CN104229901B - A kind of preparation method of magnetic ferroferric oxide nano-particles - Google Patents
A kind of preparation method of magnetic ferroferric oxide nano-particles Download PDFInfo
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- CN104229901B CN104229901B CN201410533527.0A CN201410533527A CN104229901B CN 104229901 B CN104229901 B CN 104229901B CN 201410533527 A CN201410533527 A CN 201410533527A CN 104229901 B CN104229901 B CN 104229901B
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Abstract
A preparation method for magnetic ferroferric oxide nano-particles, comprises the following steps: (1) is according to mol ratio FeCl3·6H2O:FeCl2·4H2The ratio of O=1.5-2:1, preparation mixed solution, adds sodium dodecyl sulfate solution; (2) logical nitrogen; Solution is heated to 45-55 DEG C simultaneously, then adds precipitating reagent ammoniacal liquor NH3·H2O, continues to heat up, ultrasonic; (3) magnet separates, and cleans, and freeze drying, grinds, and to obtain final product. In the preparation process of magnetic ferroferric oxide nano-particles of the present invention, omnidistance logical nitrogen, can effectively prevent the oxidation of particle in preparation process; Magnetic ferroferric oxide nano-particles prepared by the present invention has more uniform particle diameter, and particle diameter is distributed as 10-20nm; Have good magnetic property, saturated magnetic intensity >=76emu/g, can meet the requirement of magnetic carrier to particle diameter and magnetic.
Description
Technical field
The present invention relates to a kind of preparation method of magnetic ferroferric oxide nano-particles, belong to functional material preparation field.
Background technology
Magnetic ferroferric oxide nanometer material is a kind of special nano material, possesses the fundamental characteristics of common nano material, as dimensional effect, skin effect, quantum effect, macro quanta tunnel effect etc., also possess special superparamagnetism and class enzymatic activity simultaneously, at present at high density data storage, Magnetic resonance imaging, organize the aspects such as medicine release separates with classification, biological product with treatment, cell marking, immunoassays to be widely used. Based on the feature of its superparamagnetism, can separate and realize the object reclaiming fast for magnetic, the absorption carrier in separating as magnetic, prepared magnetic ferroferric oxide nanometer material requirements particle diameter is less, and magnetic is good, and specific area is large.
The method of preparing at present magnetic ferroferric oxide nano-particles is mainly chemical method, Physical, bioanalysis, Physical is mainly high energy ball milling method, bioanalysis is by from the method containing extraction magnetic nanometer in the organism of magnetic nanometer, particle diameter scope prepared by Physical is wayward, and the yield of bioanalysis is too low, therefore be not common method, very popular chemical method mainly comprises coprecipitation, emulsion method, hydro-thermal method, thermal decomposition, ultrasonic etc., chemical method can make up the deficiency of Physical and bioanalysis, forms the Fe that particle diameter is controlled, purity is higher3O4Magnetic nano-particle. In many preparation methods, coprecipitation is high with its productive rate, cost is low, good dispersion, particle diameter easily the feature of control become the most frequently used and industrialized production method, but there is the easy oxidation by air of the reactant liquor defect wide, magnetic difference that causes that particle size were is large, particle diameter distributes in traditional coprecipitation.
The domestic and international Fe for the preparation of magnetic fluid at present3O4The saturated magnetic intensity of nano particle is about 60emu/g. Zou Tao (Zou Tao, Guo Canxiong, Duan Xue. ferromagnetism Fe3O4The preparation of nano particle and performance characterization thereof. fine chemistry industry, 2002,19(12): 707-710.) the high magnetic Fe of preparation such as3O4The saturated magnetic intensity 75.9emu/g of nano particle, but its particle diameter is larger, and wider distribution, at 40-100nm. Qi Haiping etc. (Qi Haiping, Wan Junxi, Cao Hailin. co-precipitation-continuous micro-reaction method is prepared Fe3O4Nano particle. synthetic chemistry, 2014,22 (1): 114-116) magnetic Fe prepared3O4Nano particle diameter 15nm-20nm, saturation magnetization is 62.24emu/g. Be not well positioned to meet the requirement as magnetic carrier.
Summary of the invention
The technical problem to be solved in the present invention is, overcome the deficiency existing in existing precipitation method preparation method, a kind of preparation method of magnetic ferroferric oxide nano-particles is provided, its magnetic ferroferric oxide nano-particles of preparing has more uniform particle diameter, particle diameter is 10-20nm, have good magnetic property, saturated magnetic intensity >=76emu/g, can meet the requirement of magnetic carrier to particle diameter and magnetic.
