CN103663571A - Preparation method for superparamagnetism ferroferric oxide sub-micron hollow microsphere - Google Patents
Preparation method for superparamagnetism ferroferric oxide sub-micron hollow microsphere Download PDFInfo
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- CN103663571A CN103663571A CN201310722843.8A CN201310722843A CN103663571A CN 103663571 A CN103663571 A CN 103663571A CN 201310722843 A CN201310722843 A CN 201310722843A CN 103663571 A CN103663571 A CN 103663571A
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Abstract
The invention relates to a preparation method for a superparamagnetism ferroferric oxide sub-micron hollow microsphere. The preparation method comprises the following steps: 1) taking a reducing agent, an iron source and an alkali source, and dissolving into distilled water; 2) dissolving a surfactant into a solution obtained from step 1); 3) introducing a solution obtained from step 2) into a reaction kettle, reacting in a drying oven, performing natural cooling to room temperature for seasoning, water washing, alcohol washing, and drying in a vacuum drying box, so that the superparamagnetism ferroferric oxide sub-micron hollow microsphere is obtained. The preparation method has the following good effects: 1) according to the invention, the ferroferric oxide sub-micron hollow microsphere is compounded, and has superparamagnetism, high saturation magnetization and excellent oxidation resistance; 2) dispersing agents such as PEG (polyethylene glycol) and PVP (polyvinylpyrrolidone) are adopted to solve the problem of magnetic microsphere agglomeration, so that the ferroferric oxide sub-micron hollow microsphere with uniform particle size is obtained; 3) according to the invention, adopted raw materials is cheap, so that cost is minimized.
Description
Technical field
The present invention relates to the preparation method of SPIO submicron tiny balloon.
Background technology
A kind of as magneticsubstance, Z 250 has biocompatibility, wetting ability, magnetic responsiveness, nontoxic and chemical stability good, is applied to widely biological medicine (as magnetic targeting, bioseparation, tumour magnetic thermotherapy, MRI contrast medium, immunodetection etc.).People adopt the Z 250 microballoon of the various patterns of preparation such as chemical coprecipitation, organic high-temperature decomposition, microemulsion method, its hollow core Z 250 microballoon has low density, the characteristic of high-ratio surface, high saturation magnetization, and its hollow parts can hold a large amount of guest molecules and large-sized object, make it in many technical fields such as microwave absorbing material and medicine transmission, have important application prospect, be more and more subject to people's attention.In recent years have a lot about preparing the report of SPIO submicron tiny balloon microballoon, Peng and Sun (Angew Chem2007 for example, 46,4155) synthesized and there is SPIO microballoon, but dispersiveness is bad and saturation magnetization is low; Yu etc. adopt n-Laurylamine (Dodecylamine with Wang philosophy, DDA) and 1,6-hexanediamine is tensio-active agent, the micella forming of usining has been prepared Z 250 hollow magnetic microsphere as soft template, but this class soft template often need to be by a large amount of organic substances, easily form and pollute, biocompatibility is poor, is unfavorable for biomedical applications; Polystyrene (the Polystyzene after with hydrophilic modification such as Huang, PS) ball is hard template, by deposition-calcining, prepared Z 250 mesoporous microsphere. this hard template method is easy to promote, there is ubiquity and relatively easily control, but shortcoming is need to experience multistep complex operations and thus obtained microsphere pattern is bad, easily cave in, saturation magnetization is low.In order to promote Z 250 to be applied to better biomedicine field, prepare to there is superparamagnetism, good biocompatibility, antioxidant property, high saturation and magnetic intensity be the problem of needing solution badly.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of simple and fast for above-mentioned prior art, the preparation method of SPIO submicron tiny balloon with low cost, the strong and good biocompatibility of the antioxidant property of Z 250 submicron tiny balloon.
The present invention solves the problems of the technologies described above adopted technical scheme: the preparation method of SPIO submicron tiny balloon, includes following steps:
1) get 4～10mmol reductive agent, 2～6mmol source of iron and 6～15mmol alkali source, be dissolved in distilled water;
2) by tensio-active agent 1 * 10
-4～6 * 10
-4mmol is dissolved in step 1) gained solution;
3) by step 2) solution of gained moves in reactor, in 150～220 ℃ of baking ovens, react 8～20h, naturally cool to room temperature ageing, washing, alcohol wash 2～5 times, dry in 40～70 ℃ of vacuum drying ovens, obtain having SPIO submicron tiny balloon.
Press such scheme, described reductive agent is any one in trisodium citrate, glucose and citric acid; Described source of iron is any one in iron(ic) chloride, ferric sulfate and iron nitrate and hydrate thereof; Described alkali source is any one in volatile salt, bicarbonate of ammonia, ammonium acetate and urea.
