CN105289456A - Preparation method and application of superparamagnetic Fe3O4 nano material - Google Patents

Preparation method and application of superparamagnetic Fe3O4 nano material Download PDF

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CN105289456A
CN105289456A CN201510633098.9A CN201510633098A CN105289456A CN 105289456 A CN105289456 A CN 105289456A CN 201510633098 A CN201510633098 A CN 201510633098A CN 105289456 A CN105289456 A CN 105289456A
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preparation
nano material
superparamagnetic
tea
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CN105289456B (en
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韩成良
张凌云
朱德杰
姚李
徐泽忠
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Hefei University
Hefei College
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Abstract

The invention discloses a preparation method and application of a superparamagnetic Fe3O4 nano material, and relates to the technical field of nano materials. The preparation method comprises the following steps: dissolving solid FeCl3.6H2O into distilled water, stirring under room temperature, and fully dissolving, thus obtaining a solution a; slowly adding triethanolamine (TEA) into the solution a, continuously stirring, thus obtaining a brown red solution b, adjusting the pH value of the solution b by ammonia water or solid NaOH, thus obtaining a dark brown solution c, putting the solution c under a closed state for hydrothermal synthesis, and finally taking out a product by a magnetic separation method. The superparamagnetic Fe3O4 nano material prepared by the preparation method disclosed by the invehtion is better in water solubility, good in biocompatibility, high in adsorption performance and excellent in catalysis and magnetic property, can be applied to the fields such as magnetic resonance imaging, data storage, medicament and gene targeting, cell separation and sewage treatment, and has a wider application prospect.