The technical scheme that the present invention solves its technical problem employing is that a kind of preparation method of magnetic ferroferric oxide nano-particles, comprises the following steps:
(1) with FeCl3·6H2O and FeCl2·4H2O is raw material, takes FeCl3·6H2O and FeCl2·4H2O, is dissolved in respectively in ultra-pure water, is mixed with the solution of 0.020-0.060mol/L, then according to mol ratio FeCl3·6H2O﹕FeCl2·4H2The ratio of O=1.5-2 ﹕ 1, mixes two kinds of solution, obtains mixed solution, adds and be equivalent to mixed liquor volume 0.5%-1%(V/V in mixed solution) lauryl sodium sulfate (SDS) solution; Described sodium dodecyl sulfate solution concentration is the preferred 0.08-0.10mol/L of 0.05-0.12mol/L();
(2) solution preparing through step (1) is poured in there-necked flask into the high pure nitrogen of logical purity >=99.999%, the preferred 0.2-0.5L/min of nitrogen flow rate 0.03L/min-1.00L/min(), magnetic agitation, magnetic agitation speed is 300-400rpm; Solution is heated to 45-55 DEG C simultaneously, then adds precipitating reagent ammoniacal liquor NH3·H2O, to solution colour by bronzing blackening, when pH value of solution 9.5-10.5, stop adding ammoniacal liquor, continue to heat up, start timing during to 65-75 DEG C until temperature rise, after 20-40min, stop passing into nitrogen, close magnetic stirring apparatus, sealing there-necked flask, ultrasonic 3-7min, ultrasonic frequency is 20-60KHz;
(3) after question response liquid cooling but, utilize magnet separated product, product respectively cleans 3-5 time with ultra-pure water and ethanol respectively, soak 3-6min with the hydrochloric acid solution of 0.08-0.12mol/L again, then clean 1-2 time with ethanol, at-40 DEG C of-50 DEG C of freeze drying 24-30h, grind and obtain black powder again, be magnetic ferroferric oxide nano-particles.
In the preparation process of magnetic ferroferric oxide nano-particles of the present invention, omnidistance logical nitrogen, can effectively prevent the oxidation of particle in preparation process; Magnetic ferroferric oxide nano-particles prepared by the present invention has more uniform particle diameter, and particle diameter is distributed as 10-20nm; Have good magnetic property, saturated magnetic intensity >=76emu/g, can meet the requirement of magnetic carrier to particle diameter and magnetic.
Brief description of the drawings
Fig. 1 is the transmission electron microscope figure of the magnetic ferroferric oxide nano-particles of the embodiment of the present invention 1;
Fig. 2 is Fourier's infrared spectrogram of the magnetic ferroferric oxide nano-particles of the embodiment of the present invention 1;
Fig. 3 is the x-ray diffraction pattern of the magnetic ferroferric oxide nano-particles of the embodiment of the present invention 1;
Fig. 4 is the magnetic characteristic figure of the magnetic ferroferric oxide nano-particles of the embodiment of the present invention 1.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
The present embodiment comprises the following steps:
(1) take 0.018mol(4.86g) FeCl3·6H2O and 0.010mol(1.98g) FeCl2·4H2O, is dissolved into respectively in 300ml ultra-pure water, then two kinds of solution are mixed, and obtains mixed solution, adds lauryl sodium sulfate (SDS) solution of 6ml in mixed solution, and described SDS solution concentration is 0.1mol/L;
(2) solution preparing through step (1) is poured in there-necked flask, the high pure nitrogen of logical purity >=99.999%, nitrogen flow rate 0.3L/min, magnetic agitation, magnetic agitation rotating speed is 350rpm, solution is heated to 50 DEG C simultaneously, then adds precipitating reagent ammoniacal liquor NH3·H2O, can be observed solution colour and becomes bronzing from light green gradually and become bright black again, when pH value of solution 9.5-10.5, stops adding ammoniacal liquor; Continue to heat up, in the time of temperature rise to 70 DEG C, start timing, after half an hour, stop passing into nitrogen, close magnetic stirring apparatus, take off there-necked flask, sealing there-necked flask, ultrasonic (40KHz) processes 5min;
(3) after question response liquid cooling but, utilize external magnet to separate, product cleans respectively each 3 times with ultra-pure water and ethanol respectively, soak 5min with the hydrochloric acid solution of 0.1mol again,-50 DEG C of freeze drying 24h after ethanol cleaning once, grind, and obtain magnetic ferroferric oxide nano-particles.
In the preparation process of the present embodiment magnetic ferroferric oxide nano-particles, omnidistance logical nitrogen, has effectively prevented the oxidation of particle in preparation process, and magnetic ferroferric oxide nano-particles pattern characterizes by TEM, and particle diameter is shown in accompanying drawing 1 at 10-20nm(). The infrared ray diffraction spectrogram of magnetic ferroferric oxide nano-particles has shown the group (seeing accompanying drawing 2) of particle, and sample is at 569cm-1Place's sample has very strong absworption peak, can interpret sample be Fe3O4Particle, 1618cm-1The absworption peak at place is O-H bond bending generation of vibration, 3395cm-1Locate to such an extent that absworption peak is produced by the stretching vibration of O-H key, Fe is described3O4Particle surface is with a certain amount of-OH group.
