CN107601576A - Ferroso-ferric oxide hollow magnetic nano particle and preparation method thereof - Google Patents
Ferroso-ferric oxide hollow magnetic nano particle and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of ferroso-ferric oxide hollow magnetic nano particle and preparation method thereof, this method comprises the following steps：Ferric iron source and Organic Alcohol are mixed, then add sodium acid carbonate or ammonium acetate obtains emulsion, according to the mass fraction, the ferric iron source is 1~10 part, sodium acid carbonate or ammonium acetate are 5~20 parts, and the mass volume ratio of the ferric iron source and the Organic Alcohol is 1~10g：100~400ml；The emulsion is reacted 6~96 hours at 150~220 DEG C and obtains reaction solution；Obtain the magnetic-particle in the reaction solution and produce the ferroso-ferric oxide hollow magnetic nano particle.The preparation method of the ferroso-ferric oxide hollow magnetic nano particle of the present invention can be prepared with hollow-core construction, and the ferroso-ferric oxide hollow magnetic nano particle that surface roughness is higher, be more widely applied.
Description
Technical field
The present invention relates to magnetic nanoparticle field, more particularly to a kind of ferroso-ferric oxide hollow magnetic nano particle and
Its preparation method.
Background technology
Magnetic nanoparticle has magnetic conductance tropism, can assemble in magnetic field because magnetic attracts, leaving magnetic field can
It is scattered.Conventional magnetic nanoparticle is Fe3O4With γ-Fe2O3Iron oxide material, wherein Fe3O4It is the most magnetic of biologic applications
Property nano particle, can be prepared by the methods of chemical coprecipitation, thermal decomposition method and microemulsion method.Fe3O4Magnetic Nano
Particle possesses the easily advantageous characteristic such as modification, can realize separation and enriching step simultaneously, improve separating rate and bioaccumulation efficiency,
Also significantly increase analysis detection sensitivity, be widely used in nucleic acid extraction, cell sorting, protein purification, nuclear magnetic resonance into
The biochemical fields such as picture, drug targeting and magnetic thermotherapy.
The Fe of hollow-core construction3O4Magnetic nanoparticle is easier to be influenceed by external magnetic field, and hollow structure can also accommodate greatly
The guest molecule or medicine of amount, many scholars typically prepare Fe using hard template method and soft template method3O4Hollow magnetic nano particle
Preferably to meet biochemical application requirement.Huang etc. uses hydrophily polystyrene microsphere to pass through interface for hard template
Deposited magnetic nano particle, then high-temperature calcination remove template and prepare Fe3O4Hollow magnetic nano particle, but this method needs height
Temperature control system, technical process is excessively complicated, is unfavorable for industrializing.And the 1,6- hexamethylene diamines that Wang etc. is employed as surfactant are
Soft template, the micella formed in course of reaction prepare Fe as template direction agent3O4Hollow magnetic nano particle, but this method needs
Substantial amounts of organic solvent is used to cause seriously to pollute to environment, also caused serious injury to operator as raw material.
The hollow-core construction Fe being prepared at present3O4The surface roughness of magnetic nanoparticle is relatively low, and specific surface area is relatively low,
It is difficult to obtain preferable effect when carrying out the application in the fields such as biochemistry such as nucleic acid and cell, significantly limit using model
Enclose.
The content of the invention
Based on this, it is necessary to provide a kind of higher ferroso-ferric oxide hollow magnetic of surface roughness that can be prepared and receive
The preparation method of rice grain.
A kind of preparation method of ferroso-ferric oxide hollow magnetic nano particle, comprises the following steps：
Ferric iron source and Organic Alcohol are mixed, then sodium acid carbonate is added or ammonium acetate obtains emulsion, by mass fraction
Meter, the ferric iron source are 1~10 part, and sodium acid carbonate or ammonium acetate are 5~20 parts, the ferric iron source and the Organic Alcohol
Mass volume ratio is 1~10g：100~400ml；
The emulsion is reacted 6~96 hours at 150~220 DEG C and obtains reaction solution；
Obtain the magnetic-particle in the reaction solution and produce the ferroso-ferric oxide hollow magnetic nano particle.
In one of the embodiments, according to the mass fraction, the ferric iron source is 5~8 parts, sodium acid carbonate or ammonium acetate
For 15~20 parts, the mass volume ratio of the ferric iron source and the Organic Alcohol is 5~8g：250~350ml.