Description

A kind of superparamagnetic Fe 3o 4the preparation method and application of nano material
Technical field
The present invention relates to technical field of nano material, specifically relate to a kind of superparamagnetic Fe 3o 4the preparation method and application of nano material.
Background technology
Superparamagnetic nanoparticle has important using value in magnetic resonance imaging, data storage, medicine and gene target, cell separation and thermotherapy etc.Fe 3o 4there is many advantages such as nontoxic and inexpensive, can as magnetic fluid, magnetic resonance imaging and electrode material of lithium battery etc.And the application of these aspects requires Fe mostly 3o 4material has higher stability, small size and high dispersive property etc.Meanwhile, research also shows, Fe 3o 4nano grain surface has bound state Fe 2+/ Fe 3+, with the H in solution 2o 2class Fenton's reaction system can be formed, be applied to the class Fenton catalytic degradation of organic pollution materials, in sewage disposal and environmental protection etc., have potential using value.Develop many preparation methods at present, mainly comprise coprecipitation, hydro-thermal method, reversed micelle method and iron oleate thermal decomposition method etc.
Take molysite as raw material, at room temperature, adopt coprecipitation to be preparation Fe 3o 4the common method of nano material.The method principle is Fe 3+and Fe 2+2: 1 mixing wiring solution-formings in molar ratio, the pH then by improving solution precipitates soon fast and generates Fe 3o 4, its reaction equation is as follows:
In addition, with Fe 3+for raw material, also can be used for preparing the Fe of various form by hydro-thermal reaction 3o 4nano material.Such as, with FeCl 3.6H 2the O aqueous solution is raw material, adds the reducing agents such as ethylene glycol, winter propylhomoserin, hydrazine hydrate, VC and Fe powder wherein respectively, can obtain different shape Fe by hydro-thermal reaction 3o 4nano material.
But the whole preparation process of coprecipitation all needs to carry out under inert gas shielding, cause preparation process complicated.Meanwhile, the method is generally carry out at low temperatures, the Fe obtained 3o 4degree of crystallinity and magnetic property are all poor.Hydro-thermal reaction method exists that purity is low, cost is high and the limitation such as complicated operation usually, thus limits its practical application.For this reason, a kind of quick, low cost and green syt superparamagnetic Fe is sought 3o 4method is still a problem being worth research.
Summary of the invention
In order to overcome the above-mentioned defect existed in prior art, the object of the present invention is to provide a kind of superparamagnetic Fe 3o 4the preparation method of nano material, the product of preparation has biocompatibility water-soluble, good preferably, high adsorption, excellent catalysis and magnetic performance.
For realizing this object, present invention employs following technical scheme: a kind of superparamagnetic Fe 3o 4the preparation method of nano material, adopt hydrothermal synthesis method, step is as follows:
Step 1 is 0.1 ~ 0.5: 5 ~ 15 by solid-state FeCl according to mol ratio 36H 2o is dissolved in distilled water, and stirred at ambient temperature makes it fully to dissolve to obtain solution a;
Step 2, slowly joins in solution a by triethanolamine (TEA), and triethanolamine (TEA) is 10: 1 with the volume ratio of distilled water, continues stirring and obtains in henna solution b;
Step 3, regulates the pH value of solution b to be 7 ~ 14 with ammoniacal liquor or solid NaOH, obtains in auburn solution c;
Step 4, is placed in air-tight state in 160 ~ 200 DEG C of reactions 1.5 ~ 24 hours, takes out product with magnetism separate method by solution c.
As superparamagnetic Fe of the present invention 3o 4the further improvement of the preparation method of nano material, solid-state FeCl in step 1 36H 2in the dissolving of O and step 2, triethanolamine (TEA) is added and all to be mixed by magnetic stirring apparatus afterwards, and mixing time is 1 ~ 3 minute.Preparation method also comprises the product of gained in step 4 is placed in baking oven at 50 ~ 70 DEG C step of dry 2 ~ 6 hours.
The present invention successfully obtains a kind of superparamagnetic Fe by quick hydro-thermal method 3o 4nano material, and have studied its absorption and catalytic elimination organic pollution characteristic.The Fe obtained in finite concentration TEA reaction system is shown by a series of sign 3o 4nano material has the advantages such as narrower particle size distribution, higher specific area and stronger ferromagnetism.
Meanwhile, the Fe of gained 3o 4nano material has higher absorption property, at a certain amount of H 2o 2in system, can realize to the methylene blue in the aqueous solution and rhodamine B degradable.Therefore, this Fe 3o 4nano material is expected to be used as reusable organic sewage inorganic agent.In addition, it also has potential application prospect in drug targeting, biological medicine.
Compared with prior art, beneficial effect of the present invention shows:
1, present invention achieves by single Fe (TEA) 3+coordination ion solution is presoma, can obtain Fe by Fast back-projection algorithm 3o 4nano material is superparamagnetic Fe 3o 4the synthesis of nano material provides a kind of new approach.
2, present invention process is simple, and whole preparation system easily builds, easy and simple to handle, condition is easily controlled, with low cost, easily control, product are evenly distributed, not easily reunite, are suitable for large-scale industrial production product composition.
3, the present invention adopts conventional soluble molysite as reactant, and the accessory substance produced in preparation process is few, and environmental pollution is less, is a kind of environment-friendly type synthesis technique.This simple synthetic method also can construct the magnetic composite nano material of other multicomponent load as a kind of general strategy.
4, the product that prepared by the present invention has biocompatibility water-soluble, good preferably, high adsorption, excellent catalysis and magnetic performance, the fields such as magnetic resonance imaging, data storage, medicine and gene target, cell separation and sewage disposal can be applied in, have comparatively wide application prospect.
Accompanying drawing explanation
Fig. 1 is the XRD figure of embodiment 1 products therefrom.
Fig. 2 a is the FE-SEM figure of embodiment 1 products therefrom.
Fig. 2 b is the particle size distribution figure of embodiment 1 products therefrom.
Fig. 2 c is the TEM/SAED figure of embodiment 1 products therefrom.
Fig. 2 d is the HRTEM figure of embodiment 1 products therefrom.
Fig. 3 a is the VSM figure of embodiment 1 products therefrom.
Fig. 3 b is macroscopical magnetic demonstration graph of embodiment 1 products therefrom.
Fig. 4 a be embodiment 1 products therefrom be adsorbed with organic dye kinetic curve.
Fig. 4 b is the kinetic curve Linear Fit Chart of Fig. 4 a.
Fig. 5 a is the Fenton catalytic degradation organic dyestuff kinetic curve of embodiment 1 products therefrom.
Fig. 5 b is the kinetic curve Linear Fit Chart of Fig. 5 a.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.Instrument or the equipment such as X-ray powder diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscope (FE-SEM), transmission electricity border (TEM), vibration magnetometer (VSM), thermogravimetric differential thermal measuring instrument (TG/DSC), automatic absorbing instrument, ultraviolet-visible spectrophotometer (UV-Vis) has been selected respectively when the structure of products therefrom, pattern, composition are characterized.
Preparation embodiment 1: preparation superparamagnetic Fe 3o 4nano material
(1) be 0.5: 5 by solid-state FeCl according to mol ratio 36H 2o is dissolved in distilled water, and room temperature lower magnetic force stirs and within 2 minutes, makes it fully to dissolve to obtain solution a.
