CN1493608A - Nano-ferroferric oxide/polystyrene magnetic composite material and its preparation method - Google Patents
Nano-ferroferric oxide/polystyrene magnetic composite material and its preparation method Download PDFInfo
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- CN1493608A CN1493608A CNA031507247A CN03150724A CN1493608A CN 1493608 A CN1493608 A CN 1493608A CN A031507247 A CNA031507247 A CN A031507247A CN 03150724 A CN03150724 A CN 03150724A CN 1493608 A CN1493608 A CN 1493608A
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Abstract
A nano-class magnetic composite Fe3O4/polystyrene material is prepared through mixing the aqueous solution of two-valence Fe salt with that of three-valence one, adding alkali solution containing surfactant, reacting to obtain Fe3O4 nanoparticles, and ball grinding for dispersing them in styrene monomer while polymerizing reaction.
Description
Technical field
The present invention relates to the preparation method of a kind of nano ferriferrous oxide/polystyrene magnetic composite, particularly the preparation method of substance law synthesis of nano Z 250/polystyrene magnetic composite.
Background technology
As everyone knows, polystyrene is one of general-purpose plastics of a kind of applied range, have advantages such as cheap, that easy-formation is processed, water absorbability is low, but polystyrene is a kind of macromolecular material, nonmagnetic, as be applied to fields such as electronic apparatus, instrument, microwave device, and can not play the effect of shielding electromagnetic wave and absorption microwave, therefore make its range of application be subjected to limitation.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of nano ferriferrous oxide/polystyrene magnetic composite and preparation method thereof, to overcome the above-mentioned limitation of polystyrene, satisfy the needs in fields such as electronic apparatus, instrument, microwave device.
The present invention is that technical conceive is such:
Nano ferriferrous oxide is a kind of ferrite of ferrimagnetism of simple spinel type, be easy to preparation, has superparamagnetism, the contriver thinks, if the performance of nano ferriferrous oxide and polystyrene is combined, prepare a kind of have certain superparamagnetism, coercive force is low, magnetic hysteresis loss is little magneticsubstance, the magnetic functionization that not only can give polystyrene, and can enlarge the Application Areas of polystyrene, improve the added value of polystyrene.
Nano ferriferrous oxide of the present invention/polystyrene magnetic composite is a kind of composition, and its component and weight percent content comprise:
Polystyrene 90～99%, Z 250 1～10wt%.
The Z 250 particle diameter is 20～180 nanometers.
The preparation method of nano ferriferrous oxide of the present invention/polystyrene magnetic composite comprises the steps:
With the nano ferriferrous oxide particle under the effect of tensio-active agent, with the styrene monomer ball milling, the nano ferriferrous oxide particle is distributed in the styrene monomer, cause with initiator then and carry out bulk polymerization, make nano ferriferrous oxide/polystyrene magnetic composite, temperature of reaction is 60～75 ℃, and the reaction times is 3～5 hours;
The add-on of tensio-active agent is 5～30% of a Z 250 particle gross weight
In the acid of described surfactant package oil scraper, sodium oleate, sodium lauryl sulphate or the Sodium dodecylbenzene sulfonate etc. one or more, preferred surfactants is oleic acid or sodium oleate.
Described basic solution refers to ammoniacal liquor, aqueous sodium hydroxide solution, potassium hydroxide aqueous solution etc.
Most preferred basic solution is ammoniacal liquor or aqueous sodium hydroxide solution.
Described initiator refers to a kind of in benzoyl peroxide, peroxidation two (2-toluyl), Diisopropyl azodicarboxylate or the 2,2'-Azobis(2,4-dimethylvaleronitrile) etc., preferred initiator is Diisopropyl azodicarboxylate or 2,2'-Azobis(2,4-dimethylvaleronitrile), and its add-on is 0.1～1wt% of amount of monomer;
Said nano ferriferrous oxide can adopt conventional method to be prepared, as adopting Guan Chengxin, An Yuling, the preparation of super-paramagnetic ferriferrous oxide particulate and application.Magneticsubstance and device, 1992,23 (3): 23-25 document disclosed method.
The employing vibrating sample magnetometer detects, its coercive force≤20Oe;
Preparation method of the present invention is simple, only needs be mixed into equably in styrene monomer nano ferriferrous oxide, and frequent gauge polyreaction can be synthesized and obtained nano ferriferrous oxide/polystyrene magnetic composite.
Description of drawings
Fig. 1 is nano ferriferrous oxide/polystyrene magnetic composite magnetic hysteresis loop.
Fig. 2 is nano ferriferrous oxide/polystyrene magnetic composite magnetic hysteresis loop of embodiment 2.
Fig. 3 is nano ferriferrous oxide/polystyrene magnetic composite magnetic hysteresis loop of embodiment 3.
