CN101337695B - Method for preparing grain size adjustable nanometer ferroferric oxide microballoons by microwave - Google Patents
Method for preparing grain size adjustable nanometer ferroferric oxide microballoons by microwave Download PDFInfo
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- CN101337695B CN101337695B CN2008100414622A CN200810041462A CN101337695B CN 101337695 B CN101337695 B CN 101337695B CN 2008100414622 A CN2008100414622 A CN 2008100414622A CN 200810041462 A CN200810041462 A CN 200810041462A CN 101337695 B CN101337695 B CN 101337695B
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Abstract
A method for preparing nano ferroferric oxide spheres with adjustable particle size with micro wave belongs to the nano material preparation technical field. The method comprises the following steps: the first step, adding inorganic salt and a surface active agent after malysite dissolves in polylol, adding a latent solvent; mixing and stirring to obtain a precursor liquid of ferroferric oxide, wherein, the mass ratio of the polylol and the malysite is (5-100):1, the mass ratio of the inorganic salt and the malysite is (1-6): 1, the mass ratio of the surface active agent and the malysite is (0-5):1, and the volume ratio of the latent solvent and the polymol is (0-1):1; the second step, placing the precursor liquid of the ferroferric oxide in a glass tube used by microwave; conducting microwave heating reaction in a microwave reactor; and obtaining magnetic ferroferric oxide particles after the reaction. The method is simple and quick; the prepared magnetic ferroferric oxide particles have the advantages of strong magnetism, adjustable size and good dispersibility, as well as dispersion in water or organic solvent, and suitability for application in the biomedicine field or the mechanical electronic field.
Description
Technical field
That the present invention relates to is a kind of preparation method of field of nanometer technology, and specifically, what relate to is a kind of method with the microwave preparation nanometer ferroferric oxide microballoons with particle diameter adjustable.
Background technology
Z 250 (Fe
3O
4) material is a kind of ferromagnetic compound, works as Fe
3O
4Particle diameter is during less than 30 nanometers, Fe
3O
4Particle has superparamagnetism, and promptly under externally-applied magnetic field, particle has magnetic, leaves externally-applied magnetic field, and particle is nonmagnetic, disperses rapidly.Therefore, be carrier with the magnetic microsphere, utilize Fe
3O
4The superparamagnetism energy of nanoparticle can be applicable to the separation of cell, protein, nucleic acid, immunodiagnosis kit, and biomedical Application Areas such as drug targeting carrier.The preparation method of nano ferriferrous oxide has a variety of, is divided into wet method and dry method generally, and wet method is many to be raw material with ferrous salt and ferric salt, adopts methods such as coprecipitation method, oxidation reduction process, hydrothermal method, high-temperature decomposition to prepare; Dry method often adopts method preparations such as flame decomposition, vapour deposition or LASER HEAT decomposition, strict control reaction conditions of traditional preparation method and stoichiometry.Be accompanied by the development of nano materials research technology, new synthetic method and technology continue to bring out.
Find through literature search prior art, a kind of preparation method who adopts radiation chemistry is disclosed among the Chinese patent CN1260136C " manufacture method of nano ferriferrous oxide ", the electron beam that utilizes rumbatron to produce carries out radiation treatment to the basic iron solion and obtains Z 250, this method needs accelerator, is difficult for promoting; The microwave synthetizing nano material has advantages such as weak point consuming time, low, the pressure of power consumption and Controllable Temperature because of it, be applied in the synthetic and preparation field of nano material gradually.During sending out, retrieval also finds, disclosing a kind of among the Chinese patent CN100381363C " process for temperature-control pressure-control microwave synthesis of water-soluble ferroferric oxide nano crystal " is solvent with water, molysite and ferrous salt are raw material, in basic solution, adopt microwave reactor, prepare ferroferric oxide nano crystal by temperature-control pressure-control, this method needs the strict control molysite and the ratio of ferrous salt and the pH value of solution could prepare the good ferriferrous oxide nano-particle of magnetic property in preparation process, and the ferriferrous oxide nano-particle for preparing only is dispersed in the aqueous solution, the Application Areas difference of magnetic nano-particle, need different dispersion medium, therefore, in application, be restricted.
Summary of the invention
The present invention is directed to defective of the prior art, a kind of method with the microwave preparation nanometer ferroferric oxide microballoons with particle diameter adjustable is provided, with the molysite is raw material, adopt microwave technology in non-aqueous solvent fast, the novel method of safety, convenient preparation magnetic Nano microsphere, this method can prepare the magnetic nano-particle that size distribution is even, controlled, list disperses, saturation magnetization is high, according to the kind difference that adds tensio-active agent, can be scattered in different solvent mediums, to satisfy the application of different field.