In one of the embodiments, the Organic Alcohol includes diethylene glycol (DEG) and ethylene glycol.
In one of the embodiments, the ferric iron source includes FeCl3、FeCl3·6H2O, ammonium ferric sulfate, ferric sulfate and
One or more in ferric nitrate.
In one of the embodiments, it is further comprising the steps of：In the emulsion add sodium acetate, sodium hydroxide or
Potassium hydroxide.
In one of the embodiments, the quality of sodium acetate, sodium hydroxide or potassium hydroxide and sodium acid carbonate or ammonium acetate
Than for 1~5：5~20.
In one of the embodiments, obtaining the specific steps of the magnetic-particle in the reaction solution includes：Will be described anti-
It is colourless to answer liquid attraction to supernatant, and supernatant discarding produces the magnetic-particle.
In one of the embodiments, obtain further comprising the steps of after the magnetic-particle in the reaction solution：By described in
Magnetic-particle is cleaned one or many with the mixed liquor of water and ethanol.
In one of the embodiments, it is further comprising the steps of after the cleaning step：By the magnetic-particle in
65 DEG C~75 DEG C dryings 18~28 hours.
Present invention also provides a kind of ferroso-ferric oxide hollow magnetic nanometer being prepared according to above-mentioned preparation method
Grain.
The application is by with ferric iron source and Organic Alcohol, and ammonium acetate or sodium acid carbonate are raw material, at 150~220 DEG C
6~96h of lower reaction, so as to which Fe be prepared3O4Hollow magnetic nano particle.Ammonium acetate or sodium acid carbonate not only serve as bases
Promote ferric iron source to hydrolyze, and easily decompose produce gas at high temperature, make to produce hole inside magnetic nanoparticle, it is more crucial
Be that the addition of ammonium acetate or sodium acid carbonate can make the Fe being prepared3O4Hollow magnetic nano particle has higher surface thick
Rugosity, so as to obtain higher specific surface area, the Fe3O4Hollow magnetic nanoparticle suspension and permeability are good, and density is low, tool
There are the pattern rule of uniqueness and uniform particle sizes, have applied to the biochemistry such as field such as nucleic acid extraction, cell sorting very excellent
Different effect, is more widely applied.The preparation method raw material is simple, and without adding surfactant and initiator, cost is cheap,
Preparation technology is simple, and reaction condition is gentle, is protected without nitrogen, it is only necessary to simple high-temperature high-pressure reaction kettle equipment, green ring
Protect and process is simple, serious pollution will not be caused to environment or operator is caused serious injury, is advantageous to industrialized production.
Further, diethylene glycol (DEG) can be with the progress of delayed response, by adding diethylene glycol (DEG) and ethylene glycol and adjusting the two
Ratio, optimize the addition of other raw materials, can regulate and control the growth rate and granular size of magnetic nanoparticle as needed, two
The ratio of glycol is higher, and the particle diameter of magnetic nanoparticle is smaller, and the ratio of diethylene glycol (DEG) is lower, and the particle diameter of magnetic nanoparticle is got over
Greatly.In addition, by adding other alkaloids such as sodium acetate, sodium hydroxide and potassium hydroxide, solution further can be presented
Alkalescence, and the degree of hollow-core construction is adjusted, can so meet the needs of different, improve the flexibility of production, model is applied in expansion
Enclose.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of ferroso-ferric oxide hollow magnetic nano particle prepared by embodiment 1；
Fig. 2 is the grain size distribution of ferroso-ferric oxide hollow magnetic nano particle prepared by embodiment 1；
Fig. 3 is the transmission electron microscope picture of ferroso-ferric oxide hollow magnetic nano particle prepared by embodiment 2；
Fig. 4 is the grain size distribution of ferroso-ferric oxide hollow magnetic nano particle prepared by embodiment 2.
Embodiment
For the ease of understanding the present invention, the present invention will be described more fully below.But the present invention can be with perhaps
More different form is realized, however it is not limited to embodiment described herein.On the contrary, the purpose for providing these embodiments is to make
Understanding more thorough and comprehensive to the disclosure.
Unless otherwise defined, all of technologies and scientific terms used here by the article is with belonging to technical field of the invention
The implication that technical staff is generally understood that is identical.Term used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
The arbitrary and all combination of the Listed Items of pass.
