CN103058283A - Preparation method of iron oxides with adjustable size, appearance and compositions - Google Patents
Preparation method of iron oxides with adjustable size, appearance and compositions Download PDFInfo
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- CN103058283A CN103058283A CN2013100389320A CN201310038932A CN103058283A CN 103058283 A CN103058283 A CN 103058283A CN 2013100389320 A CN2013100389320 A CN 2013100389320A CN 201310038932 A CN201310038932 A CN 201310038932A CN 103058283 A CN103058283 A CN 103058283A
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Abstract
The invention discloses a preparation method of iron oxides with adjustable size, appearance and compositions. The preparation method comprises the steps of: adding ferric salt, sodium bicarbonate and organic amine to an organic solvent, and stirring to obtain a transparent solution; and carrying out heat treatment on the solution, carrying out centrifugal separation, and washing to obtain the iron oxides particles. The iron oxides particles comprise ferric oxide particles and ferroferric oxide particles, have the diameter of 10-600nm, and are solid, meso-porous or hollowly spherical in appearance. The preparation method is simple in preparation process; the yield of the iron oxides is high; the size distribution of the products is narrow, and the products have high saturated magnetic field intensity; the iron oxides with different sizes, appearances and compositions can be obtained by simply controlling reaction conditions; and the preparation method is significant for preparation and application of the iron oxide particles.
Description
Technical field
The present invention relates to a kind of preparation method of iron oxide particle, be specifically related to the preparation method of the adjustable iron oxide particle of a kind of size, pattern and composition.
Background technology
Ferriferous oxide comprises FeO, Fe
2O
3And Fe
3O
4, Fe wherein
2O
3And Fe
3O
4Micro-nano granules has widely to be used.The Fe 3 O 4 magnetic micro-and nano-particles is widely used in the fields such as magnetic fluid, Magnetic resonance imaging, biological medicine, data storage.Fe
2O
3Micro-and nano-particles has in fields such as coating, electronic product, magnetic recording material, catalyzer and biomedical engineerings extremely widely to be used.The ferriferous oxide of hollow structure makes it have unique character owing to having inner-cavity structure and the surfaces externally and internally of lower density, uniqueness, has very great application at water treatment, biomarker and the aspects such as control release, catalysis.
Have with the ferriferous oxide of solvent-thermal method preparation at present both at home and abroad that good crystallinity, output are high, the magnetic saturation intensity advantages of higher.CN 201210158461.2 discloses a kind of method of controlling Z 250 pattern and performance, the transformation that being characterized in can be simply, method realizes the ferriferrous oxide particles pattern efficiently.CN 200810062614.7 discloses the method for utilizing iron trichloride, methyl alcohol (or ethanol, ethylene glycol) and sodium hydroxide to prepare the ferriferrous oxide nano-particle of spheroidal particle as starting raw material.CN201010283732.8 discloses a kind of alpha-type ferric oxide micron ball and preparation method thereof, provides a kind of particle balling preparation rate high, the distribution of sizes homogeneous, and have the preparation method of the alpha-type ferric oxide micron ball of superior magnetic property.In addition, document " Peng Hu, Lingjie Yu, Ahui Zuo, Chenyi Guo, and Fangli Yuan. J. Phys. Chem. C, 2009,113,900 – 906 " has been reported the preparation of Z 250 hollow ball.
Gained granulometric composition and granule-morphology are certain according to the method described above, the control reaction conditions only can make the grain diameter size change, the composition and the pattern that change particle need to change the preparation method, can not realize simply, efficiently the transformation of iron oxide particle size, pattern, composition.
Summary of the invention
The present invention is directed to the deficiency that existing method exists, this has been proposed improvement, the preparation method of the adjustable iron oxide particle of a kind of size, pattern and composition is provided, selection and control composition and the pattern that can simply, effectively change ferriferous oxide of this preparation method by reaction conditions is easy to control and realizes.
Concrete technical scheme is as follows:
A kind of preparation method of iron oxide particle is characterized in that: described iron oxide particle is ferric oxide particle or ferriferrous oxide particles, may further comprise the steps:
(1) molysite, sodium bicarbonate, organic amine are joined in the organic solvent, stir and obtain clear solution;
(2) solution that step (1) is made into is heat-treated, the preparation ferriferous oxide;
(3) with reaction solution centrifugation, washing, the gained throw out is iron oxide particle.