The present invention is achieved by the following technical solutions, the present invention includes following steps:
The first step is dissolved in molysite in the polyvalent alcohol, adds inorganic salt and tensio-active agent again, and adds solubility promoter, mixes the back and stirs, and obtains preparing the precursor liquids of Z 250.
Described molysite comprise in iron(ic) chloride, iron nitrate, basic ironic acetate, the ferric acetyl acetonade etc. a kind of or their mutual blended any one.
Described polyvalent alcohol comprises ethylene glycol, glycerol, 1, any one in a kind of or their mixtures in the ammediol etc., the mass ratio 5～100: 1 of polyvalent alcohol and molysite.
Described inorganic salt comprise in sodium-acetate (or Potassium ethanoate), yellow soda ash (or salt of wormwood), sodium bicarbonate (or saleratus), Sodium Tetraborate, sodium tartrate, the trisodium citrate etc. a kind of or their mutual blended any one, the mass ratio 1～6: 1 of inorganic salt and molysite.
Described tensio-active agent comprise among polyoxyethylene glycol, cetyl trimethylammonium bromide, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, polyvinyl alcohol, polyvinylpyrrolidone, polyoxyethylene lauryl ether, oleic acid, tween, class of department, the Triton X (Triton X) etc. a kind of or their mutual blended any one, the mass ratio 0～5: 1 of tensio-active agent and molysite.If what add is that the Z 250 particle that ionic or hydrophilic nonionic surface active agent prepare can be scattered in water and the alcoholic acid polar solvent medium; If what add is that the Z 250 particle that lipophilic nonionic surface active agent prepares can be scattered in the nonpolar organic solvent medium.On the other hand, under identical volumetric molar concentration, if the chain length or the polymerization degree value height of the tensio-active agent that adds, the magnetic-particle that then prepares is big, this magnetic-particle wraps up a plurality of nano ferriferrous oxide particles by tensio-active agent and forms, the Z 250 particle number of tensio-active agent chain length parcel is many, and the magnetic microsphere particle diameter of Xing Chenging is big at last; If use tensio-active agent of the same race in the system, along with the increase of tensio-active agent add-on, the micella quantity that then forms in the system increases, and the magnetic microsphere particle diameter for preparing diminishes.
Described solubility promoter comprises quadrol, methane amide, 1, a kind of or their the mutual blended in 4-butanediamine, the butanolamine etc. any one, the volume ratio 0～1: 1 of solubility promoter and polyvalent alcohol.Volumetric molar concentration along with molysite in the increase system of solubility promoter add-on in preparation process descends, the nucleation rate of product body also descends, crystal is slowly grown, the Z 250 particle that finally prepares is big, therefore, can prepare the different nano ferriferrous oxide particle of particle diameter by the add-on that changes solubility promoter.
Stir described mixing back, and its churning time is 10 minutes～1 hour, makes the abundant mixing of mixture.
Second step, with the Glass tubing that the precursor liquids of Z 250 places microwave to use, in microwave reactor, carry out the microwave heating reaction, obtain the magnetic ferroferric oxide nano-particles of black after the reaction.
Described microwave heating reaction, its reaction conditions is: microwave power 15W～800W, 30 seconds～5 hours heat-up time, 120 ℃～250 ℃ of Heating temperatures, pressure 15PSI～250PSI.
The present invention is scattered in the different solvents magnetic particle of preparation by the kind of option table surface-active agent; Kind and add-on by changing tensio-active agent or change the particle diameter that the amount that adds solubility promoter is controlled prepared particle, the particle diameter that makes ferriferrous oxide nano-particle is at 8nm～100nm, size distribution is 5%～15%, saturation magnetization is at 55emu/g～85emu/g, and the magnetic particle of preparation can be used for biomedical sector and mechano-electronic field etc.
Description of drawings
Fig. 1 is the X-ray diffracting spectrum of the ferriferrous oxide nano-particle for preparing of the embodiment of the invention.
Fig. 2 is the magnetic hysteresis loop figure of the ferriferrous oxide nano-particle for preparing of the embodiment of the invention.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.
Take by weighing 0.3 gram iron(ic) chloride (FeCl
36H
2O) be dissolved in 10 milliliters the ethylene glycol, add the sodium-acetate and the 0.1 gram polyoxyethylene glycol (molecular weight 4000) of 0.8 gram, mix the back and stirred 20 minutes, obtain preparing the precursor liquids of Z 250.
Resulting precursor liquids is put into the glassware that is exclusively used in microwave reaction carry out microwave reaction, the condition of microwave radiation is as follows: microwave power 15W; Temperature 200 degree; Pressure 20PSI; 5 hours time.Prepare ferriferrous oxide nano-particle after the microwave radiation, particle diameter is 25nm, and saturation magnetization is 63.1emu/g, and the ferriferrous oxide nano-particle that makes can be scattered in water and the ethanol.