The preparation method of the ferroso-ferric oxide hollow magnetic nano particle of an embodiment of the present invention, comprises the following steps S1
~S3：
S1, ferric iron source and Organic Alcohol mixed, then add sodium acid carbonate or ammonium acetate obtains emulsion, by mass parts
Number meter, ferric iron source are 1~10 part, and sodium acid carbonate or ammonium acetate are 5~20 parts, the mass volume ratio of ferric iron source and Organic Alcohol
For 1~10g：100~400ml.
Alternatively, ferric iron source includes FeCl3、FeCl3·6H2O, one kind in ammonium ferric sulfate, ferric sulfate and ferric nitrate or
It is a variety of.
Specifically, according to the mass fraction, ferric iron source is 5~8 parts, and sodium acid carbonate or ammonium acetate are 15~20 parts, trivalent
The mass volume ratio of source of iron and Organic Alcohol is 5~8g：250~350ml.
In one embodiment, Organic Alcohol includes diethylene glycol (DEG) and ethylene glycol.
In one embodiment, it is further comprising the steps of：Sodium acetate, sodium hydroxide or hydroxide are added in emulsion
Potassium.Specifically, sodium acetate, sodium hydroxide or potassium hydroxide and the mass ratio of sodium acid carbonate or ammonium acetate are 1~5：5~20.
S2, emulsion is reacted 6~96 hours at 150~220 DEG C obtain reaction solution.
S3, the magnetic-particle obtained in reaction solution produce ferroso-ferric oxide hollow magnetic nano particle.
Specifically, obtaining the specific steps of the magnetic-particle in reaction solution includes：By reaction solution attraction to supernatant
Liquid is colourless, and supernatant discarding produces magnetic-particle.
In one embodiment, it is further comprising the steps of after the magnetic-particle in acquisition reaction solution：By magnetic-particle water
It is one or many with the mixed liquor cleaning of ethanol.
In one embodiment, it is further comprising the steps of after the cleaning step：Magnetic-particle is dry in 65 DEG C~75 DEG C
Dry 18~28 hours.
Present invention also offers a kind of ferroso-ferric oxide hollow magnetic nanometer being prepared according to above-mentioned preparation method
Grain.
The application is by with ferric iron source and Organic Alcohol, and ammonium acetate or sodium acid carbonate are raw material, at 150~220 DEG C
6~96h of lower reaction, so as to which Fe be prepared3O4Hollow magnetic nano particle.Ammonium acetate or sodium acid carbonate not only serve as bases
Promote ferric iron source to hydrolyze, and easily decompose produce gas at high temperature, make to produce hole inside magnetic nanoparticle, it is more crucial
Be that the addition of ammonium acetate or sodium acid carbonate can make the Fe being prepared3O4Hollow magnetic nano particle has higher surface thick
Rugosity, so as to obtain higher specific surface area, the Fe3O4Hollow magnetic nanoparticle suspension and permeability are good, and density is low, tool
There are the pattern rule of uniqueness and uniform particle sizes, have applied to the biochemistry such as field such as nucleic acid extraction, cell sorting very excellent
Different effect, is more widely applied.The preparation method raw material is simple, and without adding surfactant and initiator, cost is cheap,
Preparation technology is simple, and reaction condition is gentle, is protected without nitrogen, it is only necessary to simple high-temperature high-pressure reaction kettle equipment, green ring
Protect and process is simple, serious pollution will not be caused to environment or operator is caused serious injury, is advantageous to industrialized production.
Further, diethylene glycol (DEG) can be with the progress of delayed response, by adding diethylene glycol (DEG) and ethylene glycol and adjusting the two
Ratio, optimize the addition of other raw materials, can regulate and control the growth rate and granular size of magnetic nanoparticle as needed, two
The ratio of glycol is higher, and the particle diameter of magnetic nanoparticle is smaller, and the ratio of diethylene glycol (DEG) is lower, and the particle diameter of magnetic nanoparticle is got over
Greatly.In addition, by adding other alkaloids such as sodium acetate, sodium hydroxide and potassium hydroxide, solution further can be presented
Alkalescence, and the degree of hollow-core construction is adjusted, can so meet the needs of different, improve the flexibility of production, model is applied in expansion
Enclose.
It is specific embodiment below.