Embodiment
Embodiment 1
Prepare the aqueous solution of 1mol/L, 2mol/L, 0.9mol/L respectively with iron(ic) chloride, iron protochloride, ammoniacal liquor; Press Fe
3+: Fe
2+=2: 1 (mol ratio) mixed ferric chloride Solution, solution of ferrous chloride, high-speed stirring under 55 ℃ condition, the ammoniacal liquor that adds 0.9mol/L at twice, the oleic acid that when solution becomes sorrel, adds Z 250 weight 20%, the pH value of final control solution is 10, collect the nano ferriferrous oxide particle from solution, particle diameter is about 10nm;
To neutral, again with absolute ethanol washing repeatedly, the Z 250 after the washing is put into 70 ℃ vacuum drying oven drying to the black nano Z 250 particle that then reaction is obtained with deionized water wash.
Dried nano ferriferrous oxide and styrene monomer put on the ball mill under oleic effect, carried out ball milling 36 hours, nano ferriferrous oxide/vinylbenzene dispersion system, nano ferriferrous oxide content is 0.6421wt%.The benzoyl peroxide that adds styrene monomer weight 0.5% then, reacted 4 hours, temperature of reaction is 75 ℃, carry out mass polymerization and get nano ferriferrous oxide/polystyrene magnetic composite, wherein, the Z 250 particle diameter is 20～180 nanometers, and coercive force is 15Oe, and specific saturation magnetization is 32.84emu/g.Magnetic hysteresis loop is seen Fig. 1.
Embodiment 2
Prepare the aqueous solution of 1mol/L, 2mol/L, 0.9mol/L respectively with iron(ic) chloride, iron protochloride, sodium hydroxide; Press Fe
3+: Fe
2+=2: 1 (mol ratio) mixed ferric chloride Solution, solution of ferrous chloride, high-speed stirring under 60 ℃ condition, the sodium hydroxide solution that adds 0.9mol/L at twice, the oleic acid that when solution becomes sorrel, adds Z 250 weight 20%, the pH value of final control solution is 12, get the nano ferriferrous oxide particle, particle diameter is about 10nm.To neutral, again with absolute ethanol washing repeatedly, the Z 250 after the washing is put into 70 ℃ vacuum drying oven drying to the black nano Z 250 particle that then reaction is obtained with deionized water wash.
With dried nano ferriferrous oxide and styrene monomer put under the oleic effect of tensio-active agent, carry out on the ball mill ball milling 36 hours nano ferriferrous oxide/vinylbenzene dispersion system, nano ferriferrous oxide content is 1.591wt%.The benzoyl peroxide that adds styrene monomer weight 0.5% then is that initiator carries out mass polymerization, reacted 4 hours, temperature of reaction is 75 ℃, get nano ferriferrous oxide/polystyrene magnetic composite, wherein, the Z 250 particle diameter is 20～180 nanometers, and coercive force is 10Oe, specific saturation magnetization is 36.73emu/g, and magnetic hysteresis loop is seen Fig. 2.
Embodiment 3
Prepare the aqueous solution of 1mol/L, 2mol/L, 0.9mol/L respectively with iron(ic) chloride, iron protochloride, ammoniacal liquor; Press Fe
3+: Fe
2+=2: 1 (mol ratio) mixed ferric chloride Solution, solution of ferrous chloride, high-speed stirring under 50 ℃ condition, the ammoniacal liquor that adds 0.9mol/L at twice, the oleic acid that when solution becomes sorrel, adds Z 250 weight 20%, the pH value of final control solution gets nano ferriferrous oxide particle 10nm 8.To neutral, again with absolute ethanol washing repeatedly, the Z 250 after the washing is put into 70 ℃ vacuum drying oven drying to the black nano Z 250 particle that then reaction is obtained with deionized water wash.
With dried nano ferriferrous oxide and styrene monomer put under the oleic effect of tensio-active agent, carry out on the ball mill ball milling 36 hours nano ferriferrous oxide/vinylbenzene dispersion system, nano ferriferrous oxide content is 5.991wt%.The benzoyl peroxide that adds styrene monomer weight 0.5% then is an initiator, reacted 4 hours, temperature of reaction is 75 ℃, carry out mass polymerization and get nano ferriferrous oxide/polystyrene magnetic composite, wherein, the Z 250 particle diameter is 20～180 nanometers, and coercive force is 10Oe, and specific saturation magnetization is 46.56emu/g.Magnetic hysteresis loop is seen Fig. 3.
Claims (5)
1. nano ferriferrous oxide/polystyrene magnetic composite is characterized in that component and weight percent content comprise: polystyrene 90～99%, Z 250 1～10wt%.
2. nano ferriferrous oxide according to claim 1/polystyrene magnetic composite is characterized in that, the Z 250 particle diameter is 20～180 nanometers.