Take by weighing 0.3 gram iron(ic) chloride (FeCl
36H
2O) be dissolved in 10 milliliters 1, in the ammediol, add the sodium-acetate and the 0.2 gram polyoxyethylene glycol (molecular weight 8000) of 0.8 gram, mix the back and stirred 20 minutes, obtain preparing the precursor liquids of Z 250.
Resulting precursor liquids is put into the glassware that is exclusively used in microwave reaction carry out microwave reaction, the condition of microwave radiation is as follows: microwave power 50W; Temperature 200 degree; Pressure 30PSI; 30 minutes time.Prepare ferriferrous oxide nano-particle after the microwave radiation, particle diameter is 40nm, and saturation magnetization is 69.6emu/g, and the ferriferrous oxide nano-particle that makes can be scattered in water and the ethanol.
Embodiment 3.
Take by weighing 0.3 gram iron(ic) chloride (FeCl
36H
2O) be dissolved in 10 milliliters the glycerol, add the sodium-acetate and the 0.3 gram polyoxyethylene glycol (molecular weight 20000) of 0.5 gram, mix the back and stirred 20 minutes, obtain preparing the precursor liquids of Z 250.
Resulting precursor liquids is put into the glassware that is exclusively used in microwave reaction carry out microwave reaction, the condition of microwave radiation is as follows: microwave power 150W; Temperature 250 degree; Pressure 40PSI; 1 minute time prepared ferriferrous oxide nano-particle after the microwave radiation, particle diameter is 80nm, and saturation magnetization is 77.6emu/g, and the ferriferrous oxide nano-particle that makes can be scattered in water and the ethanol.
Embodiment 4.
Take by weighing 0.25 gram basic ironic acetate [Fe (OH) (CH
3COOH)
2] be dissolved in 10 milliliters the ethylene glycol, add the Sodium Tetraboratees of 1.2 grams, 4 milliliters of quadrols, 0.2 gram cetyl trimethylammonium bromide mixes the back and stirred 20 minutes, obtains preparing the precursor liquids of Z 250.
Resulting precursor liquids is put into the glassware that is exclusively used in microwave reaction carry out microwave reaction, the condition of microwave radiation is as follows: microwave power 150W; Temperature 200 degree; Pressure 60PSI; 3 minutes time prepared ferriferrous oxide nano-particle after the microwave radiation, particle diameter is 30nm, and saturation magnetization is 67.8emu/g, and the ferriferrous oxide nano-particle that makes can be scattered in the water.
Embodiment 5.
Take by weighing the nine nitric hydrate iron [Fe (NO of 0.45g
3)
39H
2O] be dissolved in 6 milliliters the ethylene glycol, add 0.6 gram sodium-acetate respectively, 0.2 gram trisodium citrate, 4 milliliters of quadrols, 0.1 gram sodium lauryl sulphate is mixed the back and was stirred 20 minutes, obtains preparing the precursor liquids of Z 250.
Resulting precursor liquids is put into the glassware that is exclusively used in microwave reaction carry out microwave reaction, the condition of microwave radiation is as follows: microwave power 100W; Temperature 200 degree; Pressure 60PSI; 3 minutes time prepared ferriferrous oxide nano-particle after the microwave radiation, particle diameter is 20nm, and saturation magnetization is 62.4emu/g, and the ferriferrous oxide nano-particle that makes can be scattered in the water.
Embodiment 6.
Take by weighing 0.3 gram iron(ic) chloride (FeCl
36H
2O) be dissolved in 8 milliliters the ethylene glycol, add 0.9 gram yellow soda ash respectively, 4 milliliters of quadrols, 0.5 milliliter of oleic acid mixes the back and stirred 20 minutes, obtains preparing the precursor liquids of Z 250.
Resulting precursor liquids is put into the glassware that is exclusively used in microwave reaction carry out microwave reaction, the condition of microwave radiation is as follows: microwave power 150W; Temperature 200 degree; Pressure 150PSI; 5 minutes time prepared ferriferrous oxide nano-particle after the microwave radiation, particle diameter is 10nm, and saturation magnetization is 58.1emu/g, and the ferriferrous oxide nano-particle that makes can be scattered in the organic solvents such as octane or hexanaphthene.
Embodiment 7.
Take by weighing 0.3 gram iron(ic) chloride (FeCl
36H
2O) be dissolved in 8 milliliters the ethylene glycol, add 0.9 gram sodium bicarbonate respectively, 2 milliliters of quadrols, 2 milliliters of methane amides mix the back and stirred 20 minutes, obtain preparing the precursor liquids of Z 250.
