, the median is 200nm, the particle size is normally distributed, and the monodispersity is good.
Example 2
First, 6.75g of FeCl was weighed3·6H2O, 2.5g of sodium acetate and 15.5g of ammonium acetate are put into a 500ml polytetrafluoroethylene lining, 200ml of diethylene glycol and 100ml of ethylene glycol are weighed and added into the lining, the mixture is mechanically stirred uniformly to obtain yellow emulsion, then the yellow emulsion is put into a stainless steel reaction kettle, and the stainless steel reaction kettle is screwed tightly. And (3) putting the reaction kettle into a constant-temperature oven to react for 12 hours at 200 ℃, cooling to room temperature after the reaction is finished, and taking out the reaction kettle to obtain brown or black reaction liquid. And (3) attracting the reaction solution by using a strong magnet until the supernatant is colorless, discarding the supernatant to obtain black precipitates, namely magnetic particles, repeatedly cleaning the black precipitates by using a mixed solution of water and ethanol, and then drying the magnetic particles in a drying oven at 70 ℃ for 24 hours to obtain the ferroferric oxide hollow magnetic nanoparticles.
For Fe prepared in this example3O4Performing transmission electron microscope test on the hollow magnetic nanoparticles, and observing Fe through the transmission electron microscope test3O4The chemical structure, surface morphology and particle size distribution of the hollow magnetic nanoparticles are shown in FIG. 3, and the result is that Fe is present3O4The hollow magnetic nano-particles have unique morphological characteristics, have hollow parts inside and have very obvious circlesThe hollow area of the ring structure is larger than that of the large magnetic bead of example 1, and is 100 to 300 nm. The particle size statistics of the transmission electron microscope pictures are carried out to obtain a graph 4, most of Fe3O4The particle size of the hollow magnetic nanoparticles is 300-700 nm, the median is 525nm, the particle size is in normal distribution, and the monodispersity is good.
Comparative example 1
First, 6.75g of FeCl was weighed3·6H2O and 18g of ammonium bicarbonate are put into a 500ml polytetrafluoroethylene lining, 300ml of diethylene glycol is weighed and added into the lining, the mixture is mechanically stirred uniformly to obtain emulsion, and then the emulsion is put into a stainless steel reaction kettle, and the stainless steel reaction kettle is screwed down. And (3) putting the reaction kettle into a constant-temperature oven to react for 20 hours at 200 ℃, cooling to room temperature after the reaction is finished, and taking out the reaction kettle to obtain brown or black reaction liquid. And (3) attracting the reaction solution to obtain a colorless supernatant by using a strong magnet, discarding the supernatant to obtain a black precipitate, namely magnetic particles, repeatedly cleaning the black precipitate by using a mixed solution of water and ethanol, and then drying the magnetic particles in a drying oven at 70 ℃ for 24 hours to obtain the magnetic nanoparticles. The magnetic nanoparticles of comparative example 1 had a lower specific surface area than those of examples 1 and 2, and the morphological characteristics were not the same.
Comparative example 2
First, 6.75g of FeCl was weighed3·6H2Putting O and 18g of urea into a 500ml polytetrafluoroethylene lining, measuring 300ml of diglycol, adding the diglycol into the lining, mechanically stirring uniformly to obtain emulsion, then putting the emulsion into a stainless steel reaction kettle, and screwing the stainless steel reaction kettle tightly. And (3) putting the reaction kettle into a constant-temperature oven to react for 20 hours at 200 ℃, cooling to room temperature after the reaction is finished, and taking out the reaction kettle to obtain brown or black reaction liquid. And (3) attracting the reaction solution to obtain a colorless supernatant by using a strong magnet, discarding the supernatant to obtain a black precipitate, namely magnetic particles, repeatedly cleaning the black precipitate by using a mixed solution of water and ethanol, and then drying the magnetic particles in a drying oven at 70 ℃ for 24 hours to obtain the magnetic nanoparticles. The magnetic nanoparticles of comparative example 2 had a lower specific surface area than those of examples 1 and 2, and the morphological characteristics were not the same.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (2)
- The preparation method of the ferroferric oxide hollow magnetic nanoparticles is characterized by comprising the following steps of:FeCl is added3·6H2Mixing O and organic alcohol, and then adding sodium acetate and ammonium acetate to obtain emulsion, wherein the FeCl is3·6H26.75g of O, 15.5g of ammonium acetate and 2.5g of sodium acetate, wherein the FeCl is3·6H2The mass-to-volume ratio of O to the organic alcohol is 6.75 g: 300 ml; the organic alcohol comprises diethylene glycol and ethylene glycol, and the volume ratio of the diethylene glycol to the ethylene glycol is 2: 1;reacting the emulsion at 200 ℃ for 12 hours to obtain a reaction solution;obtaining magnetic particles in the reaction liquid to obtain the ferroferric oxide hollow magnetic nanoparticles;the specific steps for obtaining the magnetic particles in the reaction solution include: attracting the reaction solution to obtain a supernatant which is colorless by using a magnet, and removing the supernatant to obtain the magnetic particles;after the magnetic particles in the reaction solution are obtained, the method also comprises the following steps of cleaning times or more times by using the mixed solution of water and ethanol;the cleaning step is followed by the steps of: and drying the magnetic particles at 65-75 ℃ for 18-28 hours.
- 2, ferroferric oxide hollow magnetic nanoparticles, which are characterized by being prepared according to the preparation method of claim 1.
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