Press such scheme, described tensio-active agent is any one or any two kinds of combinations in polyacrylamide, polyoxyethylene glycol, Sodium dodecylbenzene sulfonate and polyvinylpyrrolidone.
The reaction mechanism of this experiment is Ostwald maturing process.Its mechanism is in solution, and small-particle dissolves, the process that macrobead is grown up, and amorphous solid sphere continues to grow up, and starts crystallization on the surface of ball, and surface crystallization makes to increase in the surperficial composition grain-size of ball, and crystallinity improves.With ball surface large size, the Particle Phase ratio of good crystallinity, the specific surface energy of the amorphous particle of ball inside is larger, and this provides motivating force for Ostwald.Then the particle of ball inside trends towards dissolving, and causes the formation in ball boring region, thereby forms tiny balloon.
Excellent results of the present invention:
1) the present invention synthesized there is superparamagnetism, the Z 250 submicron tiny balloon of high saturation and magnetic intensity, antioxidant property excellence;
2) adopt polyoxyethylene glycol, polyvinylpyrrolidone etc. to do the agglomeration traits that dispersion agent has overcome magnetic microsphere, obtain the uniform Z 250 submicron of grain diameter tiny balloon.
3) the present invention's cost of material used is cheap, has realized minimizing costs.
Accompanying drawing explanation
Fig. 1 is the x-ray diffraction pattern of the prepared SPIO submicron of embodiment 1 tiny balloon;
Fig. 2 is SEM (a) and the rear TEM figure of section (b) thereof of the prepared SPIO submicron of embodiment 1 tiny balloon;
Fig. 3 is the magnetic hysteresis loop of the prepared SPIO submicron of embodiment 1 tiny balloon.
Embodiment
In order to understand better the present invention, below in conjunction with embodiment, further illustrate content of the present invention, but content of the present invention is not only confined to example below.
Embodiment 1
By 8mmol trisodium citrate, 4mmolFeCl
3.6H
2o, 12mmolNH
4hCO
3be dissolved in 80ml distilled water, use magneton stirring and dissolving, add 2 * 10
-4mmol polyacrylamide (PAM) and 1 * 10
-4mmol polyoxyethylene glycol (PEG).To be dissolved completely after, move in 100ml reactor, in 220 ℃ of baking ovens, react, reaction 8h, room temperature ageing to be chilled to, then washs respectively 2 times with distilled water, dehydrated alcohol, centrifugal, in 50 ℃ of vacuum drying ovens, dries, and obtains product.
Z 250 submicron tiny balloon of the present invention is through X-ray powder diffraction (XRD), and result is all diffraction peaks and Fe as seen from Figure 1
3o
4(JCPDS79-0419) corresponding, there is not Fe
2o
3characteristic diffraction peak (110), (210), (211) etc., show that product is pure Fe
3o
4.After scanning electronic microscope (SEM) and section, transmission electron microscope (TEM) characterizes, and result shows that prepared Z 250 has hollow structure, and size is in 250nm left and right (see figure 2).Magnetic test sample has superparamagnetism, and under room temperature, high saturation and magnetic intensity is that 70emu/g(is shown in Fig. 3).Gained sample is exposed to in air 15 days and without tawny material, generates, still present black, show that prepared Z 250 has antioxidant property.
Embodiment 2
By 10mmol trisodium citrate, 4mmol FeCl
3.6H
2o, 8mmol NH
4aC is dissolved in 60ml distilled water, use magneton stirring and dissolving, add PAM and the PEG of above-described embodiment 1 same amount to make tensio-active agent, to be dissolved completely after, move in 100ml reactor, in 220 ℃ of baking ovens, react reaction 8h, room temperature ageing to be chilled to, then with distilled water, dehydrated alcohol, wash respectively 2 times, centrifugal, in 50 ℃ of vacuum drying ovens, dry, obtain product.The pattern and the character that obtain product are similar to Example 1.
Embodiment 3
By 8mmol trisodium citrate, 4mmol FeCl
3.6H
2o, 6mmol urea is dissolved in 60ml distilled water, uses magneton stirring and dissolving, add PAM and the PEG of above-described embodiment 1 same amount to make tensio-active agent, to be dissolved completely after, move in 100ml reactor, in 180 ℃ of baking ovens, react, reaction 8h, room temperature ageing to be chilled to, then washs respectively 2 times with distilled water, dehydrated alcohol, centrifugal, in 50 ℃ of vacuum drying ovens, dry, obtain product.The pattern and the character that obtain product are similar to Example 1.