Embodiment 1
6.75g FeCl are weighed first3·6H2O and 18g sodium acid carbonates are put into 500ml polytetrafluoroethyllining lining, are measured
300ml diethylene glycol (DEG)s are added in liner, and mechanical agitation is uniform, are obtained the emulsion of yellow, are then charged into stainless steel cauldron,
Tighten stainless steel cauldron.Reactor is put into constant temperature oven and reacted 20 hours in 200 DEG C, after reaction terminates, is down to room temperature,
Reactor is taken out, obtains the reaction solution of brown or black.It is colourless that above-mentioned reaction solution is attracted into supernatant with strong magnets, is abandoned
Go supernatant to obtain black precipitate i.e. magnetic-particle, cleaned up, be then placed in drying box repeatedly with the mixed liquor of water and ethanol
Dried 24 hours in 70 DEG C, obtain ferroso-ferric oxide hollow magnetic nano particle.
To Fe manufactured in the present embodiment3O4Hollow magnetic nano particle carries out transmissioning electric mirror test, passes through transmissioning electric mirror test
Observe Fe3O4Chemical constitution, configuration of surface and the particle diameter distribution of hollow magnetic nano particle, as a result as shown in figure 1, the Fe3O4It is empty
Heart magnetic nanoparticle has unique shape characteristic, and it is made up of many little magnetic beads, has inside the big magnetic bead that little magnetic bead is formed
There are hollow parts, and little magnetic bead can so dramatically increase Fe with structures such as many small cavities and gaps3O4Hollow magnetic
Surface roughness, pore volume, aperture and specific surface area of nano particle etc..The picture progress particle diameter of transmission electron microscope is counted to obtain figure
2, most of Fe3O4The particle diameter of hollow magnetic nano particle is between 150~250nm, median 200nm, and particle diameter is in normal state
Distribution, monodispersity are good.
Embodiment 2
6.75g FeCl are weighed first3·6H2O, 2.5g sodium acetates and 15.5g ammonium acetates are put into 500ml polytetrafluoroethylene (PTFE)
In liner, measure 200ml diethylene glycol (DEG)s and 100ml ethylene glycol is added in liner, mechanical agitation is uniform, obtains the milkiness of yellow
Liquid, it is then charged into stainless steel cauldron, tightens stainless steel cauldron.Reactor is put into constant temperature oven in 200 DEG C of reactions
12 hours, after reaction terminates, room temperature is down to, reactor is taken out, obtains the reaction solution of brown or black.By above-mentioned reaction solution with by force
Power attraction to supernatant is colourless, and supernatant discarding obtains black precipitate i.e. magnetic-particle, and the mixed liquor with water and ethanol is anti-
Clean up again, be then placed in drying box and dried 24 hours in 70 DEG C, obtain ferroso-ferric oxide hollow magnetic nano particle.
To Fe manufactured in the present embodiment3O4Hollow magnetic nano particle carries out transmissioning electric mirror test, passes through transmissioning electric mirror test
Observe Fe3O4Chemical constitution, configuration of surface and the particle diameter distribution of hollow magnetic nano particle, as a result as shown in figure 3, the Fe3O4It is empty
Heart magnetic nanoparticle has unique shape characteristic, has hollow parts inside it, and with obviously circular ring structure, it is empty
Heart district domain is bigger than the hollow area inside 1 big magnetic bead of embodiment, reaches 100~300nm.Particle diameter is carried out to the picture of transmission electron microscope
Statistics obtains Fig. 4, most of Fe3O4The particle diameter of hollow magnetic nano particle is between 300~700nm, median 525nm,
Particle diameter is in normal distribution, and monodispersity is preferable.
Comparative example 1
6.75g FeCl are weighed first3·6H2O and 18g ammonium hydrogen carbonate is put into 500ml polytetrafluoroethyllining lining, is measured
300ml diethylene glycol (DEG)s are added in liner, and mechanical agitation is uniform, obtain emulsion, are then charged into stainless steel cauldron, are tightened not
Become rusty steel reactor.Reactor is put into constant temperature oven and reacted 20 hours in 200 DEG C, after reaction terminates, is down to room temperature, is taken out anti-
Kettle is answered, obtains the reaction solution of brown or black.It is colourless, supernatant discarding that above-mentioned reaction solution is attracted into supernatant with strong magnets
Black precipitate i.e. magnetic-particle is obtained, is cleaned up, is then placed in drying box in 70 DEG C repeatedly with the mixed liquor of water and ethanol
Dry 24 hours, obtain magnetic nanoparticle.The specific surface area of the magnetic nanoparticle of comparative example 1 is less than embodiment 1 and implements
Example 2, and shape characteristic differs.