In the aforesaid method, described molysite is halogenide, vitriol or the nitrate of iron, such as FERRIC CHLORIDE ANHYDROUS, Iron(III) chloride hexahydrate, ferric sulfate, iron nitrate etc.
In the aforesaid method, described organic amine is quadrol, propylene diamine, butanediamine or thanomin.
In the aforesaid method, can be by the particles of choosing to obtain different compositions of control organic solvent, during the preparation ferric oxide particle, described organic solvent is methyl alcohol, ethanol, propyl alcohol, butanols or Virahol; During the preparation ferriferrous oxide particles, described organic solvent is ethylene glycol, propylene glycol, butyleneglycol or glycerol.
In the aforesaid method, the mol ratio of molysite and sodium bicarbonate is 1:0.3-8, can by control molysite and sodium bicarbonate obtain the particulate matter of different-shape with magnitude relation, when the mol ratio of molysite and sodium bicarbonate was 1:0.3 ~ 2.9, the gained iron oxide particle was solid sphere; Mol ratio is 1:3 ~ 5 o'clock, and the gained iron oxide particle is mesoporous sphere; Mol ratio is 1:5 ~ 8 o'clock, and the gained iron oxide particle is hollow ball shape.
In the aforesaid method, the mol ratio of molysite and organic amine is 0.9 ~ 36:1.
In the aforesaid method, the volume ratio of organic solvent and organic amine is 1:0.005 ~ 0.2.
In the aforesaid method, gained particulate matter diameter is in 10 ~ 600 nm scopes, and granular size can controlling with magnitude relation, heat-treat condition by organic solvent and organic amine.Heat-treating methods is solvent-thermal method or microwave method, and heat treated temperature is 150-260 ℃, and the heat treated time is generally 4 ~ 24h.Generally, obtain the particle of a certain size, fix on the basis of other conditions, the low required time of thermal treatment temp is longer, and the high required time of thermal treatment temp is shorter.
The present invention utilizes solvent-thermal method or microwave method to prepare simply efficiently the iron oxide particle of size, pattern, sphere that composition is adjustable.By the control reaction conditions, obtain diameter at the difference composition of 10 ~ 600 nm scopes, the iron oxide particle of different-shape.In present method, can obtain the different iron oxide particles that form by the kind that changes organic solvent; By changing the ratio of molysite and sodium bicarbonate, can obtain the iron oxide particle of different-shape; By adjusting ratio and temperature of reaction and the time of organic amine and organic solvent, can control the size of iron oxide particle.The reaction controllability is strong, product production high (productive rate reaches more than 90%), and magnetic saturation intensity high (being about 65 ~ 85 emu/g), particulate component, morphology change boundary line are clear and definite, are easy to control and realize.
Preparation technology of the present invention is simple, production cost is low, Modulatory character is strong, can obtain the iron oxide particle of different size, pattern, composition by simple control reaction conditions, the products therefrom narrow diameter distribution, output is high, purity is high, saturation magnetic field intensity is high, in fields such as magnetic recording material, catalyzer, biomedical engineering, Magnetic resonance imaging, data storages extremely widely application is arranged, this invents the preparation of ferriferous oxide ball and uses significant.
Description of drawings
Fig. 1 is transmission electron microscope (TEM) picture of the synthetic solid Z 250 of the embodiment of the invention 1.
Fig. 2 is X-ray diffraction (XRD) collection of illustrative plates of the synthetic solid Z 250 of the embodiment of the invention 1.
Fig. 3 is the magnetic hysteresis loop collection of illustrative plates of the synthetic solid Z 250 of the embodiment of the invention 1.
Fig. 4 is the particle size distribution figure of the synthetic solid Z 250 of the embodiment of the invention 1.
Fig. 5 is transmission electron microscope (TEM) picture of the synthetic mesoporous ferriferrous oxide of the embodiment of the invention 2.
Fig. 6 is the particle size distribution figure of the synthetic mesoporous ferriferrous oxide of the embodiment of the invention 2.
Fig. 7 is transmission electron microscope (TEM) picture of the synthetic hollow Z 250 of the embodiment of the invention 3.
Fig. 8 is transmission electron microscope (TEM) picture of the synthetic solid Z 250 of the embodiment of the invention 4.
Fig. 9 is the magnetic hysteresis loop collection of illustrative plates of the synthetic solid Z 250 of the embodiment of the invention 4.
Figure 10 is transmission electron microscope (TEM) picture of the synthetic hollow Z 250 of the embodiment of the invention 5.