The crystalline state of magnetic ferroferric oxide nano-particles represents (seeing accompanying drawing 3) by X-ray diffraction, has obvious characteristic peak (2 θ=30.19 °, 35.53 °, 43.42 °, 53.83 °, 57.22 °, 62.81 °), with Fe3O4Standard feature diffraction maximum contrast, corresponding Emission in Cubic Fe respectively3O4(220), (311), (400), (422), (511), (440) crystal plane, show prepared Fe3O4Nano particle is typical inverse spinel profile cubic structure.
Employing vibrations sample magnetometer obtains the hysteresis curve figure (seeing accompanying drawing 4) of particle, wherein Fe3O4The saturated magnetic intensity of nano particle is 76.277emu/g.
Claims (4)
1. a preparation method for magnetic ferroferric oxide nano-particles, is characterized in that, comprises the following steps:
(1) with FeCl3·6H2O and FeCl2·4H2O is raw material, takes FeCl3·6H2O and FeCl2·4H2O, is dissolved in respectively in ultra-pure water, is mixed with the solution of 0.020-0.060mol/L, then according to mol ratio FeCl3·6H2O﹕FeCl2·4H2The ratio of O=1.5-2 ﹕ 1, mixes two kinds of solution, obtains mixed solution, adds the sodium dodecyl sulfate solution that is equivalent to mixed liquor volume 0.5%-1% in mixed solution;
(2) solution preparing through step (1) is poured in there-necked flask, the high pure nitrogen of logical purity >=99.999%, nitrogen flow rate is 0.03L/min-1.00L/min, magnetic agitation, magnetic agitation speed is 300-400rpm; Solution is heated to 45-55 DEG C simultaneously, then adds precipitating reagent ammoniacal liquor NH3·H2O, to solution colour by bronzing blackening, when pH value of solution 9.5-10.5, stop adding ammoniacal liquor, continue to heat up, start timing during to 65-75 DEG C until temperature rise, after 20-40min, stop passing into nitrogen, close magnetic stirring apparatus, sealing there-necked flask, ultrasonic 3-7min, ultrasonic frequency is 20-60KHz;
(3) after question response liquid cooling but, utilize magnet separated product, product respectively cleans 3-5 time with ultra-pure water and ethanol respectively, soak 3-6min with the hydrochloric acid solution of 0.08-0.12mol/L again, then clean 1-2 time with ethanol, at-40 DEG C～-50 DEG C freeze drying 24-30h, grind and obtain black powder again, be magnetic ferroferric oxide nano-particles.
2. the preparation method of magnetic ferroferric oxide nano-particles according to claim 1, is characterized in that, in step (1), described sodium dodecyl sulfate solution concentration is 0.05-0.12mol/L.
3. the preparation method of magnetic ferroferric oxide nano-particles according to claim 2, is characterized in that, described sodium dodecyl sulfate solution concentration is 0.08-0.10mol/L.
4. the preparation method of magnetic ferroferric oxide nano-particles according to claim 1 and 2, is characterized in that, in step (2), described nitrogen flow rate is 0.2-0.5L/min.
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| CN104689783B (en) * | 2015-02-15 | 2017-04-12 | 湖南大学 | Ion oxide magnetic composite as well as preparation method and application of composite |
| CN104829137A (en) * | 2015-04-22 | 2015-08-12 | 同济大学 | Preparation method of magnetic borate biological-activity glass support |
| CN106256765B (en) * | 2016-07-28 | 2018-01-05 | 华南理工大学 | A kind of magnetic carboxymethyl chitosan nano material and preparation method thereof |
| CN106362654B (en) * | 2016-10-08 | 2019-04-02 | 江苏大学 | A kind of method that the Pickering emulsion polymerization technology that magnetism egg-shell meal is stable prepares trace microballoon |
| CN110193345A (en) * | 2019-05-05 | 2019-09-03 | 淮海工学院 | A kind of preparation method of magnetic nanometer composite material |
| CN110156090B (en) * | 2019-06-28 | 2021-08-10 | 中国科学院合肥物质科学研究院 | For preparing Fe3O4Fluid synthesis preparation device of magnetic nanoparticles and control method thereof |
| CN110255627A (en) * | 2019-07-12 | 2019-09-20 | 中国恩菲工程技术有限公司 | Nano ferriferrous oxide and preparation method thereof and system |
| CN113184916B (en) * | 2021-05-31 | 2023-05-23 | 中山职业技术学院 | Ferroferric oxide magnetic powder and preparation method thereof |
| CN114832793B (en) * | 2022-04-26 | 2023-06-20 | 中国药科大学 | Magnetic nano material for detecting tetrahydrocannabinic acid and synthesizing cannabinoid drugs, and preparation method and application thereof |
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| CN101049975A (en) * | 2007-05-15 | 2007-10-10 | 中国科学院长春应用化学研究所 | Method for preparing Fe2O3 Nano particles clad by Fe2O3 |
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| CN101049975A (en) * | 2007-05-15 | 2007-10-10 | 中国科学院长春应用化学研究所 | Method for preparing Fe2O3 Nano particles clad by Fe2O3 |
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