(2) slowly join in solution a by triethanolamine (TEA) solution again, triethanolamine (TEA) is 10: 1 with the volume ratio of distilled water, continues magnetic agitation and within 2 minutes, obtains in henna solution b.
(3) regulate the pH of solution b to be 10 with solid NaOH, obtain in auburn solution c.
(4) load in reactor by solution c, in 180 DEG C of reactions 1.5 hours, take out product with magnetism separate method, the product obtained in an oven 60 DEG C of dryings can obtain superparamagnetic Fe in 4 hours 3o 4nano material.
Fig. 1 is the XRD spectra of embodiment 1 products therefrom, with the Fe of standard 3o 4spectrogram (JCPDS:76-1849) is compared and can be obtained, and is high-purity Fe at the product of embodiment 1 gained 3o 4, in addition, particle size can be obtained according to Scherrer formula with the halfwidth of (311) crystal face and be about 10nm.
D＝Kλ/Bcosθ
K:Scherrer constant; D is crystallite dimension; B is diffraction maximum halfwidth; θ is the angle of diffraction; λ is X-ray wavelength.
Fig. 2 (a) is ESEM (SEM) photo of embodiment 1 products therefrom, the as known in the figure Fe of embodiment 1 gained 3o 4for irregular particle, particle diameter is less, better dispersed.Nanomeasurer analysis software is adopted to carry out the result after statistical analysis as shown in Fig. 2 (b) to granularity, known Fe 3o 4size is about 10nm, consistent with the result that Fig. 1 obtains.Fig. 2 (c) and Fig. 2 (d) is respectively Fe 3o 4tEM and the HRTEM figure of product, by Tu Ke get: the form of product is that class is spherical, and crystallization degree is high, good dispersion, and the diameter of particle is about 10nm; Each particle is monocrystalline, confirms that the product obtained is tri-iron tetroxide further by (311) and (222) interplanar distance.
Fig. 3 (a) is that the room temperature magnetic hysteresis of embodiment 1 products therefrom returns money, and as seen from the figure, the product of gained is Superparamagnetic particulates (coercivity H cbe 0), saturation magnetization is about 65emu/g.Found out further by the illustration in Fig. 3 (a) lower right corner, superparamagnetic Fe 3o 4particle is very well dispersed in water, presents Tyndall phenomenon, shows colloid property.Fig. 3 (b) is in or without in both external magnetic fields situation for magnetic dispersion liquid respectively, the macroscopic magnetization demonstration graph of magnetic colloid solution.Further demonstrate dispersiveness in water of the magnetic-particle prepared and magnetic response performance all very good.
Preparation embodiment 2: preparation superparamagnetic Fe 3o 4nano material
(1) be 0.1: 5 by solid-state FeCl according to mol ratio 36H 2o is dissolved in distilled water, and room temperature lower magnetic force stirs and within 1 minute, makes it fully to dissolve to obtain solution a.
(2) slowly join in solution a by triethanolamine (TEA) solution again, triethanolamine (TEA) is 10: 1 with the volume ratio of distilled water, continues magnetic agitation and within 3 minutes, obtains in henna solution b.
(3) regulate the pH of solution b to be 9 with ammoniacal liquor, obtain in auburn solution c.
(4) load in reactor by solution c, in 200 DEG C of reactions 2 hours, take out product with magnetism separate method, the product obtained in an oven 50 DEG C of dryings can obtain superparamagnetic Fe in 6 hours 3o 4nano material.
Preparation embodiment 3: preparation superparamagnetic Fe 3o 4nano material
(1) be 0.5: 15 by solid-state FeCl according to mol ratio 36H 2o is dissolved in distilled water, and room temperature lower magnetic force stirs and within 3 minutes, makes it fully to dissolve to obtain solution a.
(2) slowly join in solution a by triethanolamine (TEA) solution again, triethanolamine (TEA) is 10: 1 with the volume ratio of distilled water, continues magnetic agitation and within 1 minute, obtains in henna solution b.
(3) regulate the pH of solution b to be 8 with ammoniacal liquor, obtain in auburn solution c.
(4) load in reactor by solution c, in 160 DEG C of reactions 6 hours, take out product with magnetism separate method, the product obtained in an oven 70 DEG C of dryings can obtain superparamagnetic Fe in 2 hours 3o 4nano material.
Application Example 1: superparamagnetic Fe 3o 4nano material absorbing dye
(1) take rhodamine B as target contaminant, at 100mL rhodamine B initial concentration C 0for adding the Fe prepared by 0.02g embodiment 1 in the solution of 10mg/L 3o 4adsorbent, obtains mixed liquor a after Quick uniform mixing, and starts timing.
(2) t 1after minute, from a solution, take out 10mL proceed in the test tube of 20mL dried and clean, and magnet is pressed close to test tube wall and carry out quick Magneto separate, then, from test tube, get part containing the liquid b of magnetic adsorbent.
(3) absorbance A of the solution b obtained after Magneto separate is tested with ultraviolet-visible spectrometer 1, after being completed, refunding test tube and back in solution a after shaking up together with remaining solution and adsorbent.
(4) t 2minute, t 3minute and t 4minute, t 5minute and t 6sampling after minute is identical with (3) two steps with (2) with test process, and the serial absorbance recorded is labeled as A respectively 2, A 3, A 4, A 5and A 6.
(5) time t is made 1and absorbance A 1(i=0,1,2,3,4,5,6) curve.The concentration C after different time is calculated again according to absorbance and concentration relationship t.
(6) last basis calculate q t, then make q t~ t relation curve gets final product curve of adsorption kinetics.
Fig. 4 a is the curve of adsorption kinetics of rhdamine B, can find out in conjunction with its illustration, and after 90 minutes, certain density rhodamine B is substantially clean by Adsorption.The linear fit that Fig. 4 (b) is kinetic curve, has fitting result known, relative coefficient R 2=0.99, can t/q be obtained thus tlinear relationship is met with t.Therefore, the kinetic model that the superparamagnetic Fe3O4 nano material that prepared by embodiment 1 adsorbs rhdamine B meets accurate second-order dynamic equation.As can be seen here, this superparamagnetic Fe 3o 4nano material has excellent absorption property and can conveniently reclaim, and can reuse.
Application Example 2: superparamagnetic Fe 3o 4nano material Fenton catalytic degradation organic matter
(1) with rhodamine B and methylene blue for target contaminant, in the 100mL rhodamine B initial concentration solution that is 20mg/L, add the Fe prepared by 0.02g embodiment 1 3o 4the H of adsorbent and 1mL 2o 2, obtain mixed liquor a after Quick uniform mixing, and start timing.
(2) t 1after minute, from a solution, take out 10mL proceed in the test tube of 20mL dried and clean, and magnet is pressed close to test tube wall and carry out quick Magneto separate, then, from test tube, get part containing the liquid b of magnetic adsorbent.
(3) absorbance A of the solution b obtained after Magneto separate is tested with ultraviolet-visible spectrometer 1, after being completed, refunding test tube and back in solution a after shaking up together with remaining solution and adsorbent.
(4) t 2minute, t 3minute and t 4minute, t 5minute and t 6sampling after minute is identical with (3) two steps with (2) with test process, and the serial absorbance recorded is labeled as A respectively 2, A 3, A 4, A 5and A 6.
(5) time t is made 1and absorbance A 1(i=0,1,2,3,4,5,6) curve.Adsorption time t and concentration C is calculated again according to absorbance A and concentration C relation (langbobier law) trelation curve.
Fig. 5 (a) is superparamagnetic Fe 3o 4nano material is to the Fenton catalytic kinetics curve of rhodamine B and methylene blue, and as seen from the figure, two kinds of organic concentration extend continuous reduction in time.Use first order reaction kinetics model wherein, C torganic concentration in solution after catalytic action t, C 0be the initial concentration of reaction solution, K is speed constant.) matching is carried out to experimental data, fitting result as shown in Fig. 5 (b), for the coefficient R that rhodamine B and methylene blue matching obtain 20.998 and 0.921 respectively.