Resulting precursor liquids is put into the glassware that is exclusively used in microwave reaction carry out microwave reaction, the condition of microwave radiation is as follows: microwave power 100W; Temperature 125 degree; Pressure 200PSI; 5 minutes time prepared ferriferrous oxide nano-particle after the microwave radiation, particle diameter is 8nm, and saturation magnetization is 55.7emu/g, and the ferriferrous oxide nano-particle that makes can be scattered in the water.
The magnetic nano-particle for preparing among the above embodiment is after ethanol and water washing, and vacuum-drying obtains the powder of magnetic nano-particle, and powder is through the test and the vibrating sample magnetometer magnetometry performance of X-ray diffraction.The position at the X-ray diffraction peak of the magnetic nano-particle for preparing as shown in Figure 1, and intensity and Fe
3O
4The data of 19-0629 in the standard powdery diffractometry card are coincide, and show that the magnetic particle for preparing is ferriferrous oxide nano-particle (Fe
3O
4), as shown in Figure 1, can be observed sharp-pointed diffraction peak, Fe is described
3O
4The crystalline state of nanoparticle is good spinel type, and does not have the existence of other impurity crystalline phase diffraction peak among the figure, illustrates that product has higher purity.As shown in Figure 2, the magnetic hysteresis loop of the ferriferrous oxide nano-particle for preparing, as can be seen from the figure Zhi Bei Fe
3O
4Particle does not at room temperature have B-H loop, and very little coercive force has superparamagnetism and high saturation magnetization.
Claims (9)
1. the method with the microwave preparation nanometer ferroferric oxide microballoons with particle diameter adjustable is characterized in that, comprises the steps:
The first step, molysite is dissolved in the polyvalent alcohol, add inorganic salt and tensio-active agent again, and the adding solubility promoter, mix the back and stir, obtain preparing the precursor liquids of Z 250, wherein: the mass ratio 5～100: 1 of polyvalent alcohol and molysite, the mass ratio 1～6: 1 of inorganic salt and molysite, the mass ratio 0～5: 1 of tensio-active agent and molysite, the volume ratio 0～1: 1 of solubility promoter and polyvalent alcohol;
Second step, with the Glass tubing that the precursor liquids of Z 250 places microwave to use, in microwave reactor, carry out the microwave heating reaction, obtain the magnetic ferroferric oxide nano-particles of black after the reaction.
2. the method with the microwave preparation nanometer ferroferric oxide microballoons with particle diameter adjustable according to claim 1 is characterized in that, described molysite be in iron(ic) chloride, iron nitrate, basic ironic acetate, the ferric acetyl acetonade a kind of or their mutual blended any one.
3. the method with the microwave preparation nanometer ferroferric oxide microballoons with particle diameter adjustable according to claim 1 is characterized in that described polyvalent alcohol is ethylene glycol, glycerol, 1, any one in a kind of or their mixtures in the ammediol.
4. the method with the microwave preparation nanometer ferroferric oxide microballoons with particle diameter adjustable according to claim 1, it is characterized in that, described inorganic salt be in sodium-acetate or Potassium ethanoate, yellow soda ash or salt of wormwood, sodium bicarbonate or saleratus, Sodium Tetraborate, sodium tartrate, the trisodium citrate a kind of or their mutual blended any one.
5. the method with the microwave preparation nanometer ferroferric oxide microballoons with particle diameter adjustable according to claim 1, it is characterized in that, described tensio-active agent be among polyoxyethylene glycol, cetyl trimethylammonium bromide, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, polyvinyl alcohol, polyvinylpyrrolidone, polyoxyethylene lauryl ether, oleic acid, tween, class of department, the Triton X a kind of or their mutual blended any one.
6. the method with the microwave preparation nanometer ferroferric oxide microballoons with particle diameter adjustable according to claim 1 is characterized in that described solubility promoter is quadrol, methane amide, 1, a kind of or their the mutual blended in 4-butanediamine, the butanolamine any one.
7. the method with the microwave preparation nanometer ferroferric oxide microballoons with particle diameter adjustable according to claim 1 is characterized in that, stir described mixing back, and its churning time is 10 minutes～1 hour, makes the abundant mixing of mixture.
8. the method with the microwave preparation nanometer ferroferric oxide microballoons with particle diameter adjustable according to claim 1, it is characterized in that, described microwave heating reaction, its reaction conditions is: microwave power 15W～800W, 30 seconds～5 hours heat-up time, 120 ℃～250 ℃ of Heating temperatures, pressure 15PSI～250PSI.
9. the method with the microwave preparation nanometer ferroferric oxide microballoons with particle diameter adjustable according to claim 1 is characterized in that, described ferriferrous oxide nano-particle, and its particle diameter is controlled by the kind of tensio-active agent and the amount of add-on or solubility promoter.
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