Embodiment 4
By 8mmol trisodium citrate, 2mmolFe
2(SO
4)
3.7H
2o, 12mmolNH
4hCO
3be dissolved in 80ml distilled water, use magneton stirring and dissolving, add PAM and the PEG of above-described embodiment 1 same amount to make tensio-active agent, to be dissolved completely after, move in 100ml reactor, in 160 ℃ of baking ovens, react, reaction 12h, room temperature ageing to be chilled to, then with distilled water, dehydrated alcohol, wash respectively 2 times, centrifugal, in 50 ℃ of vacuum drying ovens, dry, obtain product, the pattern and the character that obtain product are similar to Example 1.
Embodiment 5
By 8mmol trisodium citrate, 4mmolFe (NO
3)
3.9H
2o, 10mmolNH
4hCO
3be dissolved in 60ml distilled water, use magneton stirring and dissolving, add PAM and the PEG of above-described embodiment 1 same amount to make tensio-active agent, to be dissolved completely after, move in 100ml reactor, in 180 ℃ of baking ovens, react, reaction 12h, room temperature ageing to be chilled to, then with distilled water, dehydrated alcohol, wash respectively 2 times, centrifugal, in 50 ℃ of vacuum drying ovens, dry and obtain product.The pattern and the character that obtain product are similar to Example 1.
Embodiment 6
By 8mmol trisodium citrate, 4mmol FeCl
3.6H
2o, 12mmolNH
4aC is dissolved in 60ml distilled water, uses magneton stirring and dissolving, adds 1 * 10
-4mmol Sodium dodecylbenzene sulfonate is made tensio-active agent, to be dissolved completely after, move in 100ml reactor, in 180 ℃ of baking ovens, react reaction 10h, room temperature ageing to be chilled to, then with distilled water, dehydrated alcohol, wash respectively 2 times, centrifugal, in 50 ℃ of vacuum drying ovens, dry, obtain product.The pattern and the character that obtain product are similar to Example 1.
Obviously, above-described embodiment is to be only the example that clearly explanation is done, and the not restriction to embodiment.For those of ordinary skill in the field, in the above-mentioned data of base of above-mentioned explanation, show can also make other changes in different forms on plinth, exhaustive without also giving all embodiments here.And the apparent variation of therefore amplifying or change are still within the protection domain in the invention.
Claims (3)
1. the preparation method of SPIO submicron tiny balloon, includes following steps:
1) get 4～10mmol reductive agent, 2～6mmol source of iron and 10～15mmol alkali source, be dissolved in distilled water;
2) by tensio-active agent 2 * 10
-4～6 * 10
-4mmol is dissolved in step 1) gained solution;
3) by step 2) solution of gained moves in reactor, in 150～220 ℃ of baking ovens, react 8～20h, naturally cool to room temperature ageing 3～10h, washing, alcohol wash 2～5 times, dry in 40～70 ℃ of vacuum drying ovens, obtain having SPIO submicron tiny balloon.
2. the preparation method of SPIO submicron tiny balloon according to claim 1, is characterized in that described reductive agent is any one in trisodium citrate, glucose and citric acid; Described source of iron is any one in iron(ic) chloride, ferric sulfate and iron nitrate and hydrate thereof; Described alkali source is any one in volatile salt, bicarbonate of ammonia, ammonium acetate and urea.
3. the preparation method of SPIO submicron tiny balloon according to claim 1 and 2, is characterized in that described tensio-active agent is any one or any two kinds of combinations in polyacrylamide, polyoxyethylene glycol, Sodium dodecylbenzene sulfonate and polyvinylpyrrolidone.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058465A (en) * | 2014-07-21 | 2014-09-24 | 济南大学 | Ferroferric oxide hollow polyhedral particle and preparation method thereof |
| CN105198003A (en) * | 2015-08-17 | 2015-12-30 | 商丘师范学院 | Method for preparing paramagnetic ferroferric oxide nano particles |
| CN105776350A (en) * | 2016-03-17 | 2016-07-20 | 中国科学院宁波材料技术与工程研究所 | Hollow rod-shaped ferriferous oxide and method for preparing compounds of hollow rod-shaped ferriferous oxide |
| CN105903032A (en) * | 2016-05-31 | 2016-08-31 | 武汉理工大学 | Super-paramagnetic targeting dual-drug sustained-release carrier material and preparation method thereof |
| CN106280257A (en) * | 2016-08-16 | 2017-01-04 | 梅庆波 | A kind of preparation method of lightweight homogeneous anti-impact epoxy fill-sealing materials |