Claims (5)

1. a superparamagnetic Fe 3o 4the preparation method of nano material, adopts hydrothermal synthesis method, it is characterized in that step is as follows:
Step 1 is 0.1 ~ 0.5: 5 ~ 15 by solid-state FeCl according to mol ratio 36H 2o is dissolved in distilled water, and stirred at ambient temperature makes it fully to dissolve to obtain solution a;
Step 2, slowly joins in solution a by triethanolamine (TEA), and triethanolamine (TEA) is 10: 1 with the volume ratio of distilled water, continues stirring and obtains in henna solution b;
Step 3, regulates the pH value of solution b to be 7 ~ 14 with ammoniacal liquor or solid NaOH, obtains in auburn solution c;
Step 4, is placed in air-tight state in 160 ~ 200 DEG C of reactions 1.5 ~ 24 hours, takes out product with magnetism separate method by solution c.
2. preparation method as claimed in claim 1, is characterized in that: solid-state FeCl in step 1 36H 2in the dissolving of O and step 2, triethanolamine (TEA) is added and all to be mixed by magnetic stirring apparatus afterwards, and mixing time is 1 ~ 3 minute.
3. preparation method as claimed in claim 1, is characterized in that: the product of gained in step 4 is placed in baking oven at 50 ~ 70 DEG C dry 2 ~ 6 hours.
4. the superparamagnetic Fe for preparing of method as claimed in claim 1 3o 4the application of nano material in Adsorption organic pollution.
5. the superparamagnetic Fe for preparing of method as claimed in claim 1 3o 4the application of nano material in Fenton catalyze and degrade organic pollutants.
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CN108212127A (en) * 2018-01-18 2018-06-29 河海大学 A kind of preparation method and application of function nano composite hydrogel
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