Figure 11 is transmission electron microscope (TEM) picture of the synthetic hollow ferric oxide of the embodiment of the invention 6.
Figure 12 is X-ray diffraction (XRD) collection of illustrative plates of the synthetic hollow ferric oxide of the embodiment of the invention 6.
Embodiment
The present invention will be further elaborated below by embodiment, and following explanation only in order to explain the present invention, does not limit its content.
Embodiment 1
1.1 ferric chloride hexahydrate, the sodium bicarbonate of 0.45 g, the 1 mL quadrol of 0.676 g are joined in the 30 mL ethylene glycol and stir to clarify;
1.2 mentioned solution is transferred in the reactor, 200 ℃ of lower reactions 16 hours;
After 1.3 reaction finishes, through obtaining solid Z 250 particle after centrifugation and the washing.The diameter of particle is 320 nm, and X-ray diffraction characterizes and proves Z 250, and magnetic saturation intensity is that 78.95 emu/g. particle diameters are even.Respectively shown in Fig. 1,2,3,4.The output of sample is 92.3%.
Embodiment 2
2.1 ferric chloride hexahydrate, the sodium bicarbonate of 1 g, the 1.5 mL propylene diamine of 0.676 g are joined in the 30 mL propylene glycol and stir to clarify;
2.2 mentioned solution is transferred in the reactor, 200 ℃ of lower reactions 16 hours;
After 2.3 reaction finishes, through obtaining mesoporous Z 250 particle after centrifugation and the washing.The diameter of particle is about 120 nm.Shown in Fig. 5,6.The specific surface area of mesoporous Z 250 particle is 78 m
2g
-1, mean pore size is 18 nm.The output of sample is 92.7%.
Embodiment 3
3.1 the quadrol of the sodium bicarbonate of the ferric chloride hexahydrate of 0.676 g, 1.10 g, 0.15 mL joined in the 30 mL glycerol stirs to clarify;
3.2 mentioned solution is transferred in the reactor, 200 ℃ of lower reactions 20 hours;
After 3.3 reaction finishes, through obtaining hollow Z 250 particle after centrifugation and the washing.The diameter of particle is about 260 nm.As shown in Figure 7.The output of sample is 90.6%.
Embodiment 4
4.1 the quadrol of the sodium bicarbonate of the Fe(NO3)39H2O of 1.010 g, 0.6 g, 0.25 mL joined in the 30 mL ethylene glycol stirs to clarify;
4.2 mentioned solution is transferred in the reactor, 200 ℃ of lower reactions 10 hours;
After 4.3 reaction finishes, through obtaining solid Z 250 particle after centrifugation and the washing.Particle dia is about 30 nm, and magnetic saturation intensity is 70.33 emu/g.Respectively shown in Fig. 8,9.The output of sample is 90.9%.
Embodiment 5
5.1 the quadrol of the sodium bicarbonate of the ferric chloride hexahydrate of 0.676 g, 1.1g, 0.15 mL joined in the 30 mL ethylene glycol stirs to clarify;
5.2 mentioned solution is transferred in the reactor, 200 ℃ of lower reactions 14.5 hours;
After 5.3 reaction finishes, through obtaining hollow Z 250 particle after centrifugation and the washing.Particle dia is about 200 nm.As shown in figure 10.The output of sample is 90.3%.
Embodiment 6
6.1 the quadrol of the sodium bicarbonate of the ferric chloride hexahydrate of 0.676 g, 1.08 g, 0.2 mL joined in the 30 mL propyl alcohol stirs to clarify;
6.2 mentioned solution is transferred in the reactor, 200 ℃ of lower reactions 17 hours;
After 6.3 reaction finishes, through obtaining hollow ferric oxide particle after centrifugation and the washing.Particle dia is about 100 nm, and X-ray diffraction characterizes and proves ferric oxide.Respectively shown in Figure 11,12.The output of sample is 90.9%.
Embodiment 7
7.1 the butanediamine of the sodium bicarbonate of the ferric chloride hexahydrate of 0.676 g, 0.65 g, 2 mL joined in the 30 mL butyleneglycols stirs to clarify;
7.2 mentioned solution is transferred in the reactor, 200 ℃ of lower reactions 15 hours;
After 7.3 reaction finishes, through obtaining mesoporous Z 250 particle after centrifugation and the washing.The diameter of particle is about 110 nm.The specific surface area of mesoporous Z 250 particle is 73 m
2g
-1, mean pore size is 16 nm.The output of sample is 91.5%.