| CN107096039A (en) * | 2017-04-27 | 2017-08-29 | 武汉理工大学 | A kind of double medicines that carry of magnetic targeted pass release system and preparation method thereof |
| CN107827164A (en) * | 2017-09-30 | 2018-03-23 | 清华大学 | The preparation method of the ferroferric oxide nano granules of the high yield thermal efficiency under a kind of magnetic field |
| CN107899540A (en) * | 2017-11-22 | 2018-04-13 | 广西师范大学 | Fe is prepared using sol-gal process3O4The method of 41 magnetic composites of@MCM |
| CN108030932A (en) * | 2017-11-20 | 2018-05-15 | 苏州大学 | Mesoporous Fe3O4Composite material and preparation method thereof and the application in tumour MRI radiographies and photo-thermal/chemotherapy synergistic treatment |
| CN108658128A (en) * | 2018-08-02 | 2018-10-16 | 合肥中航纳米技术发展有限公司 | A kind of MoS with hierarchical structure2The preparation method of micro-nano ball |
| CN108682847A (en) * | 2018-05-07 | 2018-10-19 | 苏州大学 | A kind of more shell hollow microsphere shape α-Fe2O3Material, preparation method and applications |
| CN108887762A (en) * | 2018-06-11 | 2018-11-27 | 佛山市南海区佳妍内衣有限公司 | A kind of underpants with far-infrared physiotherapy function |
| CN112340780A (en) * | 2020-11-23 | 2021-02-09 | 安徽师范大学 | Monodisperse superparamagnetic Fe3O4Nano super particle and its preparation method |
| CN113975389A (en) * | 2021-09-30 | 2022-01-28 | 中山大学孙逸仙纪念医院 | Macrophage-loaded multifunctional mesoporous iron oxide nano diagnosis and treatment preparation, preparation method thereof and anti-tumor application thereof |
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Cited By (18)
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| 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 |
| CN105198003A (en) * | 2015-08-17 | 2015-12-30 | 商丘师范学院 | Method for preparing paramagnetic ferroferric oxide nano particles |
| CN105776350A (en) * | 2016-03-17 | 2016-07-20 | 中国科学院宁波材料技术与工程研究所 | Hollow rod-shaped ferriferous oxide and method for preparing compounds of hollow rod-shaped ferriferous oxide |
| CN105903032A (en) * | 2016-05-31 | 2016-08-31 | 武汉理工大学 | Super-paramagnetic targeting dual-drug sustained-release carrier material and preparation method thereof |
| CN106280257A (en) * | 2016-08-16 | 2017-01-04 | 梅庆波 | A kind of preparation method of lightweight homogeneous anti-impact epoxy fill-sealing materials |
| CN107096039B (en) * | 2017-04-27 | 2019-11-26 | 武汉理工大学 | A kind of double medicines that carry of magnetic targeted pass release system and preparation method thereof |
| CN107096039A (en) * | 2017-04-27 | 2017-08-29 | 武汉理工大学 | A kind of double medicines that carry of magnetic targeted pass release system and preparation method thereof |
| CN107827164A (en) * | 2017-09-30 | 2018-03-23 | 清华大学 | The preparation method of the ferroferric oxide nano granules of the high yield thermal efficiency under a kind of magnetic field |
| CN108030932A (en) * | 2017-11-20 | 2018-05-15 | 苏州大学 | Mesoporous Fe3O4Composite material and preparation method thereof and the application in tumour MRI radiographies and photo-thermal/chemotherapy synergistic treatment |
| CN107899540A (en) * | 2017-11-22 | 2018-04-13 | 广西师范大学 | Fe is prepared using sol-gal process3O4The method of 41 magnetic composites of@MCM |
| CN108682847A (en) * | 2018-05-07 | 2018-10-19 | 苏州大学 | A kind of more shell hollow microsphere shape α-Fe2O3Material, preparation method and applications |
| CN108682847B (en) * | 2018-05-07 | 2021-03-16 | 苏州大学 | Multi-shell hollow microspherical alpha-Fe2O3Material, preparation method and application thereof |
| CN108887762A (en) * | 2018-06-11 | 2018-11-27 | 佛山市南海区佳妍内衣有限公司 | A kind of underpants with far-infrared physiotherapy function |
| CN108658128A (en) * | 2018-08-02 | 2018-10-16 | 合肥中航纳米技术发展有限公司 | A kind of MoS with hierarchical structure2The preparation method of micro-nano ball |
| CN112340780A (en) * | 2020-11-23 | 2021-02-09 | 安徽师范大学 | Monodisperse superparamagnetic Fe3O4Nano super particle and its preparation method |
| CN113975389A (en) * | 2021-09-30 | 2022-01-28 | 中山大学孙逸仙纪念医院 | Macrophage-loaded multifunctional mesoporous iron oxide nano diagnosis and treatment preparation, preparation method thereof and anti-tumor application thereof |
| CN113975389B (en) * | 2021-09-30 | 2023-07-18 | 中山大学孙逸仙纪念医院 | Macrophage-loaded multifunctional mesoporous ferric oxide nano diagnosis and treatment preparation, preparation method thereof and anti-tumor application |
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