3. the preparation method of nano ferriferrous oxide according to claim 1 and 2/polystyrene magnetic composite, be characterised in that and comprise the steps: the nano ferriferrous oxide particle under the effect of tensio-active agent, with the styrene monomer ball milling, cause with initiator then and carry out bulk polymerization, make nano ferriferrous oxide/polystyrene magnetic composite.
4. method according to claim 3 is characterized in that, one or more in the acid of described surfactant package oil scraper, sodium oleate, sodium lauryl sulphate or the Sodium dodecylbenzene sulfonate.
5. method according to claim 3 is characterized in that, described initiator comprises a kind of in benzoyl peroxide, peroxidation two (2-toluyl), Diisopropyl azodicarboxylate or the 2,2'-Azobis(2,4-dimethylvaleronitrile).
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| CN1298791C (en) * | 2005-07-19 | 2007-02-07 | 吉林大学 | Superparamagnetic Fe3O4 nanometer particle with synthetic polymer modification from one-step method |
| CN1303136C (en) * | 2004-11-18 | 2007-03-07 | 同济大学 | Method for preparing hollow magnetic composite particulate for magnetic rheologic liquid by using polystyrene microsphere |
| CN100392025C (en) * | 2005-05-30 | 2008-06-04 | 河南大学 | In situ method for preparing modified Nano powder of hydrate, hydroxy salt, and oxide |
| CN100404609C (en) * | 2006-04-28 | 2008-07-23 | 西北工业大学 | Process for preparing polystyrene/Fe3O4 composite magnetic micro ball |
| CN101337171B (en) * | 2007-07-05 | 2011-09-28 | 上海华明高技术（集团）有限公司 | Hollow microsphere containing silicon magnetism and preparation method and use thereof |
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2003
- 2003-09-02 CN CNA031507247A patent/CN1493608A/en active Pending
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| CN1303136C (en) * | 2004-11-18 | 2007-03-07 | 同济大学 | Method for preparing hollow magnetic composite particulate for magnetic rheologic liquid by using polystyrene microsphere |
| CN100392025C (en) * | 2005-05-30 | 2008-06-04 | 河南大学 | In situ method for preparing modified Nano powder of hydrate, hydroxy salt, and oxide |
| CN1298791C (en) * | 2005-07-19 | 2007-02-07 | 吉林大学 | Superparamagnetic Fe3O4 nanometer particle with synthetic polymer modification from one-step method |
| CN100404609C (en) * | 2006-04-28 | 2008-07-23 | 西北工业大学 | Process for preparing polystyrene/Fe3O4 composite magnetic micro ball |
| CN101337171B (en) * | 2007-07-05 | 2011-09-28 | 上海华明高技术（集团）有限公司 | Hollow microsphere containing silicon magnetism and preparation method and use thereof |
| CN101768797B (en) * | 2008-12-30 | 2011-12-21 | 黑龙江大学 | One-dimensional magnetic fiber material, preparation method thereof and use thereof |
| CN102206413B (en) * | 2011-05-25 | 2013-06-12 | 广东高怡新工程塑料有限公司 | Plastic-based composite material with electric conduction and electromagnetic shielding functions and preparation method thereof |
| CN102206414A (en) * | 2011-05-25 | 2011-10-05 | 佛山市顺德区高怡新塑料有限公司 | Calorific electromagnetic shielding plastic-based composite material and preparation method thereof |
| CN102206413A (en) * | 2011-05-25 | 2011-10-05 | 佛山市顺德区高怡新塑料有限公司 | Plastic-based composite material with electric conduction and electromagnetic shielding functions and preparation method thereof |
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| CN102206414B (en) * | 2011-05-25 | 2013-02-20 | 广东高怡新工程塑料有限公司 | Calorific electromagnetic shielding plastic-based composite material and preparation method thereof |
| CN102964539A (en) * | 2012-10-19 | 2013-03-13 | 南京林业大学 | Preparation method of porous magnetic polystyrene microspheres |
| CN102964539B (en) * | 2012-10-19 | 2016-05-25 | 南京林业大学 | The preparation method of porous magnetic polystyrene microsphere |
| CN103288140A (en) * | 2013-06-21 | 2013-09-11 | 山西大同大学 | Method for simply regulating ferroferric oxide nanoparticle morphology |
| CN103288140B (en) * | 2013-06-21 | 2015-08-26 | 山西大同大学 | A kind of method of simple regulation and control ferroferric oxide nanoparticle morphology |
| CN103318972A (en) * | 2013-06-25 | 2013-09-25 | 升华集团德清华源颜料有限公司 | Preparation process of magnetic black iron oxide |
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| CN104761668B (en) * | 2015-03-24 | 2018-10-26 | 广州市香港科大***研究院 | A kind of bulk polymerization of microwave heating non-polar monomer |
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