Embodiment 8
8.1 with the ferric chloride hexahydrate of 0.676 g, the sodium bicarbonate of 0.07 g, the thanomin of 3 mL joins in the 30 mL ethylene glycol and stirs to clarify;
8.2 mentioned solution is transferred in the reactor, 155 ℃ of lower reactions 12 hours;
After 8.3 reaction finishes, through obtaining solid Z 250 particle after centrifugation and the washing.The diameter of particle is about 150 nm.The output of sample is 92.0%.
9.1 with the ferric sulfate (III) of 1.2 g, the sodium bicarbonate of 0.21 g, the thanomin of 2 mL joins in the 30 mL ethylene glycol and stirs to clarify;
9.2 mentioned solution is transferred in the reactor, 260 ℃ of lower reactions 10 hours;
After 9.3 reaction finishes, through obtaining solid Z 250 particle after centrifugation and the washing.The diameter of particle is about 210 nm.The output of sample is 90.2%.
10.1 the quadrol of the sodium bicarbonate of the ferric chloride hexahydrate of 0.676 g, 1.2 g, 6 mL joined in the 30mL propylene glycol stirs to clarify;
10.2 mentioned solution is transferred in the reactor, 200 ℃ of lower reactions 18 hours;
After 10.3 reaction finishes, through obtaining hollow Z 250 particle after centrifugation and the washing.The diameter of particle is about 80 nm.The output of sample is 93.1%.
Embodiment 11
11.1 the butanediamine of the sodium bicarbonate of the ferric chloride hexahydrate of 0.676 g, 0.6 g, 0.5 mL joined in the 25 mL methyl alcohol stirs to clarify;
11.2 mentioned solution is transferred in the reactor, 200 ℃ of lower reactions 14 hours;
After 11.3 reaction finishes, through obtaining solid ferric oxide particle after centrifugation and the washing.The diameter of particle is about 80 nm.The output of sample is 90.7%.
Claims (10)
1. the preparation method of an iron oxide particle, it is characterized in that: described iron oxide particle is ferric oxide particle or ferriferrous oxide particles, may further comprise the steps:
(1) molysite, sodium bicarbonate, organic amine are joined in the organic solvent, stir and obtain clear solution;
(2) solution that step (1) is made into is heat-treated, the preparation ferriferous oxide;
(3) with reaction solution centrifugation, washing, the gained throw out is iron oxide particle.
2. preparation method according to claim 1, it is characterized in that: described molysite is halogenide, vitriol or the nitrate of iron; Described organic amine is quadrol, propylene diamine, butanediamine or thanomin.
3. preparation method according to claim 1 is characterized in that: during the preparation ferric oxide particle, described organic solvent is methyl alcohol, ethanol, propyl alcohol, butanols or Virahol; During the preparation ferriferrous oxide particles, described organic solvent is ethylene glycol, propylene glycol, butyleneglycol or glycerol.
4. preparation method according to claim 1, it is characterized in that: the mol ratio of molysite and sodium bicarbonate is 1:0.3-8.
5. preparation method according to claim 1, it is characterized in that: the mol ratio of molysite and organic amine is 0.9 ~ 36:1.
6. preparation method according to claim 1, it is characterized in that: the volume ratio of organic solvent and organic amine is 1:0.005 ~ 0.2.
7. preparation method according to claim 1, it is characterized in that: particle diameter is 10 ~ 600 nm, granule-morphology is the spheroidal particle of solid, mesoporous or hollow structure.
8. preparation method according to claim 7 is characterized in that: during the preparation full particle, the mol ratio of molysite and sodium bicarbonate is 1:0.3 ~ 2.9; During the preparation mesoporous particles, the mol ratio of molysite and sodium bicarbonate is 1:3 ~ 5; During the preparation hollow bead, the mol ratio of molysite and sodium bicarbonate is 1:5 ~ 8.
9. preparation method according to claim 1, it is characterized in that: in the step (2), heat-treating methods is solvent-thermal method or microwave method, and heat treated temperature is 150-260 ℃.
10. preparation method according to claim 1, it is characterized in that: in the step (2), the heat treated time is 4 ~ 24h.