Comparative example 2
6.75g FeCl are weighed first3·6H2O and 18g urea is put into 500ml polytetrafluoroethyllining lining, is measured
300ml diethylene glycol (DEG)s are added in liner, and mechanical agitation is uniform, obtain emulsion, are then charged into stainless steel cauldron, are tightened not
Become rusty steel reactor.Reactor is put into constant temperature oven and reacted 20 hours in 200 DEG C, after reaction terminates, is down to room temperature, is taken out anti-
Kettle is answered, obtains the reaction solution of brown or black.It is colourless, supernatant discarding that above-mentioned reaction solution is attracted into supernatant with strong magnets
Black precipitate i.e. magnetic-particle is obtained, is cleaned up, is then placed in drying box in 70 DEG C repeatedly with the mixed liquor of water and ethanol
Dry 24 hours, obtain magnetic nanoparticle.The specific surface area of the magnetic nanoparticle of comparative example 2 is less than embodiment 1 and implements
Example 2, and shape characteristic differs.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that come for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of preparation method of ferroso-ferric oxide hollow magnetic nano particle, it is characterised in that comprise the following steps：
Ferric iron source and Organic Alcohol are mixed, then sodium acid carbonate is added or ammonium acetate obtains emulsion, according to the mass fraction, institute
Ferric iron source is stated as 1~10 part, sodium acid carbonate or ammonium acetate are 5~20 parts, the quality of the ferric iron source and the Organic Alcohol
Volume ratio is 1~10g：100~400ml；
The emulsion is reacted 6~96 hours at 150~220 DEG C and obtains reaction solution；
Obtain the magnetic-particle in the reaction solution and produce the ferroso-ferric oxide hollow magnetic nano particle.
2. the preparation method of ferroso-ferric oxide hollow magnetic nano particle according to claim 1, it is characterised in that by matter
Number meter is measured, the ferric iron source is 5~8 parts, and sodium acid carbonate or ammonium acetate are 15~20 parts, and the ferric iron source has with described
The mass volume ratio of machine alcohol is 5~8g：250~350ml.
3. the preparation method of ferroso-ferric oxide hollow magnetic nano particle according to claim 1, it is characterised in that described
Organic Alcohol includes diethylene glycol (DEG) and ethylene glycol.
4. the preparation method of ferroso-ferric oxide hollow magnetic nano particle according to claim 1, it is characterised in that described
Ferric iron source includes FeCl3、FeCl3·6H2O, the one or more in ammonium ferric sulfate, ferric sulfate and ferric nitrate.
5. the preparation method of the ferroso-ferric oxide hollow magnetic nano particle according to any one of Claims 1 to 4, its feature
It is, it is further comprising the steps of：Sodium acetate, sodium hydroxide or potassium hydroxide are added in the emulsion.
6. the preparation method of ferroso-ferric oxide hollow magnetic nano particle according to claim 5, it is characterised in that acetic acid
Sodium, sodium hydroxide or potassium hydroxide are 1~5 with the mass ratio of sodium acid carbonate or ammonium acetate：5~20.
7. the preparation method of ferroso-ferric oxide hollow magnetic nano particle according to claim 1, it is characterised in that obtain
The specific steps of magnetic-particle in the reaction solution include：It is colourless by the reaction solution attraction to supernatant, abandons
Supernatant is gone to produce the magnetic-particle.
8. the preparation method of ferroso-ferric oxide hollow magnetic nano particle according to claim 7, it is characterised in that obtain
It is further comprising the steps of after magnetic-particle in the reaction solution：The magnetic-particle is cleaned one with the mixed liquor of water and ethanol
It is secondary or multiple.
9. the preparation method of ferroso-ferric oxide hollow magnetic nano particle according to claim 8, it is characterised in that in institute
State further comprising the steps of after cleaning step：By the magnetic-particle in 65 DEG C~75 DEG C dryings 18~28 hours.
10. a kind of ferroso-ferric oxide hollow magnetic nano particle, it is characterised in that according to any one of claim 1~9
Preparation method is prepared.
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