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|---|---|---|---|---|
| CN103263886A (en) * | 2013-06-06 | 2013-08-28 | 湖北大学 | Hydrothermal preparation method and application of magnetic ferroferric oxide nanochain |
| CN103274477A (en) * | 2013-06-07 | 2013-09-04 | 三明学院 | Preparation method of superparamagnetic Fe3O4 microspheres |
| CN103480324A (en) * | 2013-09-29 | 2014-01-01 | 中南大学 | Mesoporous Fe3O4 microspheres and preparation and application method thereof |
| CN103663571A (en) * | 2013-12-24 | 2014-03-26 | 武汉理工大学 | Preparation method for superparamagnetism ferroferric oxide sub-micron hollow microsphere |
| CN103708564A (en) * | 2014-01-03 | 2014-04-09 | 南昌航空大学 | Solvothermal method for preparing nano ferroferric oxide powder |
| CN103801263A (en) * | 2013-12-26 | 2014-05-21 | 华南师范大学 | Method for preparing EDA-Fe3O4 nano-particles by using steel pickling waste liquor and application thereof |
| CN104058465A (en) * | 2014-07-21 | 2014-09-24 | 济南大学 | Ferroferric oxide hollow polyhedral particle and preparation method thereof |
| CN105502513A (en) * | 2015-12-23 | 2016-04-20 | 淮北师范大学 | Preparation method of hollow ferroferric oxide wave-absorbing material |
| CN107628648A (en) * | 2017-09-13 | 2018-01-26 | 清华大学 | A kind of preparation method of pattern and the controllable ferric oxide particles of size |
| WO2018187924A1 (en) * | 2017-04-11 | 2018-10-18 | 深圳市佩成科技有限责任公司 | Method for preparing fe2o3 having hollow structure based on hydrothermal synthesis |
| CN110379636A (en) * | 2019-06-06 | 2019-10-25 | 东南大学 | It is a kind of to prepare Zn ion doping Fe3O4Hollow sphere-Graphene electrodes material method |
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| CN116040689A (en) * | 2022-11-28 | 2023-05-02 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing alpha-Fe 2O3 powder with assistance of microwaves, alpha-Fe 2O3 powder and application thereof |
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| CN103263886A (en) * | 2013-06-06 | 2013-08-28 | 湖北大学 | Hydrothermal preparation method and application of magnetic ferroferric oxide nanochain |
| CN103274477B (en) * | 2013-06-07 | 2015-02-11 | 三明学院 | Preparation method of superparamagnetic Fe3O4 microspheres |
| CN103274477A (en) * | 2013-06-07 | 2013-09-04 | 三明学院 | Preparation method of superparamagnetic Fe3O4 microspheres |
| CN103480324A (en) * | 2013-09-29 | 2014-01-01 | 中南大学 | Mesoporous Fe3O4 microspheres and preparation and application method thereof |
| CN103480324B (en) * | 2013-09-29 | 2015-09-23 | 中南大学 | A kind of mesoporous Fe 3o 4microballoon and methods for making and using same thereof |
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| CN103708564B (en) * | 2014-01-03 | 2015-06-24 | 南昌航空大学 | Solvothermal method for preparing nano ferroferric oxide powder |
| CN103708564A (en) * | 2014-01-03 | 2014-04-09 | 南昌航空大学 | Solvothermal method for preparing nano ferroferric oxide powder |
| CN104058465B (en) * | 2014-07-21 | 2016-03-02 | 济南大学 | A kind of Z 250 hollow polyhedral particle and preparation method thereof |
| CN104058465A (en) * | 2014-07-21 | 2014-09-24 | 济南大学 | Ferroferric oxide hollow polyhedral particle and preparation method thereof |
| CN105502513A (en) * | 2015-12-23 | 2016-04-20 | 淮北师范大学 | Preparation method of hollow ferroferric oxide wave-absorbing material |
| WO2018187924A1 (en) * | 2017-04-11 | 2018-10-18 | 深圳市佩成科技有限责任公司 | Method for preparing fe2o3 having hollow structure based on hydrothermal synthesis |
| CN107628648A (en) * | 2017-09-13 | 2018-01-26 | 清华大学 | A kind of preparation method of pattern and the controllable ferric oxide particles of size |
| CN110379636A (en) * | 2019-06-06 | 2019-10-25 | 东南大学 | It is a kind of to prepare Zn ion doping Fe3O4Hollow sphere-Graphene electrodes material method |
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| CN111589186A (en) * | 2020-06-02 | 2020-08-28 | 林多炉 | Magnetic super-hydrophobic polyurethane sponge oil-water separation material and preparation method thereof |
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| CN116040689A (en) * | 2022-11-28 | 2023-05-02 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing alpha-Fe 2O3 powder with assistance of microwaves, alpha-Fe 2O3 powder and application thereof |
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